CN100335420C - Production process of solid composite ferric sulfate polymer - Google Patents
Production process of solid composite ferric sulfate polymer Download PDFInfo
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- CN100335420C CN100335420C CNB2005100375516A CN200510037551A CN100335420C CN 100335420 C CN100335420 C CN 100335420C CN B2005100375516 A CNB2005100375516 A CN B2005100375516A CN 200510037551 A CN200510037551 A CN 200510037551A CN 100335420 C CN100335420 C CN 100335420C
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Abstract
The present invention provides a method for producing solid composite polymeric ferric sulfate, which comprises the following processing steps: 600 to 900 weight percent of sulfuric acid cinder, 300 to 800 weight percent of water and 600 to 800 weight percent of concentrated sulfuric acid are put into a reactor, heated and stirred, the reaction temperature is controlled to be from 100 to 150DEG C, and the reactor pressure is controlled to be less than or equal to 0.5MPa; after the reaction is carried out for 3.0 to 5.0 hours, 100 to 180 weight percent of an additive agent is added, and the reaction is continued for 20 to 60 minutes; after cooled to reach the temperature below 80DEG C, the mixed solution is puffed, solidified, dried and crushed to obtain a finished product. The present invention directly obtains a solid polymeric ferric sulfate product in a one-step method. The product of the present invention can be used for pretreatment, decolorization, deodorization, COD removal, heavy metal removal and algae removal in water treatment and for treating paper manufacturing polluted water, printing polluted water, oily polluted water, etc. The present invention has the advantages of rapidity, convenience, energy saving, obvious effect, large alum patterns and high settling velocity.
Description
Technical field
The invention belongs to the chemical industry of inorganic salt field, particularly a kind of production method of new and effective composite solid water purification agent.
Background technology
Treatment effect is not ideal enough on the one hand for low molecular inorganic salt water treatment agent, not as polymer inorganic salt water treatment agent, as: polymeric aluminum series, polymerization iron series; High molecular on the other hand inorganic salt water treatment agent cost of manufacture is lower than low molecular inorganic salt water treatment agent.
Bodied ferric sulfate is a kind of inorganic polymer water treatment agent.Mostly being with the ferrous sulfate on the market now is main raw material, the liquid product that is prepared from through oxidation style or catalytic oxidation, or processes such as liquid product is spray-dried are obtained solid phase prod.Oxygenant that is adopted in the production or catalytic oxidant are generally sodium chlorate, Sodium Nitrite or nitric acid etc., not only price is higher, and be easy in process of production produce gas contamination problems such as oxynitride, chlorine, and contain nitrate radical, nitrite anions etc. in the product.Liquid product less stable of producing and transportation are inconvenient, the solid phase prod energy consumption height of spray-dried gained.
Summary of the invention
The objective of the invention is to overcome the weak point that prior art exists, a kind of solid composite ferric sulfate polymer production method is provided.The solid composite ferric sulfate polymer that the present invention produces, be that employing industrial solid castoff sulfate slag is a main raw material, make the inorganic high molecular water purifier of solid high-efficiency through single stage method, that this method products obtained therefrom has is with low cost, energy-saving and cost-reducing characteristics, has reduced the cost of inorganic salt water treatment agents; In addition, also be that the industrial solid castoff sulfate cinder has obtained recycling treatment, having reached turns waste into wealth.
Purpose of the present invention realizes by following technical proposals: a kind of solid composite ferric sulfate polymer production method comprises the steps:
The water of the sulfate cinder of 600～900 parts of weight, 300～800 parts of weight and the vitriol oil of 600～800 parts of weight are added in the reactor, heating is also stirred, temperature of reaction is controlled at 100～150 ℃, reactor pressure is controlled at≤0.5MPa, after reaction is carried out 3.0～5.0 hours, in calcium oxide, lime carbonate, yellow soda ash, aluminum oxide, aluminate or the magnesium salts of 100～180 parts of weight of adding one or more are as additive, continue reaction after 20～60 minutes, blowing after cooling off, pass through expanded fast, mummification again, pulverize, get finished product.When not adding water, can working concentration be the mixture that corresponding sulphuric acid soln more than 50% replaces the vitriol oil of the water of above-mentioned 300～800 parts of weight and 600～800 parts of weight.
Contain Fe in the described sulfate cinder
2O
3, Fe
3O
4, oxide compounds such as the oxide compound of silicon or silicate.
Iron-holder is 30～65% in the described sulfate cinder.
As a kind of preferred version, according to chemical equation Fe
2O
3+ 3H
2SO
4=Fe
2(SO
4)
3+ 3H
2O just with sulfate cinder in the iron complete reaction time needed vitriolic amount of substance be B, in order to add fast response, actual to add vitriolic amount of substance C be 105%～120%B, generally adopts C=105%～110%B.
In order to realize the present invention better, the described vitriol oil is that mass concentration is 98% technical grade sulfuric acid or 92.5% technical grade sulfuric acid.Temperature of reaction preferably is controlled at about 120 ℃.The time of described mummification is 2～12 hours.
The present invention adopts single stage method to prepare solid ferric polysulfate, promptly can directly make the solid bodied ferric sulfate by physical-chemical reaction, without concentrate drying.Byproduct sulfate cinder when the main raw material that the present invention adopts is industrial preparation sulfuric acid is red-brown or brown or black, and Fe is contained in general the inside
2O
3, Fe
3O
4, silicon oxide compound or silicate, and the oxide compound of metals such as calcium, magnesium, aluminium etc. also has 98% sulfuric acid or 92.5% sulfuric acid and auxiliary material additive, all be on the market valency easy raw material.Added additive in the reaction, on the one hand, can make to solidify expandedly to become faster, shortened and solidified the expanded time, and made product become more fluffy, be easy to pulverize; On the other hand, some solid nucleus can be provided in product, these nucleus mainly are calcium sulfate etc., the nucleus that these precipitations are served as had both helped the rapid solidification of product behind the blowing, help water purification agent in the water treatment coagulation process, to bring into play again and help the effect of coagulating, can serve as the nucleus that flco forms in the coagulation process, impel little flco to grow up, become bigger flco, improve the coagulation performance of water purification agent.In use flocculating effect is better to make product, and settling of floccus speed is faster.
Among the present invention in the gained solid composite ferric sulfate polymer product except that containing main component polymerization iron, also contain a certain amount of positively charged ion, as Ca
2+, Mg
2+, Al
3+, Fe
2+Deng; Also contain certain negatively charged ion in the products obtained therefrom of the present invention, as SO
4 2-, Cl
-, SiO
4 2-Deng.
Product of the present invention can be used for pre-treatment, decolouring, the deodorizing in the water treatment and removes COD
Cr, BOD
5, heavy metal and algae, handle papermaking, printing and dyeing, oily(waste)water various industrial sewage and urban comprehensive wastewater etc., effect is obvious, alumen ustum is big, settling velocity is fast.
The present invention compares with prior art, has following advantage and beneficial effect:
1, processes such as sour molten hydrolysis have been adopted in invention, and directly single stage method obtains high-performance solid composite ferric sulfate polymer product, have quick, convenient, energy-conservation characteristics.
2, the present invention has adopted additives such as adding calcium oxide, lime carbonate, yellow soda ash, aluminum oxide, aluminate or magnesium salts to promote polymerization, solidify and accelerate reaction process such as expanded, increase metal ions such as calcium, magnesium etc. simultaneously, help the carrying out of the process such as elimination of colloid stability, cohesion, flocculation, adsorption precipitation in the water treatment.
3, invention is not owing to adopt oxygenant such as Sodium Nitrite, nitric acid, chlorine or sodium chlorate etc., so can be in product not residual have objectionable impuritiess such as nitrate radical, nitrite anions, can when producing, not overflow toxic gas such as oxynitride and chlorine yet and environment is produced pollute.
4, products obtained therefrom of the present invention is compared with traditional inorganic flocculating agent, removes COD
Cr, BOD
5, heavy metal, suspended substance, colourity etc. effect obvious.
5, products obtained therefrom of the present invention is compared with polymerize aluminum chloride, and the alumen ustum of formation is big, and settling velocity is fast.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, but embodiments of the present invention are not limited thereto.
Embodiment 1
With 900kg sulfate cinder, 600kg water and 800kg concentration is that 92.5～98% the vitriol oil is put into reactor, heating is also stirred, temperature of reaction is controlled at 140 ± 5 ℃, pressure 0.4 ± 0.05MPa, keep this reaction conditions, reaction was carried out 3.0 hours, added additive calcium oxide 160kg and yellow soda ash 10kg, reacted 20 minutes, cooling reduces system temperature below 80 ℃ then again; Reactant put into solidify the mummification reaction tank, after mummification in 4 hours, crushing packing promptly gets solid composite ferric sulfate polymer.Total iron content is 14% in this product, and basicity is greater than 8～14%, and product appearance is soil Red or khaki color powder or block.
Embodiment 2
With 600kg sulfate cinder, 300kg water and 700kg concentration is that 92.5～98% the vitriol oil is put into reactor, heating is also stirred, temperature of reaction is controlled at 120 ± 5 ℃, pressure 0.3 ± 0.05MPa, keep this reaction conditions, reaction was carried out 4.0 hours, added additive yellow soda ash 100kg and lime carbonate 40kg, reacted 40 minutes, cooling reduces system temperature below 80 ℃ then again; Blowing goes into to solidify in the mummification reaction tank, and after mummification in 2 hours, crushing packing promptly gets solid composite ferric sulfate polymer.Total iron content is 12% in this product, and basicity is greater than 9～13%, and product appearance is soil Red or khaki color powder or block.
Embodiment 3
With 850kg sulfate cinder, 580kg water and 750kg concentration is that 92.5～98% the vitriol oil is put into reactor, heating is also stirred, temperature of reaction is controlled at 130 ± 5 ℃, pressure 0.3 ± 0.05MPa, keep this reaction conditions, reaction was carried out 3.5 hours, added additive aluminum oxide 50kg, sodium aluminate 20kg and lime carbonate 50kg, reacted 30 minutes, cooling reduces system temperature below 80 ℃ then again; Reactant put into solidifies the mummification reaction tank, through 4～5 hours expanded, solidify mummification after, crushing packing promptly gets product.Total iron content is 14% in this product, and basicity is greater than 8～14%, and product appearance is soil Red or khaki color powder or block.
Embodiment 4
With 900kg sulfate cinder, 600kg water and 800kg concentration is that 92.5～98% the vitriol oil is put into reactor, heating is also stirred, temperature of reaction is controlled at 145 ± 5 ℃, pressure 0.4 ± 0.05MPa, keep this reaction conditions, reaction was carried out 5.0 hours, added additive 160kg magnesium chloride and 20kg sodium aluminate, reacted 60 minutes, cooling reduces system temperature below 80 ℃ then again; Reactant put into solidify the mummification reaction tank, after mummification in 6 hours, crushing packing promptly gets solid composite ferric sulfate polymer.Total iron content is 14% in this product, and basicity is greater than 8～14%, and product appearance is soil Red or khaki color powder or block.
As mentioned above, can realize the present invention preferably.
Claims (8)
1, a kind of solid composite ferric sulfate polymer production method comprises following processing step:
The water of the sulfate cinder of 600～900 parts of weight, 300～800 parts of weight and the vitriol oil of 600～800 parts of weight are put into reactor, heating is also stirred, temperature of reaction is controlled at 100～150 ℃, reactor pressure is controlled at≤0.5MPa, after reaction is carried out 3.0～5.0 hours, in calcium oxide, lime carbonate, yellow soda ash, aluminum oxide, aluminate or the magnesium salts of 100～180 parts of weight of adding one or more are as additive, continue reaction 20～60 minutes, be cooled to below 80 ℃ the back expanded, solidify, mummification, pulverize, get finished product.
2, production method according to claim 1 is characterized in that: described sulfate cinder contains Fe
2O
3, Fe
3O
4, the oxide compound of silicon or silicate.
3, production method according to claim 1 is characterized in that: iron-holder is 30～65% in the described sulfate cinder.
4, production method according to claim 1 is characterized in that: according to chemical equation Fe
2O
3+ 3H
2SO
4=Fe
2(SO
4)
3+ 3H
2O just with sulfate cinder in the iron complete reaction time needed vitriolic amount of substance be B, it is actual that to add the vitriolic amount of substance be 105%～120%B.
5, production method according to claim 4 is characterized in that: actual adding vitriolic amount of substance is 105%～110%B.
6, production method according to claim 1 is characterized in that: the described vitriol oil is that mass concentration is 98% the vitriol oil or 92.5% the vitriol oil.
7, production method according to claim 1 is characterized in that: the temperature that sulfuric acid adds the post-heating that finishes is controlled at 120 ± 5 ℃.
8, production method according to claim 1 is characterized in that: the time of described mummification is 2～12 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100375516A CN100335420C (en) | 2005-09-27 | 2005-09-27 | Production process of solid composite ferric sulfate polymer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100375516A CN100335420C (en) | 2005-09-27 | 2005-09-27 | Production process of solid composite ferric sulfate polymer |
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|---|---|
| CN1772642A CN1772642A (en) | 2006-05-17 |
| CN100335420C true CN100335420C (en) | 2007-09-05 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544407B (en) * | 2008-03-24 | 2011-07-13 | 中南大学 | Method for preparing solid polyferric sulfate by swelling and solidifying methods |
| CN102718268B (en) * | 2012-06-12 | 2014-01-01 | 河南师范大学 | Method for producing solid poly ferric sulfate |
| CN106241889B (en) * | 2016-08-10 | 2018-07-24 | 浙江合众环保科技有限公司 | A kind of preparation method of solid sulphuric acid iron |
| CN107200388A (en) * | 2017-07-20 | 2017-09-26 | 许伟琦 | The sewage-treating agent of a variety of sewage can be handled with deodorizing effect |
| CN108751280B (en) * | 2018-06-06 | 2021-12-10 | 四川科尔瑞环保科技有限责任公司 | Solid iron-magnesium composite phosphorus removal agent and preparation method thereof |
| CN108751369B (en) * | 2018-06-08 | 2021-03-26 | 高密博宇环保科技有限公司 | Production method of polymeric ferric sulfate |
| CN111320355A (en) * | 2019-11-21 | 2020-06-23 | 佛山科学技术学院 | Preparation method of efficient flocculant for sludge dewatering |
| CN111874967A (en) * | 2020-07-17 | 2020-11-03 | 仇建芳 | Efficient phosphorus removal agent for removing phosphorus from sewage |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE451999B (en) * | 1983-09-08 | 1987-11-09 | Stora Kopparbergs Bergslags Ab | Ferric sulphate prodn. |
| CN1043297A (en) * | 1990-01-09 | 1990-06-27 | 谭正洪 | Technology for making polyiron sulfate |
| CN1052293A (en) * | 1989-12-06 | 1991-06-19 | 北京科技大学 | The quick production method of bodied ferric sulfate |
| JPH11278849A (en) * | 1998-03-31 | 1999-10-12 | Nittetsu Mining Co Ltd | Method for producing ferric polysulfate solution and device for executing the method |
-
2005
- 2005-09-27 CN CNB2005100375516A patent/CN100335420C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE451999B (en) * | 1983-09-08 | 1987-11-09 | Stora Kopparbergs Bergslags Ab | Ferric sulphate prodn. |
| CN1052293A (en) * | 1989-12-06 | 1991-06-19 | 北京科技大学 | The quick production method of bodied ferric sulfate |
| CN1043297A (en) * | 1990-01-09 | 1990-06-27 | 谭正洪 | Technology for making polyiron sulfate |
| JPH11278849A (en) * | 1998-03-31 | 1999-10-12 | Nittetsu Mining Co Ltd | Method for producing ferric polysulfate solution and device for executing the method |
Non-Patent Citations (1)
| Title |
|---|
| 利用硫铁矿烧渣研制聚铁混凝剂 宁寻安等，中国给水排水，第19卷第5期 2003 * |
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