CN105217754A - A kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant - Google Patents
A kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant Download PDFInfo
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- CN105217754A CN105217754A CN201510628423.2A CN201510628423A CN105217754A CN 105217754 A CN105217754 A CN 105217754A CN 201510628423 A CN201510628423 A CN 201510628423A CN 105217754 A CN105217754 A CN 105217754A
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Abstract
The present invention relates to a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant, comprise step: Aluminiferous waste slag is acid-soluble, heavy metals removal, preparation is containing aluminium liquid; Prepare inorganic type compound coagulant; Prepare Inorganic whisker coagulating agent.The invention has the beneficial effects as follows: raw material sources are extensive, low production cost, quality product is excellent, production process environmental protection.
Description
Technical field
The present invention relates to a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant, belong to solidification disposal of waste, resource regeneration, technical field of developing a circular economy.
Background technology
Hydrochloric acid can be used in the process of ferro-aluminum metallic surface processing and carry out cleanup acid treatment, produce a large amount of spent pickle liquors, because these waste liquids do not have suitable utilization ways, these spent pickle liquors are often taken as waste water and process, the body refuse produced also directly carries out landfill, not only consume a large amount of manpower and financial resources, and occupy limited land resources.
In aluminium shape surface spent pickle liquor aluminium content and acidity relatively low, without the value directly utilized, general enterprises takes the treatment process adding alkali neutralization precipitation, discharged wastewater met the national standard after neutralization or enter subsequent treatment process, precipitation enters the concentrated rear filter-press dehydration of concentration basin, and the Aluminiferous waste slag after dehydration directly carries out landfill.By carrying out index of correlation detection to the waste residue after the spent pickle liquor process of multiple aluminium section bar processing enterprises, detected result shows: in waste residue, aluminium exists mainly with gel state aluminium hydroxide, possesses good acid-soluble, under normal pressure acid adding condition, just can dissolve completely, possess the value of recycling.Iron and steel pickling waste liquid divides two kinds: the waste liquid adopting chlorohydric acid pickling to obtain and the waste liquid adopting sulfuric acid washing to obtain.What relate to herein is hydrochloric acid type iron and steel pickling waste liquid, its main component Fe
2o
3% (Fe
3+) content is 0.5% ~ 3.0%, Fe
2o
3% (Fe
2+) content is 5 ~ 19%, HCl%>=2%, possesses the feasibility directly utilized.
Inorganic type flocculation agent is the conventional medicament in industrial sewage, process water and drinking water treatment process.The flocculation agent that market generally uses mainly contains the large class of aluminium system and iron system two, and poly aluminium chloride and poly-iron chloride are Typical Representative wherein respectively, and the two has different flocculating properties.Poly aluminium chloride hydrolysis is weak, alumen ustum is little, loose, sedimentation slow and residual Al has detrimentally affect to HUMAN HEALTH, but remaining colourity is little; Poly-iron chloride hydrolysis is strong, flco is large, closely knit, sedimentation fast, but remaining colourity is large.And the two is made composite coagulant product poly aluminium chloride iron rule and can overcome the two defect in use, not only can accelerate floc settling velocity, and can effluent color dilution be reduced.We add quaternary organic cation type polymeric colloid in the poly aluminium chloride iron product of preparation simultaneously, obtain more efficient Inorganic whisker coagulating agent product.
The angle that the present invention utilizes from solid wastes recycling, utilizing aluminum profile industry Aluminiferous waste slag and iron and steel pickling waste liquid compared with preparing the polychloride ferro-aluminum of composite coagulant product under mild conditions, adding quaternary organic cation type polymeric colloid simultaneously on this basis and carrying out synergy.Not only there is actual application value, and there is the double benefit of economy and environment.
Summary of the invention
The technical problem to be solved in the present invention is: based on the problems referred to above, the invention provides a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant.
The present invention solves the technical scheme that its technical problem adopts: a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant, comprises the following steps:
(1) acid-soluble, the heavy metals removal of Aluminiferous waste slag, preparation is containing aluminium liquid: technical hydrochloric acid, Aluminiferous waste slag are added in pre-molten still, stirring at normal temperature, adds heavy metal chelating agent, stirs, filter press, obtains faint yellow clarification containing aluminium liquid;
(2) inorganic type compound coagulant is prepared: will add in reactor containing aluminium liquid, steel surface spent pickle liquor, and add oxygenant, normal-temperature reaction 15 ~ 30 minutes, add calcium aluminate powder, 95 ~ 105 DEG C of reaction 1 ~ 2h, cooling press filtration, obtains inorganic type compound coagulant;
(3) prepare Inorganic whisker coagulating agent: add in mixing kettle by quaternary organic cation type polymeric colloid, inorganic type compound coagulant, stir, obtain Inorganic whisker coagulating agent.
Further, Aluminiferous waste slag is the semi-solid material of the canescence that obtains of aluminium shape surface spent pickle liquor process or white in step (1), and main component is Al (OH)
3, aluminium content is with Al
2o
3count 10 ~ 50%, technical hydrochloric acid dosage is 60 ~ 250% of waste residue amount, and heavy metal chelating agent is Sodium Dimethyldithiocarbamate, and dosage is 0.1% of solution total mass in pre-molten still, containing aluminium content in aluminium liquid with Al
2o
3meter>=4%, pH>=2.
Further, add service water in reaction process in step (1), service water dosage is 50 ~ 400% of Aluminiferous waste slag quality.
Further, in step (2), steel surface spent pickle liquor is blue-greenish colour clear liquid, and main component is Fe
3+, Fe
2+and HCl, wherein Fe
3+content is with Fe
2o
3count 0.5 ~ 3%, Fe
2+content is with Fe
2o
3count 5 ~ 19%, HCl content>=2%, the dosage of steel surface spent pickle liquor is containing aluminium liquid quality 13 ~ 25%.
Further, in step (2), oxygenant is technical grade sodium chlorate, and oxygenant dosage is 1 ~ 3% of steel surface spent pickle liquor quality; Calcium aluminate powder aluminium content is with Al
2o
3% counts 47 ~ 56%, and the dosage of calcium aluminate powder is containing aluminium liquid and steel surface spent pickle liquor quality summation 12 ~ 20%.
Further, add service water in step (2) in reaction process, service water dosage is containing aluminium liquid quality 10 ~ 25%.
Further, in step (3), quaternary organic cation type polymeric colloid is the one in Poly Dimethyl Diallyl Ammonium Chloride, polymethyl acyloxyethyl trimethyl ammonium chloride, polyacrylamide oxy-ethyl-trimethyl salmiac, and the dosage of quaternary organic cation type polymeric colloid is 1 ~ 3% of Inorganic complex coagulant quality.
Further, the Inorganic whisker coagulating agent obtained in step (3) is sorrel clarified liq, and wherein aluminium content is with Al
2o
3meter>=10%, Fe
3+content is with Fe
2o
3count 0.5 ~ 2%, Fe
2+content is with Fe
2o
3meter≤0.2%, basicity is 40 ~ 90%.
The invention has the beneficial effects as follows: raw material sources are extensive: ferro-aluminum surface working industry distribution is extensive, produces a large amount of spent acid waste residues, for industrialization of the present invention provides abundant raw material sources;
Low production cost: the Aluminiferous waste slag that the present invention adopts and iron ion bearing scrap acid solution are waste material, with low cost; Not only oxidation efficiency is high as oxygenant to adopt sodium chlorate, wide material sources and with low cost;
Quality product is excellent: the compound coagulant product obtained by this technique is sorrel liquid, and constant product quality, has the advantage of aluminium system and Iron-based product concurrently, can be widely used in the process of all kinds of sewage;
Production process environmental protection: this product, from raw material, to producing, arrives the equal energy-conserving and environment-protective of the whole process of application.Raw material is waste material, and production process utilizes reaction heat to complete at ambient pressure, and the product produced may be used for sewage purification again.Meet national energy-saving to reduce discharging, the guiding theory of developing a circular economy.
Embodiment
The invention will be further described in conjunction with specific embodiments now, and following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
In pre-molten still, add technical hydrochloric acid 70kg, service water 50kg, normal temperature starts stirring, and (aluminium content is with Al to add Aluminiferous waste slag
2o
3count 15%) 80kg, add heavy metal chelating agent 0.2kg, filter press obtains faint yellow clarification containing aluminium liquid.Be 200kg containing aluminium liquid, aluminium content is with Al
2o
3counting 6.0%, pH is 2.5.
Joining in reactor containing aluminium liquid 200kg, service water 40kg and steel surface spent pickle liquor 30kg, waste hydrochloric acid containing iron index is: Fe
3+content is with Fe
2o
3count 1.5%, Fe
2+content is with Fe
2o
3count 6%, HCl content is 10%, add oxygenant 0.4kg, normal temperature oxidation reacts 30 minutes, and (aluminium content is with Al to add calcium aluminate powder 38kg
2o
3count 50.13%), 95 DEG C of hydrolytic-polymeric reaction 1h, cooling press filtration obtains inorganic type compound coagulant 308.4kg.
Add inorganic type compound coagulant in quaternary organic cation type polymeric colloid Poly Dimethyl Diallyl Ammonium Chloride 3.09kg and reactor stirs composite in mixing kettle, obtains finally required coagulating agent product 311.49kg.
In coagulating agent product, aluminium content is with Al
2o
3count 10.07%, Fe
3+content is with Fe
2o
3count 0.72%, Fe
2+content is with Fe
2o
3count 0.01%, basicity is 77.98%.
Embodiment 2
In pre-molten still, add technical hydrochloric acid 115kg, service water 77kg, normal temperature starts stirring, and (aluminium content is with Al to add Aluminiferous waste slag
2o
3count 18.05%) 108kg, add heavy metal chelating agent 0.3kg, filter press obtains faint yellow clarification containing aluminium liquid.Be 300kg containing aluminium liquid, aluminium content is with Al
2o
3counting 6.5%, pH is 2.3.
Joining in reactor containing aluminium liquid 300kg, service water 30kg and steel surface spent pickle liquor 60kg, waste hydrochloric acid containing iron index is: Fe
3+content is with Fe
2o
3count 1.2%, Fe
2+content is with Fe
2o
3count 8%, HCl content is 8%, add oxygenant 1kg, normal temperature oxidation reacts 30 minutes, and (aluminium content is with Al to add calcium aluminate powder 50kg
2o
3count 52.22%), 105 DEG C of hydrolytic-polymeric reaction 2h, cooling press filtration obtains inorganic type compound coagulant 441kg.
Add inorganic type compound coagulant in quaternary organic cation type polymeric colloid polymethyl acyloxyethyl trimethyl ammonium chloride 8.82kg and reactor stirs composite in mixing kettle, obtains finally required coagulating agent product 449.82kg.
In coagulating agent product, aluminium content is with Al
2o
3count 10.34%, Fe
3+content is with Fe
2o
3count 1.17%, Fe
2+content is with Fe
2o
3count 0.09%, basicity is 70.89%.
Embodiment 3
In pre-molten still, add technical hydrochloric acid 82kg, service water 133.5kg, normal temperature starts stirring, and (aluminium content is with Al to add Aluminiferous waste slag
2o
3count 39.89%) 34.5kg, add heavy metal chelating agent 0.25kg, filter press obtains faint yellow clarification containing aluminium liquid.Be 250kg containing aluminium liquid, aluminium content is with Al
2o
3counting 5.5%, pH is 2.2.
Joining in reactor containing aluminium liquid 250kg, service water 30kg and steel surface spent pickle liquor 60kg, waste hydrochloric acid containing iron index is: Fe
3+content is with Fe
2o
3count 1.2%, Fe
2+content is with Fe
2o
3count 11%, HCl content is 6%, add oxygenant 1.45kg, normal temperature oxidation reacts 30 minutes, and (aluminium content is with Al to add calcium aluminate powder 52kg
2o
3count 49.82%), 105 DEG C of hydrolytic-polymeric reaction 2h, cooling press filtration obtains inorganic type compound coagulant 393.45kg.
Add inorganic type compound coagulant in quaternary organic cation type polymeric colloid polyacrylamide oxy-ethyl-trimethyl salmiac 11.81kg and reactor stirs composite in mixing kettle, obtains finally required coagulating agent product 405.26kg.
In coagulating agent product, aluminium content is with Al
2o
3count 10.08%, Fe
3+content is with Fe
2o
3count 1.81%, Fe
2+content is with Fe
2o
3count 0.05%, basicity is 84.01%.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to right.
Claims (8)
1. fully utilize the method that compound coagulant prepared by ferro-aluminum surface acid-washing spent acid waste residue, it is characterized in that: comprise the following steps:
(1) acid-soluble, the heavy metals removal of Aluminiferous waste slag, preparation is containing aluminium liquid: technical hydrochloric acid, Aluminiferous waste slag are added in pre-molten still, stirring at normal temperature, adds heavy metal chelating agent, stirs, filter press, obtains faint yellow clarification containing aluminium liquid;
(2) inorganic type compound coagulant is prepared: will add in reactor containing aluminium liquid, steel surface spent pickle liquor, and add oxygenant, normal-temperature reaction 15 ~ 30 minutes, add calcium aluminate powder, 95 ~ 105 DEG C of reaction 1 ~ 2h, cooling press filtration, obtains inorganic type compound coagulant;
(3) prepare Inorganic whisker coagulating agent: add in mixing kettle by quaternary organic cation type polymeric colloid, inorganic type compound coagulant, stir, obtain Inorganic whisker coagulating agent.
2. a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant according to claim 1, it is characterized in that: Aluminiferous waste slag is the semi-solid material of the canescence that obtains of aluminium shape surface spent pickle liquor process or white in described step (1), and main component is Al (OH)
3, aluminium content is with Al
2o
3count 10 ~ 50%, technical hydrochloric acid dosage is 60 ~ 250% of waste residue amount, and heavy metal chelating agent is Sodium Dimethyldithiocarbamate, and dosage is 0.1% of solution total mass in pre-molten still, containing aluminium content in aluminium liquid with Al
2o
3meter>=4%, pH>=2.
3. a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant according to claim 1, it is characterized in that: add service water in reaction process in described step (1), service water dosage is 50 ~ 400% of Aluminiferous waste slag quality.
4. a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant according to claim 1, is characterized in that: in described step (2), steel surface spent pickle liquor is blue-greenish colour clear liquid, and main component is Fe
3+, Fe
2+and HCl, wherein Fe
3+content is with Fe
2o
3count 0.5 ~ 3%, Fe
2+content is with Fe
2o
3count 5 ~ 19%, HCl content>=2%, the dosage of steel surface spent pickle liquor is containing aluminium liquid quality 13 ~ 25%.
5. a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant according to claim 1, it is characterized in that: in described step (2), oxygenant is technical grade sodium chlorate, and oxygenant dosage is 1 ~ 3% of steel surface spent pickle liquor quality; Calcium aluminate powder aluminium content is with Al
2o
3% counts 47 ~ 56%, and the dosage of calcium aluminate powder is containing aluminium liquid and steel surface spent pickle liquor quality summation 12 ~ 20%.
6. a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant according to claim 1, it is characterized in that: add service water in reaction process in described step (2), service water dosage is containing aluminium liquid quality 10 ~ 25%.
7. a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant according to claim 1, it is characterized in that: in described step (3), quaternary organic cation type polymeric colloid is the one in Poly Dimethyl Diallyl Ammonium Chloride, polymethyl acyloxyethyl trimethyl ammonium chloride, polyacrylamide oxy-ethyl-trimethyl salmiac, and the dosage of quaternary organic cation type polymeric colloid is 1 ~ 3% of Inorganic complex coagulant quality.
8. a kind of method fully utilizing ferro-aluminum surface acid-washing spent acid waste residue and prepare compound coagulant according to claim 1, it is characterized in that: the Inorganic whisker coagulating agent obtained in described step (3) is sorrel clarified liq, and wherein aluminium content is with Al
2o
3meter>=10%, Fe
3+content is with Fe
2o
3count 0.5 ~ 2%, Fe
2+content is with Fe
2o
3meter≤0.2%, basicity is 40 ~ 90%.
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| CN105776465A (en) * | 2016-03-04 | 2016-07-20 | 江苏永葆环保科技股份有限公司 | Composite coagulant used for treating printing and dyeing waste water and preparing method thereof |
| CN105883946A (en) * | 2016-06-22 | 2016-08-24 | 南京永禾环保工程有限公司 | Compound water purifying agent for deep treatment of chemimechanical pulp effluents and preparation method of compound water purifying agent for deep treatment of chemimechanical pulp effluents |
| CN107697998A (en) * | 2017-10-27 | 2018-02-16 | 安徽工业大学 | One kind is based on Al3+The hasty and careless black digestion liquid preprocess method of rice paper of endogenous flocculation |
| CN108408960A (en) * | 2018-03-08 | 2018-08-17 | 湖南大学 | A method of liquid is scrapped in the iron-containing pickling of recovery processing |
| CN109970110A (en) * | 2019-03-26 | 2019-07-05 | 岳阳林纸股份有限公司 | A kind of preparation method of HCA-PAC composite water disposal agent |
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| CN105776465A (en) * | 2016-03-04 | 2016-07-20 | 江苏永葆环保科技股份有限公司 | Composite coagulant used for treating printing and dyeing waste water and preparing method thereof |
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| CN108408960A (en) * | 2018-03-08 | 2018-08-17 | 湖南大学 | A method of liquid is scrapped in the iron-containing pickling of recovery processing |
| CN109970110A (en) * | 2019-03-26 | 2019-07-05 | 岳阳林纸股份有限公司 | A kind of preparation method of HCA-PAC composite water disposal agent |
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Application publication date: 20160106 |