CN104085973B - A kind of preparation method of service water defluorinating agent - Google Patents
A kind of preparation method of service water defluorinating agent Download PDFInfo
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- CN104085973B CN104085973B CN201410327823.5A CN201410327823A CN104085973B CN 104085973 B CN104085973 B CN 104085973B CN 201410327823 A CN201410327823 A CN 201410327823A CN 104085973 B CN104085973 B CN 104085973B
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Abstract
A preparation method for service water defluorinating agent, belongs to fluorochemical in service water and removes technical field.The synthesis material of industry defluorinating agent comprises: vinylformic acid, deionized water, acrylamide, urea, sodium carbonate, ferrous hydroxide, aluminium hydroxide, 10 ~ 30% sodium hydroxide, activated carbon, 10% quadrol, nitrilo, ammonium persulphate, sodium bisulfite, calcium chloride.Prepared by each synthesis material, be polymerized, be mixed with out industrial water fluoridation agent, advantage is, the defluorinating agent fluorine removing rate of preparation is high, and fluorine removing rate is stablized.Especially have good defluorination effect to content of fluoride in water at the low fluorine water of 20 ~ 50mg/L, medicament preparation and technique simple.
Description
Technical field
The invention belongs to fluorochemical in service water and remove technical field, particularly a kind of preparation method of service water defluorinating agent, effectively fluorochemical in removing industrial sewage.
Background technology
Along with environment-friendly type industrial expansion, the utilize trend of industrial system to water resources is that factory effluent is carried out recycle through further advanced treatment (reverse osmosis desalination), to reduce the environmental pollution that wastewater disposition brings.But there is fluoride pollution water system in the industrial production, such as: the turbid ring of continuous casting, the turbid ring of OG etc. of iron and steel enterprise, dirty stifled to causing water treatment system to cause in the advanced treatment process of its discharge water.And in reuse process, expanding the fluoride pollution of water system, this is by the heat exchange efficiency of the normal operation and heat-exchange system that directly affect circulating water system equipment.The present invention be directed to a kind of defluorinating agent production method of fluorine-containing trade effluent, have better defluorination effect to Oil repellent at the industrial sewage of 20-200mg/L.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of service water defluorinating agent, realize the removal of fluorochemical in service water.The preparation method of defluorinating agent is as follows:
Synthesis material: comprising: vinylformic acid, deionized water, acrylamide, urea, sodium carbonate, ferrous hydroxide, aluminium hydroxide, 10 ~ 30% sodium hydroxide, activated carbon, 10% quadrol, nitrilo, ammonium persulphate, sodium bisulfite, calcium chloride.
Preparation method:
One, synthesis material preparation:
1, vinylformic acid iron, vinylformic acid aluminium and sodium acrylate mixed solution preparation:
1. 15 ~ 25 parts of vinylformic acid (CH, are taken
2=CHCOOH) add in neutralizing well.
2., take 30 ~ 45 parts of deionized waters and add in 1# dissolving tank, then add 8 ~ 15 parts of sodium carbonate, stirring and dissolving, wiring solution-forming 1#.
3., take 8 ~ 15 parts of deionized waters and add in 2# dissolving tank, then add 1 ~ 3 part of ferrous hydroxide and 1 ~ 3 part of aluminium hydroxide, stirring and dissolving, wiring solution-forming 2#.
4., by the solution 2# prepared slowly add in neutralizing well, constantly stir simultaneously.
2CH
2＝CHCOOH+Fe(OH)
2→Fe(CH
2CHCOO)
2
3CH
2＝CHCOOH+Al(OH)
3→Al(CH
2CHCOO)
3
5., by the solution 1# prepared slowly add in neutralizing well, constantly stir, a large amount of CO simultaneously
2release.Till being stirred to bubble-free releasing.
CH
2＝CHCOOH+Na
2CO
3→CH
2＝CHCOO-Na+H
2O+CO
2↑
6., solution ph to 9 ~ 11 in neutralizing well are regulated with 10-30% sodium hydroxide solution.
7., add 1 ~ 5 part of activated carbon in neutralizing well, constantly stir and make to mix, stir 50 ~ 90 minutes, leave standstill 15 ~ 30 minutes.
8., with hay tank filter, release clear liquid, leave standstill venting, stand-by.This solution is solution 3#, and its main component is vinylformic acid iron, vinylformic acid aluminium and sodium acrylate mixed solution.
2, acrylamide soln preparation:
Take 35 ~ 45 parts of deionized waters, put into enamel still, add the urea of 20 ~ 30 parts of acrylamides and 1 ~ 5 part respectively.Be heated to 40-48 DEG C, be dissolved as clear liquid completely.This solution is solution 4#.
Two, polymerization process:
1, take 80 ~ 110 parts of solution 3# prepared to mix in the reactor with 50 ~ 70 parts of solution 4#, during mixing, the temperature of solution controls at 18 ~ 30 DEG C.
2, in the first step mixed solution, first add 10% ethylenediamine solution 0.5 ~ 2 part and nitrilo solution 1 ~ 4 part, added-time otherwise stop stirring simultaneously, then add 10% ammonium persulfate solution 0.5 ~ 3 part and 5% sodium sulfite solution 1 ~ 2 part simultaneously, stir.
aFe(CH
2CHCOO)
2+b Al(CH
2CHCOO)
3+cNaCH
2CHCOO+dCH
2＝CHCONH
2→—(C
3H
3O
2-Fe)
2a—(C
3H
3O
2-Al)
3b—(C
3H
3O
2-Na)
c—(C
3H
3O-NH
2)
d—
3, the mixed solution of second step is poured in plastics bag, place 4 ~ 8 hours.Synthesized by the material that goes out be solid colloidal thing, i.e. organic polymer component.
Three, mixing process:
1, organic polymer component and water are hydrolyzed than mix and blend by 2 ~ 5:1000 quality.This solution is solution 5#.
2, calcium chloride and water are compared mix and blend by 200 ~ 300:1000 quality.This solution is solution 6#.
3, solution 5# and solution 6# press 1:1 quality than mix and blend, obtain defluorinating agent.
The defluorinating agent composition that the method is prepared is exactly the mixture of the above-mentioned organic polymer component made and calcium chloride, and organic polymer component and calcium chloride directly do not react, and being mixed in is exactly wherein a kind of activator as in fluorine process
In service water, content of fluoride scope is 20 ~ 200 mg/litre.Defluorinating agent dosage is that in water, content of fluoride quality is 5 ~ 50:1 than scope.After defluorinating agent fully mixes with service water, precipitate more than 30 minutes, in supernatant liquor, fluorochemical clearance is 70 ~ 90%.
Compared with traditional defluorinating agent, aforesaid method tool has the following advantages:
(1) fluorine removing rate is high, and fluorine removing rate is stablized.Especially good defluorination effect is had to content of fluoride in water at the low fluorine water of 20 ~ 50mg/L.
(2) medicament preparation is simple.
(3) treatment process is simple, and traditional settling tank can meet processing requirements.
Embodiment
Embodiment
1,20 grams of vinylformic acid (CH are taken
2=CHCOOH) add in neutralizing well.
2, measure 38ml deionized water to add in 1# dissolving tank, then add 12 grams of sodium carbonate, stirring and dissolving, wiring solution-forming 1#.
3, measure 12ml deionized water to add in 2# dissolving tank, then add 2 grams of ferrous hydroxides and 2 grams of aluminium hydroxides, stirring and dissolving, wiring solution-forming 2#.
4, the solution 2# prepared slowly is added in neutralizing well, constantly stir simultaneously.
5, the solution 1# prepared slowly is added in neutralizing well, constantly stir simultaneously, have a large amount of CO
2release, what can not add is too fast, runs liquid with anti-overflow groove.
6, after solution 1# adds, continue to stir, till making gas all be discarded to bubble-free releasing.
7, the pH value to 10. of the solution in neutralizing well is adjusted with 30% sodium hydroxide solution
8, add 3 grams of activated carbon in neutralizing well, constantly stir and make to mix, stir 50 minutes, leave standstill 20 minutes.
9, filter with hay tank, release clear liquid, leave standstill venting, stand-by.This solution is solution 3#, and its main component is vinylformic acid iron, vinylformic acid aluminium and sodium acrylate mixed solution.
10, measure 40ml deionized water, put into porcelain enamel barrel, add 25 grams of acrylamides, then add the urea of 4 grams, be heated to 43 DEG C.This solution is solution 4#.
11, take the solution 3# that 90g prepared to mix with 60g solution 4#, during mixing, the temperature of solution controls at 28 DEG C.
12, first add 10% ethylenediamine solution 1.5ml and nitrilo solution 3ml, added-time otherwise stop stirring simultaneously, then add 10% ammonium persulfate solution 2.5ml and 5% sodium sulfite solution 2ml simultaneously, stir.
13, mixed solution is poured in plastics bag, to be applied.
14, above-mentioned synthetics and water are hydrolyzed than mix and blend by 3:1000 quality.This solution is solution 5#.
15, calcium chloride and water are compared mix and blend by 250:1000 quality.This solution is solution 6#.
16, solution 5# and solution 6# press 1:1 quality than mix and blend, obtain defluorinating agent.
Claims (1)
1. a preparation method for service water defluorinating agent, is characterized in that: processing step is as follows:
(1) synthesis material preparation:
Prepared by A, vinylformic acid iron, vinylformic acid aluminium and sodium acrylate mixed solution:
Take 15 ~ 25 parts of vinylformic acid CH
2=CHCOOH adds in neutralizing well;
Take 30 ~ 45 parts of deionized waters to add in 1# dissolving tank, then add 8 ~ 15 parts of sodium carbonate, stirring and dissolving, wiring solution-forming 1#;
Take 8 ~ 15 parts of deionized waters to add in 2# dissolving tank, then add 1 ~ 3 part of ferrous hydroxide and 1 ~ 3 part of aluminium hydroxide, stirring and dissolving, wiring solution-forming 2#;
The solution 2# prepared slowly is added in neutralizing well, constantly stirs simultaneously;
2CH
2＝CHCOOH+Fe(OH)
2→Fe(CH
2CHCOO)
2
3CH
2＝CHCOOH+Al(OH)
3→Al(CH
2CHCOO)
3
The solution 1# prepared is added in neutralizing well, constantly stirs, CO simultaneously
2release; Till being stirred to bubble-free releasing;
CH
2＝CHCOOH+Na
2CO
3→CH
2＝CHCOO-Na+H
2O+CO
2↑
Solution ph to 9 ~ 11 in neutralizing well are regulated with 10-30% sodium hydroxide solution;
Add 1 ~ 5 part of activated carbon in neutralizing well, stir and make to mix, stir 50 ~ 90 minutes, leave standstill 15 ~ 30 minutes;
Filter with hay tank, release clear liquid, leave standstill venting, stand-by; This solution is solution 3#, and its composition is vinylformic acid iron, vinylformic acid aluminium and sodium acrylate mixed solution;
Prepared by B, acrylamide soln:
Take 35 ~ 45 parts of deionized waters, put into enamel still, add the urea of 20 ~ 30 parts of acrylamides and 1 ~ 5 part respectively; Be heated to 40-48 DEG C, be dissolved as clear liquid completely; This solution is solution 4#;
(2) be polymerized:
A, take 80 ~ 110 parts of solution 3# prepared and mix in the reactor with 50 ~ 70 parts of solution 4#, during mixing, the temperature of solution controls at 18 ~ 30 DEG C;
B, in the first step mixed solution, first add 10% ethylenediamine solution 0.5 ~ 2 part and nitrilo solution 1 ~ 4 part, added-time otherwise stop stirring simultaneously, then add 10% ammonium persulfate solution 0.5 ~ 3 part and 5% sodium sulfite solution 1 ~ 2 part simultaneously, stir;
aFe(CH
2CHCOO)
2+b Al(CH
2CHCOO)
3+cNaCH
2CHCOO+dCH
2＝CHCONH
2→
—(C
3H
3O
2-Fe)
2a—(C
3H
3O
2-Al)
3b—(C
3H
3O
2-Na)
c—(C
3H
3O-NH
2)
d—
C, the mixed solution of second step is poured in plastics bag, place 4 ~ 8 hours; Synthesized by the material that goes out be solid colloidal thing, i.e. organic polymer component;
(3), mix:
A, organic polymer component and water to be hydrolyzed than mix and blend by 2 ~ 5:1000 quality; This solution is solution 5#;
B, calcium chloride and water are compared mix and blend by 200 ~ 300:1000 quality; This solution is solution 6#;
C, solution 5# compare mix and blend with solution 6# by 1:1 quality; Obtain defluorinating agent.
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| CN104085973B true CN104085973B (en) | 2015-08-26 |
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| CN105198059A (en) * | 2015-10-13 | 2015-12-30 | 桂林市春晓环保科技有限公司 | Water treatment coagulant |
| CN108911091A (en) * | 2018-07-24 | 2018-11-30 | 湖北蓝钴环保科技有限公司 | A kind of compound defluorinating agent and preparation method thereof |
| CN111036167B (en) * | 2019-12-27 | 2020-12-11 | 吉林大学 | Use of boroaluminates as fluorine adsorbents |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS59373A (en) * | 1982-06-25 | 1984-01-05 | Hitachi Plant Eng & Constr Co Ltd | Treatment of fluorine-contg. waste water |
| KR0176744B1 (en) * | 1996-12-30 | 1999-04-01 | 삼성중공업주식회사 | Method for treating warte water containing fluoride isn by an electron beam |
| JP2005177669A (en) * | 2003-12-22 | 2005-07-07 | Tokuyama Corp | Treating method of fluorine-containing waste water |
| CN100488997C (en) * | 2006-12-29 | 2009-05-20 | 陕西科技大学 | Preparing method for fluorine containing copolymer flocculating agent |
| CN101289260B (en) * | 2008-05-28 | 2010-09-29 | 侯玉奇 | System and method for treating fluorine-containing acid wastewater after graphite purification |
| CN101525394A (en) * | 2009-03-19 | 2009-09-09 | 扬州科宇化工有限公司 | Induction system for preparing especially large molecule amphoteric water treatment absorbent |
| CN102516455B (en) * | 2011-12-15 | 2013-09-04 | 东营市诺尔化工有限责任公司 | Multi-polymerization preparation method of flocculant |
| CN103881006B (en) * | 2014-04-01 | 2016-06-29 | 山东宝莫生物化工股份有限公司 | Large arch dam high molecular weight anionic modified polyacrylamide reversed emulsion polymerization |
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Address after: 066326 Du Zhuang Township, Funing County, Qinhuangdao, Hebei Co-patentee after: Shougang Group Co. Ltd. Patentee after: Qinhuangdao Shouqin Metal Material Co., Ltd. Address before: 066326 Du Zhuang Township, Funing County, Qinhuangdao, Hebei Co-patentee before: Capital Iron & Steel General Company Patentee before: Qinhuangdao Shouqin Metal Material Co., Ltd. |
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Effective date of registration: 20190522 Address after: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Patentee after: Shougang Group Co. Ltd. Address before: 066326 Du Zhuang Township, Funing County, Qinhuangdao, Hebei Co-patentee before: Shougang Group Co. Ltd. Patentee before: Qinhuangdao Shouqin Metal Material Co., Ltd. |