CN1121488A - Decolor coagulant for waste water in dyeing industry and producing method - Google Patents
Decolor coagulant for waste water in dyeing industry and producing method Download PDFInfo
- Publication number
- CN1121488A CN1121488A CN 94111581 CN94111581A CN1121488A CN 1121488 A CN1121488 A CN 1121488A CN 94111581 CN94111581 CN 94111581 CN 94111581 A CN94111581 A CN 94111581A CN 1121488 A CN1121488 A CN 1121488A
- Authority
- CN
- China
- Prior art keywords
- coagulating agent
- waste water
- feso
- grog
- dense
- 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
- 239000000701 coagulant Substances 0.000 title claims abstract description 34
- 239000002351 wastewater Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000004043 dyeing Methods 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000011575 calcium Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 150000002681 magnesium compounds Chemical class 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract description 6
- 239000011790 ferrous sulphate Substances 0.000 abstract description 4
- 235000003891 ferrous sulphate Nutrition 0.000 abstract description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 abstract description 4
- 239000013049 sediment Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001448 ferrous ion Inorganic materials 0.000 abstract description 2
- 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 abstract description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 abstract description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 abstract 1
- 230000032683 aging Effects 0.000 abstract 1
- 229910001447 ferric ion Inorganic materials 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 21
- 239000000047 product Substances 0.000 description 14
- 239000000975 dye Substances 0.000 description 12
- 238000004042 decolorization Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 150000002505 iron Chemical class 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000000984 vat dye Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The coagulating agent uses ferric sulfate and ferrous sulfate as main components, the molar ratio of ferric and ferrous ions approximates to 1. The product features wide range of decolouring and strong adaptability. The dosage of chemical for treating dyeing waste water is small, the decolouring rate is high, the produced sediment being sturdy, quick precepitating speed, norecolouring, product being solid, convenient for storage, transportation and application. In the production, there are only dewatering oxidation, acidifying and ageing three steps, so that it features simple process, low cost and without "three wastes".
Description
The present invention relates to a kind of water conditioner, particularly coagulating agent and the production method thereof that dyeing waste water is decoloured and handles.
Decolor coagulant for waste water in dyeing industry that contains trivalent iron salt or ferrous salt such as ferrous sulfate (FeSO commonly used at present
47H
2O), polyiron sulfate (PFS) etc., processing to dyeing waste water, there is the decolouring narrow range, the mal-condition that incompatibility water quality is changeable, the precipitation that is produced is fluffy, settling velocity waits shortcoming slowly, as PFS the waste water that contains reactive dyestuffs is not almost had decolorizing effect, though ferrous sulfate has decolorizing effect to the waste water that contains reactive dyestuffs, but consumption is big, and alumen ustum is fluffy and easily return look; The production of coagulating agent, main " wet method " production technique that adopts, its energy consumption is big, the cost height, and have " three wastes " to produce.
The objective of the invention is to adopt " dry method " production technique, produce the decolouring coagulating agent of a kind of iron content and ferrous salt, its wide ranges of decolouring, adaptability is strong.
Coagulating agent of the present invention, product are light grey powdered solid, and good water solubility mainly contains (weight percentage):
FeSO
4·H
2O 25～33％
Fe
2(SO
4)
3·8H
2O 44～54％
MgSO
4·2H
2O 8～15％
CaSO
4·2H
2O 2～4％
H
2SO
4 5～15％
That a main decolorization is divalent iron salt and trivalent iron salt, wherein Fe in the coagulating agent
3+/ Fe
2+Ratio be the main quality index of product, have only Fe
3+/ Fe
2+(mol ratio) is 0.8～1.2 o'clock, just has the characteristics of decolouring wide ranges, and the ideal ratio is 1.Ca in the product, Mg plasma play a part to improve decolorizing effect, H
2SO
4Then can play neutralizing effect to the strong basicity dyestuff.
If adopt the industrial goods raw material, then also have a spot of ash in the product, be mainly SiO
2Deng impurity, add that the product water absorbability is strong, also have 1.5～4% hygroscopic water, product is the mixture that inorganic salt are formed, and is nontoxic, tasteless, not flammable.
The production method of coagulating agent of the present invention is as follows: with FeSO
47H
2O is a main raw material, and the oxide compound of magnesium, calcium or oxyhydroxide are auxiliary material, and the oxidation 50～150 minutes of dewatering under 160～250 ℃ of temperature after mixing obtains Fe
3+/ Fe
2+(mol ratio) is 0.8～1.2 qualified grog, adds dense H
2SO
4Acidifying, slaking just gets product more than 24 hours then.
The charge ratio of raw material percentage composition by weight is calculated as: 83～96%FeSO
47H
2O, 3～12% magnesium compounds, 1～4% calcium cpd; Auxiliary material can be MgO and Ca (OH)
2, at this moment preferable raw material charge ratio percentage composition by weight is calculated as: 92～96%FeSO
47H
2O, 3～5%MgO, 1～3%Ca (OH)
2
Under the certain situation of the charge ratio of raw material, the temperature and time of decolouring oxidation is determining the quality of product, and temperature is if be lower than 160 ℃, and the dehydration oxidation is insufficient, if be higher than 300 ℃, SO
4 2-Can decompose, soaking time, i.e. the length of the time of oxidation is product quality indicator Fe
3+/ Fe
2+The major influence factors of mol ratio can be by measuring the Fe in the grog
3+/ Fe
2+Mol ratio decides oxidization time, if drop between 0.8～1.2, then is qualified grog, can carry out subsequent step, if less than 0.8, needs to prolong oxidization time, if surpass 1.2, then soaking time is long.Under above-mentioned charge ratio situation, the heated oxide temperature is with 180～200 ℃, and the time is to be advisable Fe in 60～90 minutes
3+/ Fe
2+Mol ratio is 1 o'clock the best.
The vitriol oil that is added during acidifying is 2.3～2.7 better with the weight ratio of the grog and the vitriol oil, the amount of grog is meant that qualified grog is through grinding and cross the amount of the grog of 80 mesh sieves, the vitriol oil that this step added is excessive, make and contain a certain amount of free acid in the product, so that the strong basicity dyeing waste water is played certain neutralizing effect, make producer when handling waste water, reduce operation steps.
Before the slaking, temperature of charge is reduced to below 100 ℃.
Coagulating agent of the present invention (FT coagulating agent), with ferrous sulfate and ferric sulfate is main component, and the mol ratio of trivalent and ferrous ion makes product have the decolouring wide ranges near 1, adaptable characteristics, be applicable to reactive dyestuffs, dispersed dye, substantive dyestuff, vat dyes, intellectual circle's dyestuff, the Naphthol dyestuff, the decolouring of the matching stain of metallized dye and most of kinds etc. is handled; It is few that product also has a dosage, the percent of decolourization height, and characteristics easy and simple to handle, the sediment that produces in the decolouring treating processes of waste water is solid, and sedimentation speed is fast, does not return look; One ton of need of waste water by the per 100 times of colourities of the colourity of waste water aspect consumption add about 100 grams of medicament, and percent of decolourization reaches more than 95%, and the COD clearance reaches 40～52%, the PH scope 7.5～9 of use, and product is a solid, good water solubility, convenient storage and transportation.
FT coagulating agent of the present invention adopts " dry method " production technique, the oxidation of only dewatering, and acidifying and slaking three big basic steps, technology is simple, and condition is easy to control, and cost is low, and does not have " three wastes " generation in the production process.
Coagulating agent of the present invention compares with the coagulating agent of using always at present, and decolorizing effect is illustrated with following two experiments: experiment one:
In dye solution, measure its residue colourity behind the different coagulants of adding same amount and calculate percent of decolourization, relatively decolorizing effect of different coagulants.
Employed coagulating agent is: 1. FT coagulating agent of the present invention: be mixed with 10% aqueous solution; (2.TA Jiangsu) coagulating agent: 10% aqueous solution; (3.FS Foshan) coagulating agent: 10% aqueous solution; (4.PFS poly-iron) coagulating agent: contain Fe10.1%; 5.PACS contain Al
2O
37%6.Al
2(SO
4)
3Contain Al
2O
37%
Handled waste water is aqueous dye solutions, and it is 600 the aqueous solution that promptly various dyestuffs all are mixed with colourity.
Experimentation is as follows: respectively get a certain amount of aqueous dye solutions (1 liter), the coagulating agent mechanical stirring that adds same amount respectively transferred PH8-8.5 (wherein FS coagulating agent in Foshan need not transferred PH originally as alkalescence) restir to place after 5 minutes with NaOH after 10 minutes.Measure remaining colourimetric number in the solution with visual colorimetry, calculate percent of decolourization.
For cationic dyestuff, every liter of experiment liquid adds 6ml sodium dodecyl sulfate solution (0.2%) earlier and stirred 2 minutes, add a certain amount of coagulating agent again, stir after 10 minutes, transfer PH8-8.5, place a moment, after treating that precipitation fully, get supernatant liquor, measure remaining colourimetric number in the solution, calculate percent of decolourization with visual colorimetry.
Experimental result is as shown in table 1.
Because handled waste water only is dye solution, do not contain other auxiliary agents, so percent of decolourization can be represented the COD clearance.
Experiment two: the test coagulating agent is to the maximum percent of decolourization of dyestuff.
Table 1
Table 2
Table 3
Can find out obviously that from table 3 decolouring coagulating agent of the present invention is handled various decolorization of dyeing, from every indexs such as dosage, sedimentation speed, sediment weights, its decolorizing effect all is better than the former with medicament of factory.
The present invention is further illustrated below by specific embodiment: embodiment 1
1. with 83.3 gram FeSO
47H
2O and 3gMgO and 1gCa (OH)
2Place and grind the alms bowl mill evenly, be placed on to spread out in the Stainless Steel Disc and pave, the about 0.5cm of thickness places baking oven to heat up and heats, and treats that temperature begins air blast when rising to 120 ℃, continues to be warming up to 180～200 ℃, is incubated 90 minutes, takes out grog and analyzes Fe
3+/ Fe
2+Mol ratio be 1: 1;
2. grog was ground 80 mesh sieves, then by grog after sieving and dense H
2SO
42.5 weight ratio mix, grog is placed in the container made of iron, limit enriching H
2SO
4The limit stirs, and at this moment the color of reactant is progressively by the brown canescence that changes into.
When 3. the reactant after the acidifying treats that temperature is reduced to below 100 ℃, containing with evaporating dish and to place slowly slaking in the moisture eliminator, the curing time is 24 hours.
Product after the slaking is the bulk solid, further pulverizes the back with medicament bottled year, adds a cover and seals up for safekeeping.
The detailed process of following examples is all with embodiment 1, and raw material throwing amount and processing condition are listed in table 4:
Table 4
Claims (9)
1, a kind of decolor coagulant for waste water in dyeing industry is characterized in that coagulating agent is light grey powdered solid, mainly contains (weight percentage):
FeSO
4·H
2O 25～33％
Fe
2(SO
4)
3·8H
2O 44～54％
MgSO
4·2H
2O 8～15％
CaSO
4·2H
2O 2～4％
H
2SO
4 5～15％
2, according to the described coagulating agent of claim 1, it is characterized in that the Fe in the said coagulating agent
3+/ Fe
2+Mol ratio be 0.8～1.2.
3, according to the described coagulating agent of claim 1, it is characterized in that the Fe in the said coagulating agent
3+/ Fe
2+Mol ratio be 1.
4, a kind of production method of coagulating agent as claimed in claim 1 is characterized in that with FeSO
47H
2O is a main raw material, and the oxide compound of calcium, magnesium or hydrochloride are auxiliary material, mixes the back 160～250 ℃ of dehydration oxidations 50～150 minutes, obtains Fe
3+/ Fe
2+(mol ratio) is 0.8～1.2 qualified grog, adds dense H
2SO
4Acidifying, slaking is more than 24 hours then, and wherein the raw material charge ratio is (weight percentage): 83～96%FeSO
47H
2O, 3～12% magnesium compounds, 1～4% calcium cpd; Dense H
2SO
4Add-on is: grog/dense H
2SO
4(weight)=2.1～3.3.
5, by the described method of claim 4, it is characterized in that said auxiliary material is MgO and Ca (OH)
2
6,, it is characterized in that said proportioning raw materials is (weight percentage): 92～96%FeSO by power requirement 5 described methods
47H
2O, 3～5%MgO, 1～3%Ca (OH)
2
7, in accordance with the method for claim 4, it is characterized in that said oxidizing temperature is 180～200 ℃.
8, in accordance with the method for claim 4, it is characterized in that said dehydration oxidization time is 60～90 minutes.
9, in accordance with the method for claim 4, it is characterized in that said vitriol oil add-on is: grog/dense H
2SO
4(weight)=2.3～2.7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94111581 CN1075795C (en) | 1994-10-28 | 1994-10-28 | Decolor coagulant for waste water in dyeing industry and producing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94111581 CN1075795C (en) | 1994-10-28 | 1994-10-28 | Decolor coagulant for waste water in dyeing industry and producing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1121488A true CN1121488A (en) | 1996-05-01 |
| CN1075795C CN1075795C (en) | 2001-12-05 |
Family
ID=5035432
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94111581 Expired - Fee Related CN1075795C (en) | 1994-10-28 | 1994-10-28 | Decolor coagulant for waste water in dyeing industry and producing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1075795C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927548A (en) * | 2015-12-30 | 2017-07-07 | 上海丰远环保科技有限公司 | A kind of agent of NEW TYPE OF COMPOSITE decoloration coagulant, preparation method and its discoloration method |
| CN109626732A (en) * | 2018-12-29 | 2019-04-16 | 合肥市东方美捷分子材料技术有限公司 | A kind of mixed lower drip black and odorous water administering method |
| CN114368819A (en) * | 2020-10-14 | 2022-04-19 | 刘耀红 | Sewage decolorant and preparation method thereof |
-
1994
- 1994-10-28 CN CN 94111581 patent/CN1075795C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927548A (en) * | 2015-12-30 | 2017-07-07 | 上海丰远环保科技有限公司 | A kind of agent of NEW TYPE OF COMPOSITE decoloration coagulant, preparation method and its discoloration method |
| CN106927548B (en) * | 2015-12-30 | 2020-10-27 | 上海丰远环保科技有限公司 | Composite decoloring coagulant, preparation method and decoloring method thereof |
| CN109626732A (en) * | 2018-12-29 | 2019-04-16 | 合肥市东方美捷分子材料技术有限公司 | A kind of mixed lower drip black and odorous water administering method |
| CN109626732B (en) * | 2018-12-29 | 2021-11-19 | 合肥市东方美捷分子材料技术有限公司 | Upper-mixing and lower-dropping black and odorous water body treatment method |
| CN114368819A (en) * | 2020-10-14 | 2022-04-19 | 刘耀红 | Sewage decolorant and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1075795C (en) | 2001-12-05 |
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