CN103922448B - A kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black - Google Patents
A kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black Download PDFInfo
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- CN103922448B CN103922448B CN201310011449.3A CN201310011449A CN103922448B CN 103922448 B CN103922448 B CN 103922448B CN 201310011449 A CN201310011449 A CN 201310011449A CN 103922448 B CN103922448 B CN 103922448B
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Abstract
The invention discloses a kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black, belong to red mud resource utilization field; Technical problem to be solved for providing a kind of starting material easily to obtain, can be mass-produced and the low method preparing red mud Quito unit flocculation agent coproduction composite white carbon black of cost; The technical scheme adopted is: the first step, carries out acidleach to red mud; Second step, is mixed with polymeric ferric aluminum inorganic flocculating agent by pickling liquor and telogen; 3rd step, mixes polymeric ferric aluminum inorganic flocculating agent with mineral material and macromolecular material, obtained red mud Quito unit flocculation agent; 4th step: the acid leaching residue the first step obtained after dry 2 ~ 12h, obtains composite white carbon black at 150 ~ 600 DEG C.
Description
Technical field
The invention belongs to the technical field of red mud comprehensive utilization.Be specifically related to a kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black.
Background technology
Red mud be from bauxite, extract aluminum oxide after the waste residue that produces, because taking on a red color, therefore be called as red mud more.According to statistics, in the world the red mud that produces every year of aluminum oxide industry more than 7,000 ten thousand tons.And the red mud generation of China in 2009 has just exceeded 3,000 ten thousand tons, and the gesture in increase year by year.The red mud of external alumina producing enterprise was originally mainly filled out sea and was stored up, and in recent years, along with the enhancing of global environmental consciousness, red mud is filled out sea and stored up and prohibited, and building a dam to store up becomes main discharging modes.Alumina producing enterprise of China limits by geographical position, red mud is except being applied to except manufacture of cement on a small quantity for many years, outdoor the building a dam of most wet method is stored up, and this not only takies a large amount of soil, expends more stockyard construction and maintenance cost, and the alkali be present in red mud is to subsurface wastewater infiltration system, cause body of groundwater and soil pollution, the dust that exposed red mud is formed flies upward with the wind, atmosphere pollution, negative impact is caused to the mankind and vegeto-animal existence, worsens ecotope.Research red mud being carried out to comprehensive utilization aspect is imperative.But the comprehensive utilization of red mud is a global problem, at present, China to the comprehensive utilization ratio of red mud less than 4%.Red mud has become an important factor of restriction China Aluminum development, and the comprehensive utilization of red mud is significant for the sustainable development of China and even Aluminum Industry in The World.
For solving the problem, a large amount of Test And Research Works has been carried out both at home and abroad in the comprehensive utilization of red mud, as extracted rare metal scandium (Jiang Pingguo from red mud, Liang Yong, Wang Hongzhen. reclaim rare metal [J] in red mud. Shanghai non-ferrous metal, 2006,1 (27): 36-39), this is feasible technically, but will realize the contradiction that industrialization also exists technology and economy, has effective practicable techniques to be developed.Meng Tiehong etc. utilize red mud to prepare flocculation agent (Meng Tiehong, Hu Zhaoping, Zhu Yunqin. Bayer process red mud modification-gel method prepares aluminium iron polychloride research [J]. inorganic chemicals industry, 2009, (6): 54-56), but due to complex process, cost is higher, still rest on the experimental study stage, do not form technical scale, the series of problems that a large amount of red muds that thoroughly can not solve China's alumina producing generation bring.Yao Keyu has invented a kind of recycling technique (CN1164515) of discarded red mud, from discarded red mud, extract many kinds of substance.Above method solves the problem of environment protection and energy conservation, but there is the deficiencies such as complex process, cost is higher, exploitativeness is poor.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, technical problem to be solved for providing a kind of starting material easily to obtain, can be mass-produced and the low method preparing red mud Quito unit flocculation agent coproduction composite white carbon black of cost.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black, carries out according to the following steps.
The first step, acidleach is carried out to red mud: by red mud and acidic solution ratio be by weight 1: 1 ~ 10 mix after, 1 ~ 6h is stirred at 30 ~ 100 DEG C, suction filtration obtains pickling liquor and acid leaching residue, in described acidic solution, the volumetric molar concentration of H+ is 0.5 ~ 4mol/L, and in described pickling liquor, the conversion of institute's alferric metal ion for the mass percentage of oxide compound is: Al
2o
3, 2 ~ 10%; Fe
2o
3, 2 ~ 10%; Surplus is H
2o and other inevitable foreign ion;
Second step, prepare polymeric ferric aluminum inorganic flocculating agent: after pickling liquor being mixed with telogen, 1 ~ 12h is stirred at 30 ~ 100 DEG C, stop stirring, slaking 6 ~ 24h, obtain polymeric ferric aluminum inorganic flocculating agent, the massfraction ratio that described poly-ferric & aluminum flocculants institute alferric metal ion is converted as oxide compound is: Al
2o
3, 2 ~ 10%; Fe
2o
3, 2 ~ 10%; Surplus is H
2o and other inevitable foreign ion;
3rd step, prepare red mud Quito unit flocculation agent: after being mixed with mineral material and macromolecular material by polymeric ferric aluminum inorganic flocculating agent, at 10 ~ 80 DEG C, stir 0.5 ~ 2h, obtain polynary flocculation agent, described its composition of polynary flocculation agent is mineral material by mass percentage, 3 ~ 10%; Macromolecular material, 1 ~ 10%; Al
2o
3, 2 ~ 10%; Fe
2o
3, 2 ~ 10%; Surplus is H
2o and other inevitable foreign ion;
4th step: prepare composite white carbon black: the acid leaching residue the first step obtained is at 150 ~ 600 DEG C after dry 2 ~ 12h, and the solid obtained is composite white carbon black.
Acidic solution described in the first step or be one or more in hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid.
Telogen described in second step is one or more in sodium hydroxide, calcium aluminate, potassium hydroxide, ammoniacal liquor and sodium aluminate.
Poly-ferric & aluminum flocculants described in second step is the flocculation agent that basicity is greater than 50%.
Mineral material described in 3rd step is one or more in wilkinite, diatomite, sepiolite and attapulgite.
Macromolecular material described in 3rd step or be starch, or be Poly Dimethyl Diallyl Ammonium Chloride, or be polyacrylamide or be Xylo-Mucine.
In composite white carbon black described in 4th step, the mass percentage of silicon-dioxide is greater than 70%.
The present invention compared with prior art has following beneficial effect.
The present invention is to produce the waste residue of aluminum oxide---and red mud, for raw material, prepares polynary flocculation agent and co-producing white carbon black through acidleach, hydrolysis, polymerization, complex reaction, and preparation method is simple, and raw material sources are extensive, are the technique of a kind of economy, energy saving standard.Flocculation agent of the present invention integrates the advantage of aluminium salt and Ferric Salt Flocculants, solve cationic flocculant and anionic flocculant can not stablize the problem coexisted, have the feature of inorganic polymer flocculant and organic polymer coargulator concurrently, there is coenocytism, it is the substitute that poly-aluminium and Polyferric Sulfate are good, of many uses in sewage disposal, having alumen ustum is formed soon, the feature that flco is large and closely knit, the selective adsorption of the polynary flocculation agent of red mud on water-oil interface is distributed with and helps abolish water micro emulsion colloid, particularly suitable for cleaning process oily(waste)water, can be used as assistant agent and emulsion splitter with the use of, reduce the consumption of emulsion splitter, when process condensed oil sewage and dyeing and printing sewage, under the prerequisite not increasing sewage disposal comprehensive cost, increase substantially the flocculating effect of inorganic polymer class flocculation agent, .
Embodiment
Embodiment 1
Add in there-necked flask by 25g red mud and 75ml30% hydrochloric acid, at 100 DEG C, stir 2h, suction filtration obtains pickling liquor and acid leaching residue; 3g calcium aluminate is joined in pickling liquor, at 60 DEG C, stirs 4h, after slaking 24h, obtain poly-ferric & aluminum flocculants; By 4g polyacrylamide, 10g aquation attapulgite, 86g poly-ferric & aluminum flocculants hybrid reaction, obtains polynary flocculation agent after stirring 1h at 50 DEG C; Acid leaching residue dries 6h at 150 DEG C, obtains composite white carbon black.SiO in composite white carbon black
2content is 70.1%; In polynary flocculation agent, the mass percentage of each component is:
Embodiment 2
Add in there-necked flask by 25g red mud, 25ml30% hydrochloric acid and 25ml75% sulfuric acid, at 90 DEG C, stir 2h, suction filtration obtains pickling liquor and acid leaching residue; 60mlNaOH (1M) solution liquid is slowly joined in the pickling liquor of rapid stirring, at 75 DEG C, reacts 2h, after slaking 24h, obtain poly-ferric & aluminum flocculants; By 2g Poly Dimethyl Diallyl Ammonium Chloride, 5g wilkinite, 93g poly-ferric & aluminum flocculants hybrid reaction, obtains polynary flocculation agent after stirring 0.5h at 40 DEG C; Acid leaching residue dries 3h at 200 DEG C, obtains composite white carbon black.SiO in composite white carbon black
2content is 77.5%; In polynary flocculation agent, the mass percentage of each component is:
Embodiment 3
Add in there-necked flask by 25g red mud 75ml75% sulfuric acid, at 80 DEG C, stir 2h, suction filtration obtains pickling liquor and acid leaching residue; 40mlNaOH (1M) solution liquid is slowly joined in the pickling liquor of rapid stirring, at 80 DEG C, reacts 2h, then add 4g calcium aluminate, continue reaction 2h, after slaking 12h, obtain poly-ferric & aluminum flocculants; By 1.5g Xylo-Mucine, 5g sepiolite, 93.5g poly-ferric & aluminum flocculants hybrid reaction, obtains polynary flocculation agent after reacting 0.5h at 50 DEG C; Acid leaching residue dries 2h at 250 DEG C, obtains composite white carbon black.SiO in composite white carbon black
2content is 85.0%; In polynary flocculation agent, the mass percentage of each component is:
Embodiment 4
Add in there-necked flask by 25g red mud and 25ml30% hydrochloric acid, add 25ml75% sulfuric acid at 80 DEG C after stirring 2h, stirring reaction 2h, suction filtration obtains pickling liquor and acid leaching residue; 40mlKOH (1M) solution liquid is slowly joined in the pickling liquor of rapid stirring, at 75 DEG C, stirs 4h, after slaking 12h, obtain poly-ferric & aluminum flocculants; By 2.5g Poly Dimethyl Diallyl Ammonium Chloride, 8g diatomite, 89.5g poly-ferric & aluminum flocculants hybrid reaction, slaking obtains polynary flocculation agent stir 1h at 40 DEG C after; Acid leaching residue dries 4h at 150 DEG C, obtains composite white carbon black.SiO in composite white carbon black
2content is 75.5%; In polynary flocculation agent, the mass percentage of each component is:
Embodiment 5
Add in there-necked flask by 25g red mud and 25ml75% sulfuric acid, stir 2h at 70 DEG C after, add 25ml30% hydrochloric acid, stirring reaction 2h, suction filtration obtains pickling liquor and acid leaching residue; 7g sodium aluminate is added in pickling liquor, at 75 DEG C, reacts 2h, after slaking 24h, obtain poly-ferric & aluminum flocculants; By 5g starch, 8g aquation attapulgite, 87g poly-ferric & aluminum flocculants hybrid reaction, obtains polynary flocculation agent after stirring 0.5h at 40 DEG C; Acid leaching residue dries 2h at 300 DEG C, obtains composite white carbon black.SiO in composite white carbon black
2content is 80.0%; In polynary flocculation agent, the mass percentage of each component is:
Embodiment 6: flocculating properties contrasts
Table 1 is the polynary flocculation agent and technical grade PAC that obtain by embodiment 1 ~ 5 is the result of 1000NTU diatomite Simulated Water to turbidity, and the turbidity removal effect of the flocculation agent utilizing red mud to prepare as seen to diatomite Simulated Water is better than technical grade PAC.
Table 1 uses flocculation agent of the present invention to the treatment effect of diatomite Simulated Water
| Flocculation agent | Flocculation agent addition (mg/L) | Residual turbidity (NTU) |
| Polynary flocculation agent prepared by example 1 | 40 | 5.8 |
| Polynary flocculation agent prepared by example 2 | 40 | 6.7 |
| Polynary flocculation agent prepared by example 3 | 40 | 5.0 |
| Polynary flocculation agent prepared by example 4 | 40 | 6.2 |
| Polynary flocculation agent prepared by example 5 | 40 | 5.5 |
| Comparative example (technical grade PAC) | 40 | 10.0 |
Embodiment 7: composite white carbon black performance
Table 2 is the composite white carbon black prepared of embodiment 2 and embodiment 5 and commercially available reinforced white carbon black results for styrene-butadiene rubber(SBR) reinforcement, the visible composite white carbon black utilizing red mud to prepare has good reinforcing effect to styrene-butadiene rubber(SBR), and its reinforcing effect is close to the effect of commercially available reinforced white carbon black.
Table 2 uses composite white carbon black of the present invention to the reinforcing effect of styrene-butadiene rubber(SBR)
| White carbon black | Stress at definite elongation/MPa | Tensile strength/MPa | Tensile yield/% |
| Composite white carbon black prepared by embodiment 2 | 3.5 | 10.5 | 730 |
| Composite white carbon black prepared by embodiment 5 | 4.2 | 11.8 | 755 |
| Commercially available reinforced white carbon black | 3.8 | 11.3 | 760 |
Claims (5)
1. utilize red mud to prepare a method for polynary flocculation agent coproduction composite white carbon black, it is characterized in that, carry out according to the following steps:
The first step, acidleach is carried out to red mud: by red mud and acidic solution ratio be by weight 1: 1 ~ 10 mix after, at 30 ~ 100 DEG C stir 1 ~ 6h, suction filtration obtains pickling liquor and acid leaching residue, H in described acidic solution
+volumetric molar concentration be 0.5 ~ 4mol/L, in described pickling liquor, the conversion of institute's alferric metal ion for the mass percentage of oxide compound is: Al
2o
3, 2 ~ 10%; Fe
2o
3, 2 ~ 10%; Surplus is H
2o and other inevitable foreign ion;
Second step, prepare polymeric ferric aluminum inorganic flocculating agent: after pickling liquor being mixed with telogen, 1 ~ 12h is stirred at 30 ~ 100 DEG C, stop stirring, slaking 6 ~ 24h, obtain polymeric ferric aluminum inorganic flocculating agent, the mass percentage that described poly-ferric & aluminum flocculants institute alferric metal ion is converted as oxide compound is: Al
2o
3, 2 ~ 10%; Fe
2o
3, 2 ~ 10%; Surplus is H
2o and other inevitable foreign ion;
3rd step, prepare red mud Quito unit flocculation agent: after being mixed with mineral material and macromolecular material by polymeric ferric aluminum inorganic flocculating agent, at 10 ~ 80 DEG C, stir 0.5 ~ 2h, obtain polynary flocculation agent, described its composition of polynary flocculation agent by mass percentage is: mineral material, 3 ~ 10%; Macromolecular material, 1 ~ 10%; Al
2o
3, 2 ~ 10%; Fe
2o
3, 2 ~ 10%; Surplus is H
2o and other inevitable foreign ion;
Described mineral material is one or more in wilkinite, diatomite, sepiolite and attapulgite; Described macromolecular material or be starch, or be Poly Dimethyl Diallyl Ammonium Chloride, or be polyacrylamide or be Xylo-Mucine;
4th step: prepare composite white carbon black: the acid leaching residue the first step obtained is at 150 ~ 600 DEG C after dry 2 ~ 12h, and the solid obtained is composite white carbon black.
2. a kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black as claimed in claim 1, is characterized in that: the acidic solution described in the first step is one or more in hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid.
3. a kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black as claimed in claim 1, is characterized in that: the telogen described in second step is one or more in sodium hydroxide, potassium hydroxide, ammoniacal liquor, calcium aluminate and sodium aluminate.
4. a kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black as claimed in claim 1, is characterized in that: the poly-ferric & aluminum flocculants described in second step is the flocculation agent that basicity is greater than 50%.
5. a kind of method utilizing red mud to prepare polynary flocculation agent coproduction composite white carbon black as claimed in claim 1, is characterized in that: in the composite white carbon black described in the 4th step, the mass percentage of silicon-dioxide is greater than 70%.
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| CN105152194A (en) * | 2015-07-16 | 2015-12-16 | 中国铝业股份有限公司 | Red mud separation and settlement method in alumina production |
| CN106187550B (en) * | 2016-08-02 | 2019-02-22 | 中国地质大学（北京） | A method of siliceous fertilizer is prepared using red mud flocculation agent acid leaching residue |
| CN106241997B (en) * | 2016-09-21 | 2019-08-02 | 百色学院 | The method of rock phosphate in powder-red mud-inulin composite flocculation agent preparation method and processing sewage |
| CN109336236B (en) * | 2018-12-10 | 2021-05-18 | 河南理工大学 | Method for preparing aluminum-iron flocculating agent from red mud |
| 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 |
| CN110194479A (en) * | 2019-06-12 | 2019-09-03 | 北京博雅合众环保科技有限公司 | A method of aluminium polychloride is prepared using red mud |
| CN114853134A (en) * | 2022-03-29 | 2022-08-05 | 中环保水务投资有限公司 | Composite polyaluminum ferric chloride water purifying agent and preparation method thereof |
| CN114853133A (en) * | 2022-03-29 | 2022-08-05 | 中环保水务投资有限公司 | Preparation method of polyaluminum ferric chloride water purifying agent |
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| JPH10309404A (en) * | 1997-05-12 | 1998-11-24 | Kyowa Technos:Kk | Flocculant for phosphoric acid having chitosan as effective component and method for removal of phosphoric acid using the same |
| CN101041450B (en) * | 2006-03-15 | 2011-06-01 | 中国地质大学（北京） | Clean production technique for preparation of aluminium oxide and white carbon black by using high-alumina coal ash |
| CN101885526B (en) * | 2009-05-16 | 2011-12-21 | 兰州大欣水工业有限责任公司 | Ternary composite type flocculant, preparation and application |
| CN103086489A (en) * | 2013-02-07 | 2013-05-08 | 天津水泥工业设计研究院有限公司 | Method for preparing flocculant polyaluminum ferric chloride from red mud |
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