CN112093870A - Method for preparing efficient composite flocculant by taking red mud as raw material - Google Patents
Method for preparing efficient composite flocculant by taking red mud as raw material Download PDFInfo
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- CN112093870A CN112093870A CN202010857489.XA CN202010857489A CN112093870A CN 112093870 A CN112093870 A CN 112093870A CN 202010857489 A CN202010857489 A CN 202010857489A CN 112093870 A CN112093870 A CN 112093870A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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Abstract
The invention discloses a method for preparing a high-efficiency composite flocculant by using red mud as a raw material, which relates to the technical field of red mud recovery treatment and utilization, and provides the following scheme aiming at the problem of poor red mud treatment in the prior art, and the method comprises the following steps: s1: adding red mud and hydrochloric acid into a reaction kettle, then carrying out acid leaching in the reaction kettle at the temperature of 60-100 ℃, and then carrying out filter pressing by using a filter press to obtain filtrate and a filter cake; s2: and (5) putting the filter cake into the reaction kettle again in the step S1, adding a sodium hydroxide solution, stirring at the temperature of 80-140 ℃, mixing for a certain time, and performing filter pressing by using a filter press to obtain a sodium silicate solution and residues.
Description
Technical Field
The invention relates to the technical field of red mud recovery treatment and utilization, in particular to a method for preparing a high-efficiency composite flocculant by using red mud as a raw material.
Background
The red mud is waste residue generated when bauxite is leached by strong alkali in the production process of alumina, and is strong alkaline. In recent years, the alumina industry in China is rapidly developed, and the red mud generation amount is large. For example, the conventional Bayer process can produce 0.5-0.6 tons of red mud per 1 ton of alumina, and the alumina yield of Shandong aluminum industry group alone reaches 1000 million tons in 2006.
The red mud contains a large amount of alumina and iron oxide, as well as magnesium, titanium, silicic acid and other substances. The aluminum oxide and the ferric oxide are basic raw materials for producing the polyaluminum chloride and the polyferric chloride, and the magnesium and the titanium are elements which are required to be added for producing the decolorizing flocculant; the silicon dioxide in the red mud is active silicon dioxide which is a raw material for preparing polysilicic acid, the polysilicic acid is the earliest and best non-toxic flocculant, and the polyaluminium chloride, the polyferric chloride and the polysilicic acid are compounded to obtain the high-efficiency composite flocculant with excellent performance, so that the environmental protection problem caused by the red mud is solved, and the water purifying agent with wide adaptability is prepared.
At present, the comprehensive utilization rate of the red mud is less than 20%, the main utilization modes are mainly used for manufacturing low value-added products such as cement, road base materials and various baking-free bricks, and the rest of a large amount of red mud has no effective large-scale industrial treatment method, so that even though some enterprises are developing a method for producing the flocculating agent by using the red mud, the rest of the residues cannot be utilized. And the fertilizer is piled up in large scale by various enterprises, cannot be utilized and causes huge pollution to the environment.
Disclosure of Invention
The invention provides a method for preparing a high-efficiency composite flocculant by using red mud as a raw material, which solves the problem of poor red mud treatment.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a high-efficiency composite flocculant by using red mud as a raw material comprises the following steps:
s1: adding red mud and hydrochloric acid into a reaction kettle, then carrying out acid leaching in the reaction kettle at the temperature of 60-100 ℃, and then carrying out filter pressing by using a filter press to obtain filtrate and a filter cake;
s2: putting the filter cake obtained in the step S1 into the reaction kettle again, adding a sodium hydroxide solution, stirring at the temperature of 80-140 ℃, mixing for a certain time, and performing filter pressing by using a filter press to obtain a sodium silicate solution and residues;
s3: putting the sodium silicate solution obtained in the step S2 into the reaction kettle again, adding hydrochloric acid, adjusting the pH value to 1-4, standing for 1-6 h, and adjusting the pH value to 1-3 to obtain a polysilicic acid solution;
s4: sampling the proportion of Al, Mg, Fe, Si and the like in the solution obtained in the steps S3 and S1, then adding the filtrate obtained in the step S1 into the solution obtained in the step S3, and simultaneously adding a proper amount of Al, Mg and Fe according to needs, so that Al, Mg, Fe and Si form a certain proportion;
s5: in step S4, adding a sodium hydroxide solution, adjusting the pH value to 3-4, and alkalizing with an alkalizer to a degree of alkalization of 0.8-1.2 to obtain the high-efficiency composite flocculant.
Preferably, in step S1, the reaction temperature is 80 to 95 ℃, the pressure is 0.101MPa, and preferably, the reaction temperature is 80 to 90 ℃, and the pressure is 0.11 MPa.
Preferably, in step S1, the red mud is ground to form 1000-2000 mesh powder particles.
Preferably, the concentration of the sodium hydroxide solution in the step S2 is 28-40%, and the reaction temperature is 90-135 ℃.
Preferably, the concentration of the sodium hydroxide solution is 30-36%, and the reaction temperature is 110-130 ℃.
Preferably, the residue obtained in step S2 is washed with acid and alkali again, and then washed clean with clean water to obtain titanium oxide.
Preferably, the concentration of the hydrochloric acid in the step S3 is 1% -5%, the pH value is firstly adjusted to 1-4, the mixture is stood for 2-5 hours, and then the pH value is adjusted to 1-3.
Preferably, the pH value is firstly adjusted to 2-3, the mixture is kept stand for 3-4 hours, and then the pH value is adjusted to 1.5-2.5.
Preferably, aluminum chloride, ferric chloride and magnesium chloride solutions are used for adding Al, Mg and Fe in the step S3.
Preferably, the aluminum chloride, the ferric chloride and the magnesium chloride are all industrial grade magnesium chloride hexahydrate, and the hydrochloric acid is industrial grade hydrochloric acid.
Preferably, the molar ratio of Al, Mg, Fe and Si in step S3 is 9:1:1: 0.3.
Preferably, in step S5, the alkalifying agent is aluminate.
The invention has the beneficial effects that:
1. the high-efficiency composite flocculant prepared by the invention is a water treatment multifunctional polymeric flocculant, and is a product prepared by taking alumina industrial waste red mud and byproduct hydrochloric acid as raw materials and carrying out acid leaching, solid-liquid separation, residue transformation and polymerization. The product integrates the advantages of polysilicic acid, aluminum salt, ferric salt and magnesium salt flocculating agents, has the functions of adsorption bridge and electric neutralization, introduces the decoloring function of magnesium salt, has the characteristics of high molecular polymerization degree and multi-component synergistic effect, has stability and water purification effect far superior to the high-molecular flocculating agents on the current market, can be widely applied to the coagulation process of municipal sewage, industrial wastewater and the like, and has no problems of residual aluminum and high chroma in the treated water.
2. The flocculant prepared by using the industrial solid waste red mud as the raw material has low production cost and high product added value, realizes the full utilization of the red mud, provides a new way for the comprehensive utilization of the red mud, and has good social benefit, economic benefit and environmental benefit.
3. The invention has the advantages of simple process, short flow, low production cost, low investment, good product stability and strong market competitiveness.
4. The high-efficiency composite flocculant prepared by the invention passes coagulation tests of various modes and actual wastewater treatment, and the results show that the product has good flocculation effect, large and solid flocs and short floc settling time.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1:
putting the red mud and hydrochloric acid into a reaction kettle according to the mass ratio of 2:1, carrying out acid leaching reaction at 80 ℃ for 3 hours, carrying out solid-liquid separation by a plate-and-frame filter press, wherein the filtrate is a mixed solution of aluminum chloride, ferric chloride and magnesium chloride, and the filter cake is reserved.
And (3) putting the filter cake into another reaction kettle, adding 30% of sodium hydroxide solution, reacting at 100 ℃ until the filter cake completely reacts to obtain sodium silicate solution, preparing 2% of solution, adjusting the pH value to 3 by using hydrochloric acid, standing for 3 hours to polymerize the solution, adding hydrochloric acid after the polymerization is finished, and adjusting the pH value to 1.5 to obtain the polysilicic acid solution.
Slowly adding polysilicic acid into the mixed solution of the aluminum chloride, the ferric chloride and the magnesium chloride, and stirring, wherein the ratio of Al to Fe to Mg to Si is 9:1:1:0.3, mixing.
And adding 30% of sodium hydroxide into the mixed liquid, adjusting the pH to 4, and adding an alkalizer to enable the alkalization degree to be 0.8-1.2 to obtain the high-efficiency composite flocculant.
Example 2:
putting the red mud and hydrochloric acid into a reaction kettle according to the mass ratio of 1:1, carrying out acid leaching reaction for 3 hours at 90 ℃, carrying out solid-liquid separation by a plate-and-frame filter press, wherein the filtrate is a mixed solution of aluminum chloride, ferric chloride and magnesium chloride, and the filter cake is reserved.
And (3) putting the filter cake into another reaction kettle, adding 32% of sodium hydroxide solution, reacting at 120 ℃ until the filter cake completely reacts to obtain sodium silicate solution, adding water to adjust the solution to be 3% of solution, adjusting the pH value to be 2 by hydrochloric acid, standing for 3.5 hours to polymerize the solution, adding hydrochloric acid after the polymerization is finished, and adjusting the pH value to be 2.5 to obtain the polysilicic acid solution.
Slowly adding polysilicic acid into the mixed solution of the aluminum chloride, the ferric chloride and the magnesium chloride, and stirring, wherein the ratio of Al to Fe to Mg to Si is 9:1:1:0.3, mixing.
And adding 32% of sodium hydroxide into the mixed liquid, adjusting the pH to 4, and adding an alkalizer to enable the alkalization degree to be 0.8-1.2 to obtain the high-efficiency composite flocculant.
Example 3:
putting the red mud and hydrochloric acid into a reaction kettle according to the mass ratio of 1:2, carrying out acid leaching reaction for 4 hours at 110 ℃, carrying out solid-liquid separation by a plate-and-frame filter press, wherein the filtrate is a mixed solution of aluminum chloride, ferric chloride and magnesium chloride, and the filter cake is reserved.
And (3) putting the filter cake into another reaction kettle, adding a 40% sodium hydroxide solution, reacting at 125 ℃ until the filter cake completely reacts to obtain a sodium silicate solution, adding water to prepare a 5% solution, adjusting the pH value to 3 by using hydrochloric acid, standing for 5 hours to polymerize the solution, adding hydrochloric acid after the polymerization is finished, and adjusting the pH value to 2 to obtain the polysilicic acid solution.
Slowly adding polysilicic acid into the mixed solution of the aluminum chloride, the ferric chloride and the magnesium chloride, and stirring, wherein the ratio of Al to Fe to Mg to Si is 9:1:1:0.3, mixing.
And adding 30% of sodium hydroxide into the mixed liquid, adjusting the pH to 4, and adding an alkalizer to enable the alkalization degree to be 0.8-1.2 to obtain the high-efficiency composite flocculant.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A method for preparing a high-efficiency composite flocculant by using red mud as a raw material is characterized by comprising the following steps:
s1: adding red mud and hydrochloric acid into a reaction kettle, then carrying out acid leaching in the reaction kettle at the temperature of 60-100 ℃, and then carrying out filter pressing by using a filter press to obtain filtrate and a filter cake;
s2: putting the filter cake obtained in the step S1 into the reaction kettle again, adding a sodium hydroxide solution, stirring at the temperature of 80-140 ℃, mixing for a certain time, and performing filter pressing by using a filter press to obtain a sodium silicate solution and residues;
s3: putting the sodium silicate solution obtained in the step S2 into the reaction kettle again, adding hydrochloric acid, adjusting the pH value to 1-4, standing for 1-6 h, and adjusting the pH value to 1-3 to obtain a polysilicic acid solution;
s4: sampling the proportion of Al, Mg, Fe, Si and the like in the solution obtained in the steps S3 and S1, then adding the filtrate obtained in the step S1 into the solution obtained in the step S3, and simultaneously adding a proper amount of Al, Mg and Fe according to needs, so that Al, Mg, Fe and Si form a certain proportion;
s5: in step S4, adding a sodium hydroxide solution, adjusting the pH value to 3-4, and alkalizing with an alkalizer to a degree of alkalization of 0.8-1.2 to obtain the high-efficiency composite flocculant.
2. The method for preparing the efficient composite flocculant from red mud according to claim 1, wherein in step S1, the reaction temperature is 80-95 ℃ and the pressure is 0.101MPa, preferably, the reaction temperature is 80-90 ℃ and the pressure is 0.11 MPa.
3. The method for preparing the efficient composite flocculant from the red mud as the raw material according to claim 1, wherein in the step S1, the red mud needs to be ground to form 1000-2000 mesh powder particles.
4. The method for preparing the efficient composite flocculant from the red mud as the raw material according to claim 1, wherein the concentration of the sodium hydroxide solution in the step S2 is 28-40%, the reaction temperature is 90-135 ℃, preferably, the concentration of the sodium hydroxide solution is 30-36%, and the reaction temperature is 110-130 ℃.
5. The method for preparing the efficient composite flocculant from red mud as the raw material according to claim 1, wherein the residue obtained in the step S2 is subjected to acid washing and alkali washing again, and then is washed clean with clear water to obtain titanium oxide.
6. The method for preparing the efficient composite flocculant from the red mud as the raw material according to claim 1, wherein the concentration of the hydrochloric acid in the step S3 is 1% -5%, the pH value is firstly adjusted to 1-4, the mixture is allowed to stand for 2-5 h, and then the pH value is adjusted to 1-3, preferably, the pH value is firstly adjusted to 2-3, the mixture is allowed to stand for 3-4 h, and then the pH value is adjusted to 1.5-2.5.
7. The method for preparing the efficient composite flocculant from the red mud as the raw material according to claim 1, wherein the Al, Mg and Fe are added in step S3 by using aluminum chloride, ferric chloride and magnesium chloride solution.
8. The method for preparing the efficient composite flocculant by using the red mud as the raw material according to claim 7, wherein the aluminum chloride, the ferric chloride and the magnesium chloride are all industrial-grade magnesium chloride hexahydrate, and the hydrochloric acid is industrial-grade hydrochloric acid.
9. The method for preparing the efficient composite flocculant from the red mud as the raw material according to claim 1, wherein the molar ratio of Al, Mg, Fe and Si in the step S3 is 9:1:1: 0.3.
10. The method for preparing the efficient composite flocculant from red mud according to claim 1, wherein in step S5, an alkalizer is aluminate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072150A (en) * | 2021-04-22 | 2021-07-06 | 重庆理工大学 | Method for preparing iron-titanium-vanadium ternary inorganic polymeric flocculant based on sulfuric acid acidolysis vanadium-titanium magnetite two-step method |
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| CN103342406A (en) * | 2013-07-02 | 2013-10-09 | 山东大学 | Polymeric silicic acid-polyferric sulfate titanium inorganic macromolecular composite flocculant and preparation method and application thereof |
| CN106335981A (en) * | 2015-07-07 | 2017-01-18 | 云南民族大学 | Comprehensive utilization method of nickel slag and red mud |
| CN108083345A (en) * | 2017-12-14 | 2018-05-29 | 中山大学 | A kind of method that polymeric aluminum sulfate silicate iron composite flocculation agent is prepared using red mud waste material |
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2020
- 2020-08-24 CN CN202010857489.XA patent/CN112093870A/en active Pending
Patent Citations (4)
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| JP2000271574A (en) * | 1999-03-24 | 2000-10-03 | Asahi Kagaku Kogyo Co Ltd | Water purifying flocculant and production thereof |
| CN103342406A (en) * | 2013-07-02 | 2013-10-09 | 山东大学 | Polymeric silicic acid-polyferric sulfate titanium inorganic macromolecular composite flocculant and preparation method and application thereof |
| CN106335981A (en) * | 2015-07-07 | 2017-01-18 | 云南民族大学 | Comprehensive utilization method of nickel slag and red mud |
| CN108083345A (en) * | 2017-12-14 | 2018-05-29 | 中山大学 | A kind of method that polymeric aluminum sulfate silicate iron composite flocculation agent is prepared using red mud waste material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072150A (en) * | 2021-04-22 | 2021-07-06 | 重庆理工大学 | Method for preparing iron-titanium-vanadium ternary inorganic polymeric flocculant based on sulfuric acid acidolysis vanadium-titanium magnetite two-step method |
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