CN102092828B - Method for preparing polymer calcium-aluminum silicate coagulant from carbide slag - Google Patents
Method for preparing polymer calcium-aluminum silicate coagulant from carbide slag Download PDFInfo
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- CN102092828B CN102092828B CN201010583622A CN201010583622A CN102092828B CN 102092828 B CN102092828 B CN 102092828B CN 201010583622 A CN201010583622 A CN 201010583622A CN 201010583622 A CN201010583622 A CN 201010583622A CN 102092828 B CN102092828 B CN 102092828B
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Abstract
The invention discloses a method for preparing an agent for treating water, wastewater and sewage, particularly a method for preparing a polymer calcium-aluminum silicate coagulant from carbide slag, which is characterized by comprising the following steps of drying the carbide slag; purifying the dried carbide slag by using ammonium chloride to obtain carbide slag extract; preparing the solution of sodium silicate, and adjusting the pH value of the solution of sodium silicate by using a concentrated sulfuric acid or sodium hydroxide to obtain polymer silicate solution; performing condensation polymerization on the polymer silicate solution to obtain high polymer silicate solution; and performing sedimentation on the high polymer silicate solution, solution of aluminum sulfate and the carbide slag to prepare the polymer calcium-aluminum silicate coagulant product. The method has the advantages of scientificity, rationalism, low energy consumption, low cost and the like. The polymer calcium-aluminum silicate coagulant prepared by the method has high stability and ensures good water treatment effects.
Description
Technical field
The present invention is the preparation method of a water, waste water, sewage-treating agent, is a kind of method of utilizing carbide slag to prepare polymeric silicicacid calcium aluminium coagulating agent.
Background technology
Polymeric silicicacid salt coagulating agent is a kind of inorganic polymer coagulant.At present, the method for developing the polymeric silicicacid salt coagulant both at home and abroad mainly is divided into three kinds: the one, and the polymeric silicicacid flocculation agent of metal ion, the 2nd, recombining process polymeric silicicacid compound coagulant, the 3rd, copolymerization process polymeric silicicacid flocculation agent.Polymeric silicicacid and metal-salt directly mix the polymeric silicicacid flocculation agent that generation polymeric silicicacid metal composite coagulating agent belongs to metal ion; It is the recombining process polymeric silicicacid that polymeric silicicacid and polymer/metallic salt are mixed and made into the PASM flocculation agent; Mix earlier the back with metallic salt and adding OH
-The flocculation agent that its polymerization is processed is a copolymerization process.In addition, doing raw material with ore, abandoned mine slag, flyash etc. develops novel coagulating agent and has had related.
" safety and environment journal " 2002 1 phases 2 volume, the carbide slag and the CaCl of people's experimental studies such as Li Yafeng
2To the coagulating treatment effect of Shenyang Tiefa Mine Administration black water and adopt carbide slag-PAM coagulant sedimentation to handle the back black water, each item index all can reach the report of discharging standards.Open (bulletin) number CN1778702 of Chinese invention patent discloses people such as Zhao Qinghai invention; Name is called " a kind of sewage-treating agent "; This sewage-treating agent is made up of coagulating agent and coagulant aids two portions; Composite use, coagulant aids is processed by the raw material of following weight part: carbide slag 8～20, preparation water 600～1000.Use treatment agent of the present invention to handle town sewage or industrial sewage, can reach the purpose of purification of water quality.
There are weak point in traditional low molecule, high molecular polymerization silicic acid composite coagulant at aspects such as molecular conformation, the polymerization degree and corresponding flocculation-flocculating results more, therefore, be necessary development of new efficiently compound coagulant compensate its defect.With polymeric silicicacid and inorganic metal salt coagulant double crossing, the novel inorganic high molecular polymerization silicate coagulating agent that processability is stable.The present invention brings into play the advantage of polymeric silicicacid, remedies the shortcoming of metal-salt self, produces synergy.Be that raw material and high-polymeric silicic acid salt prepare coagulating agent and is applied to water treatment field and do not appear in the newspapers as yet with the carbide slag.
Content of the present invention
The objective of the invention is; Prior art is carried out substantial improvements; A kind of preparing method's science, reasonable is provided, and energy consumption is low, and the carbide slag that utilizes that cost is low prepares the method for polymeric silicicacid calcium aluminium coagulating agent; With the good stability of the polymeric silicicacid calcium aluminium coagulating agent of method for preparing, the treating water effect is good.
The objective of the invention is to realize by following technical scheme:
A kind of method of utilizing carbide slag to prepare polymeric silicicacid calcium aluminium coagulating agent is characterized in that it comprises following step:
(1) carbide slag is carried out drying treatment, 100 ℃～200 ℃ of carbide slag drying temperatures, time of drying 2～6h, dried carbide slag is Powdered;
(2) carry out purification processes after the carbide slag drying treatment; The mass ratio of getting carbide slag that step (1) obtains and ammonium chloride is 1～6, preparation water is 200～1200ml, 20 ℃～60 ℃ of controlled temperature, regulate pH=7～9; Control stirring velocity 100～300r/min; Churning time 20～30min leaves standstill 20～30min and obtains the carbide slag extracting solution;
(3) prepare silicon acid sodium solution, described sodium silicate solution percentage concentration is 4%～8%, with SiO
2The massfraction meter, the pH of the sodium silicate solution of the vitriol oil of use 10%～30% or sodium hydroxide adjusting 4%～8% is 1～3, must be to polymerization of silicic acid solution;
(4) polymerization of silicic acid solution that step (3) is obtained carries out polycondensation, and the reaction times is 0.5～1.5h, obtains high-polymeric silicic acid solution, this solution emulsus liquid state that is white in color;
(5) compound concentration is the alum liquor of 0.03～0.1mol/L;
(6) under room temperature, stirring velocity 50～150r/min, churning time 1～5min condition, in high-polymeric silicic acid solution, add the alum liquor 100mL that step (5) obtains, the mol ratio that makes Al and Si is 0.3～0.8;
(7) under room temperature, stirring velocity 50～150r/min, the churning time 1～5min condition; In high-polymeric silicic acid that step (6) obtains and Tai-Ace S 150 mixing solutions, add the carbide slag extracting solution 100mL that step (2) obtains; The mol ratio that makes Ca and Si is 0.2～0.8; The heavyization time is 4～10h, and it is 14.1%～15.6% polymeric silicicacid calcium aluminium coagulating agent product that preparation becomes massfraction, and polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
It is simple that preparation of the present invention has a process step, the characteristics of low cost of manufacture.Reaction is carried out at normal temperatures, is easy to control, good stability.Flocculate rapidly when product is used as flocculation agent, flco is big and solid, and sedimentation is fast, applied range, suitable pH wide ranges.Preparing method of the present invention is easy to realize that can realize industrial production of polymeric Calucium Silicate powder aluminium, product has broad application prospects at water treatment field, and economic benefit is considerable.
Embodiment
Embodiment 1: the power taking rock ballast carries out drying treatment, 100 ℃ of carbide slag kiln temperatures, time of drying 2h, obtaining massfraction is 40.5% Powdered carbide slag; Use ammonium chloride during purification; The mass ratio of carbide slag and ammonium chloride is 1; Power taking rock ballast 3.6g, ammonium chloride 3.6g mixes in 200mL preparation water; Control 20 ℃ of its temperature, pH=7, stirring velocity 100r/min, churning time 20min, leave standstill 20min, obtain the carbide slag extracting solution of calcium ions 0.02mol/L; Get 10ml, 4% sodium silicate solution is incorporated in 5ml, 10% sulphuric acid soln; The pH that utilizes 10% sodium hydroxide and sulfuric acid to regulate sodium silicate solution is 1, obtains polymerization of silicic acid solution; The control polycondensation reaction time is 0.5h, obtains white emulsus high-polymeric silicic acid solution; Introduce 0.03mol/L in the high-polymeric silicic acid solution after polycondensation, the alum liquor of 100mL and calcium ions 0.02mol/L, the carbide slag extracting solution of 100mL; Under room temperature, stirring velocity 50r/min, the churning time 1min condition, polycondensation takes place; The heavyization time is 4h, obtains 14.1% polymeric silicicacid calcium aluminium coagulating agent, and polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
Embodiment 2: the power taking rock ballast carries out drying treatment, 150 ℃ of carbide slag kiln temperatures, time of drying 4h, obtaining massfraction is 43.6% Powdered carbide slag; Carbide slag carries out will carrying out purification processes after the drying treatment, uses ammonium chloride during purification; The mass ratio of carbide slag and ammonium chloride is 3; Power taking rock ballast 10.8g; Ammonium chloride 3.6g mixes in 700mL preparation water, controls 40 ℃ of its temperature, pH=8, stirring velocity 200r/min, churning time 25min, leaves standstill the carbide slag extracting solution that 25min obtains calcium ions 0.05mol/L; Get 20ml, 6% sodium silicate solution, be incorporated in 7ml, 20% sulphuric acid soln under the control stirring velocity 100r/min condition; The pH that utilizes 20% sodium hydroxide and sulfuric acid to regulate sodium silicate solution is 2; The control polycondensation reaction time is 1.0h, obtains white emulsus high-polymeric silicic acid solution; Introduce 0.06mol/L successively in the high-polymeric silicic acid solution after polycondensation; The alum liquor of 100mL and calcium ions 0.05mol/L; Polycondensation under room temperature, stirring velocity 100r/min, the churning time 3min condition, takes place in the carbide slag extracting solution of 100mL; The heavyization time is 8h, obtains 14.6% polymeric silicicacid calcium aluminium coagulating agent, and polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
Embodiment 3: the power taking rock ballast carries out drying treatment, 200 ℃ of carbide slag kiln temperatures, time of drying 6h, obtaining massfraction is 44.3% Powdered carbide slag; Carbide slag carries out will carrying out purification processes after the drying treatment, uses ammonium chloride during purification; The mass ratio of carbide slag and ammonium chloride is 6; Power taking rock ballast 216g; Ammonium chloride 3.6g mixes in 1200mL preparation water, controls 60 ℃ of its temperature, pH=9, stirring velocity 300r/min, churning time 30min, leaves standstill the carbide slag extracting solution that 30min obtains calcium ions 0.08mol/L; Get 30ml, 8% sodium silicate solution, be incorporated in 10ml, 30% sulphuric acid soln under the control stirring velocity 150r/min condition; The pH that utilizes 30% sodium hydroxide and sulfuric acid to regulate sodium silicate solution is 3; The control polycondensation reaction time is 1.5h, obtains white emulsus high-polymeric silicic acid solution; Introduce 0.1mol/L successively in the high-polymeric silicic acid solution after polycondensation, the alum liquor of 100mL and calcium ions 0.08mol/L, polycondensation under room temperature, stirring velocity 150r/min, the churning time 5min condition, takes place in the extracting solution of 100mL; The heavyization time is 10h.Obtain 15.6% polymeric silicicacid calcium aluminium coagulating agent, polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
Ammonium chloride, Tai-Ace S 150 adopt analytical pure, sodium hydroxide, and raw materials such as sulfuric acid are easy to get, and are the commercially available prod.
The related loft drier of the method for utilizing carbide slag to prepare polymeric silicicacid calcium aluminium coagulating agent of the present invention, whisking appliance etc. are the commercially available prod.
Claims (1)
1. method of utilizing carbide slag to prepare polymeric silicicacid calcium aluminium coagulating agent is characterized in that it comprises following step:
(1) carbide slag is carried out drying treatment, 100 ℃～200 ℃ of carbide slag drying temperatures, time of drying 2～6h, dried carbide slag is Powdered;
(2) carry out purification processes after the carbide slag drying treatment; The mass ratio of getting carbide slag that step (1) obtains and ammonium chloride is 1～6, preparation water is 200～1200ml, 20 ℃～60 ℃ of controlled temperature, regulate pH=7～9; Control stirring velocity 100～300r/min; Churning time 20～30min leaves standstill 20～30min and obtains the carbide slag extracting solution;
(3) prepare silicon acid sodium solution, described sodium silicate solution percentage concentration is 4%～8%, with Si0
2The massfraction meter, the pH of the sodium silicate solution of the vitriol oil of use 10%～30% or sodium hydroxide adjusting 4%～8% is 1～3, obtains polymerization of silicic acid solution;
(4) polymerization of silicic acid solution that step (3) is obtained carries out polycondensation, and the reaction times is 0.5～1.5h, obtains high-polymeric silicic acid solution, this solution emulsus liquid state that is white in color;
(5) compound concentration is the alum liquor of 0.03～0.1mol/L;
(6) under room temperature, stirring velocity 50～150r/min, churning time 1～5min condition, in high-polymeric silicic acid solution, add the alum liquor 100mL that step (5) obtains, the mol ratio that makes Al and Si is 0.3～0.8;
(7) under room temperature, stirring velocity 50～150r/min, the churning time 1～5min condition; In high-polymeric silicic acid that step (6) obtains and Tai-Ace S 150 mixing solutions, add the carbide slag extracting solution 100mL that step (2) obtains; The mol ratio that makes Ca and Si is 0.2～0.8; The heavyization time is 4～10h, and it is 14.1%～15.6% polymeric silicicacid calcium aluminium coagulating agent product that preparation becomes massfraction, and polymeric silicicacid calcium aluminium coagulating agent form is white emulsion liquid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010583622A CN102092828B (en) | 2010-12-08 | 2010-12-08 | Method for preparing polymer calcium-aluminum silicate coagulant from carbide slag |
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| CN201010583622A CN102092828B (en) | 2010-12-08 | 2010-12-08 | Method for preparing polymer calcium-aluminum silicate coagulant from carbide slag |
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| CN102092828B true CN102092828B (en) | 2012-10-03 |
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| CN108821413B (en) * | 2018-07-10 | 2021-07-06 | 无锡锐众环保科技有限公司 | Coagulant for efficiently treating COD (chemical oxygen demand) |
| CN115368164B (en) * | 2022-08-31 | 2023-06-06 | 山东鲁碧绿色建筑科技有限公司 | Preparation method of porous concrete for external wall panel |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059505A (en) * | 1991-09-28 | 1992-03-18 | 张伯温 | Polymeric silicicacid-aluminium composite flocculation agent and preparation method |
| WO2001034294A1 (en) * | 1999-11-12 | 2001-05-17 | University Of Greenwich | Silicate/aluminate materials |
| CN101823721A (en) * | 2010-03-19 | 2010-09-08 | 合肥学院 | Method for producing poly silicate aluminium ferric flocculating agent by utilizing coal gangue |
| CN101830476A (en) * | 2009-03-13 | 2010-09-15 | 抚顺矿业集团有限责任公司 | Method for preparing polymeric ferric aluminum silicate flocculant from waste oil shale slag |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059505A (en) * | 1991-09-28 | 1992-03-18 | 张伯温 | Polymeric silicicacid-aluminium composite flocculation agent and preparation method |
| WO2001034294A1 (en) * | 1999-11-12 | 2001-05-17 | University Of Greenwich | Silicate/aluminate materials |
| CN101830476A (en) * | 2009-03-13 | 2010-09-15 | 抚顺矿业集团有限责任公司 | Method for preparing polymeric ferric aluminum silicate flocculant from waste oil shale slag |
| CN101823721A (en) * | 2010-03-19 | 2010-09-08 | 合肥学院 | Method for producing poly silicate aluminium ferric flocculating agent by utilizing coal gangue |
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