CN1197038A - High effective polymeric aluminium-silicon chloride flocculant and prepn. tech. thereof - Google Patents
High effective polymeric aluminium-silicon chloride flocculant and prepn. tech. thereof Download PDFInfo
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- CN1197038A CN1197038A CN 98101425 CN98101425A CN1197038A CN 1197038 A CN1197038 A CN 1197038A CN 98101425 CN98101425 CN 98101425 CN 98101425 A CN98101425 A CN 98101425A CN 1197038 A CN1197038 A CN 1197038A
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Abstract
An efficient flocculant of aluminium silicon polychloride for treating water is prepared through polymerizing and activating sodium silicate to obtain high-polymerization-degree polysilicic acid, and adding it to concentrated solution of aluminium polychloride while stirring at ordinary temp to obtain high-stability, high-concentration aluminium silicon polychloride as flocculant. Its advantages are higher flocculating effect and chemical stability, and long storage period.
Description
The present invention relates to a kind of high effective polymeric aluminium-silicon chloride flocculant and preparation technology thereof, this kind flocculation agent is applicable to and anyly gives, need the coagulating treatment process in the waste water treatment engineering.
Coagulation process is most widely used general, a most general unit operation technology in the engineering of water treatment.The coagulating treatment effect is directly determining the operation condition of follow-up processing flow, final outflow water quality and cost, so it is one of Technology important in the engineering of water treatment all the time.The key of highly effective coagulation is to select the coagulating agent of excellent property.Therefore, coagulating agent is to use the important chemical agent that has a large capacity and a wide range in the water treatment industry always.In recent years, inorganic macromolecule flocculant poly aluminium, polymerization iron etc. are existing to develop on a large scale very much, and is used widely, wherein polymerize aluminum chloride existing market sales volume maximum.Compare with traditional flocculation agent, inorganic polymer flocculant can obviously improve water purification usefulness, reduces dosage, reduces running cost, improves effluent quality.Therefore, the various composite flocculants based on inorganic polymer flocculant are developed application in succession in recent years, and especially aluminium, silicon composite flocculant kind receive much concern.At present, aluminium, silicon composite flocculant mainly can be classified as two big classes: a class is silicon, the aluminium flocculating agent preparation method that U.S. Pat Patent4923629, Chinese patent CN1069470A are reported, come down to form by the hybrid modulation of activated silicic acid and conventional aluminum salt, though it has better coagulation usefulness than conventional aluminum salt flocculation agent, but the effective concentration of aluminium is low, and stability is relatively also relatively poor; Another kind of is the polymerization aluminium silicate-sulphate, U.S. Pat Patent 4981675, Chinese patent CN1042340A, CN1082006A have all reported its preparation technology, though this polymerization aluminium silicate-sulphate has good efficiency of coagulation, its complicated process of preparation, material quality requires tight, the preparation cost height.In addition, Chinese patent CN1049323A, CN1050708A, CN1059505A, CN1067031A have also reported the technology that contains the aluminium silicon composite flocculant of the rough feedstock production of aluminium with bauxitic clay, aluminium scrap bits etc., but its product effective concentration is low, impurity many and content is high, stability is also relatively poor relatively, difficult quality guarantee.
The present invention mainly helps ability with fixed attention based on the good efficiency of coagulation of inorganic macromolecule flocculant poly aluminum chloride and the efficient adhesion bridge formation of poly-silicic acid, adopts the synthetic high effective polymeric aluminium-silicon chloride flocculant that prepared of short-cut method.
SiO in related polymerization (activation) silicic acid in the patent specification
2Al in %, the polymerized aluminium silicon chloride
2O
3% and SiO
2% all refers to the quality concentration expressed in percentage by volume, i.e. contained Al in 100 ml samples
2O
3Or SiO
2The weight in grams number.
Major technique content of the present invention is:
1 is stirring fast under the condition of divergence, and the sulfuric acid of 1: 1 hydrochloric acid or 1: 2 is quantitatively promptly added in the sodium silicate solution, reaches 1～2 until pH, obtains containing SiO
26.0% activated silicic acid, this operation can at room temperature be finished.
2 activated silicic acids with above-mentioned gained are heated to 30～40 ℃, and keep 30 minutes, obtain having the polymeric silicicacid of high-polymerization degree.If room temperature surpasses 40 ℃, then needn't thermostatically heating.
3 under quick agitation condition, and above-mentioned polymeric silicicacid is slowly added in the liquid aluminium polychloride, and continuously stirring can obtain high effective polymeric aluminium-silicon chloride flocculant in 10 minutes.This operation can be carried out at normal temperatures and pressures.
One of example
Taking by weighing 230 gram moduluses is 3.1 liquid sodium silicate, SiO in this water glass
2And Na
2The mass percent of O is respectively 26.1%, 8.9%; Add 500mL water, obtain 667mLSiO
2The sodium silicate solution of content 9%.Measure the sulfuric acid 132mL of 1+2.Under quick magnetic agitation, sulfuric acid is added in the sodium silicate solution rapidly, and add water to 1L, stir, obtain 1LpH value 1.0, SiO
2The activated silicic acid of content 6%.This activated silicic acid is placed 30～40 ℃ of water-bath insulations 10 minutes.
Press proportioning shown in the table 1, to contain Al
2O
316% (4.4mol/L Al
3+), the polymerize aluminum chloride and the quantitative mixing and stirring of water of basicity 47.3%, measure a certain amount of polymeric silicicacid then, under magnetic agitation is operated fast, in 2 minutes, slowly add polymeric silicicacid in the polymeric aluminum chlorides solution, continue then to stir 10 minutes, making volume is 0.6L, the polymeric aluminium-silicon chloride flocculant that concentration is as shown in table 1.
The synthesizing formula of table 1 polymeric aluminium-silicon chloride flocculant and product composition
| No. | Polymerize aluminum chloride (mL) | Water (mL) | Polymeric silicicacid (mL) | Al in the product 2O 3??(％) | SiO in the product 2????(％) | The Si/Al mol ratio |
| 1 | ????400 | ???0 | ??200 | ????15.1 | ????2.0 | ??0.11 |
| 2 | ????300 | ?100 | ??200 | ????11.3 | ????2.0 | ??0.15 |
| 3 | ????450 | ???0 | ??150 | ????17.0 | ????1.5 | ??0.075 |
| 4 | ????300 | ?150 | ??150 | ????11.3 | ????1.5 | ??0.11 |
| 5 | ????200 | ?250 | ??150 | ????7.5 | ????1.5 | ??0.17 |
| 6 | ????150 | ?300 | ??150 | ????5.7 | ????1.5 | ??0.23 |
Two of example
Taking by weighing 116 gram moduluses is 3.2 liquid sodium silicate, SiO in this water glass
2And Na
2The mass percent of O is respectively 28.0%, 9.04%; Add 448mL water, obtain 530mLSiO
2The sodium silicate solution of content 6%.Measure the hydrochloric acid 70mL of 1+1.Under quick magnetic agitation, hydrochloric acid is added rapidly in the sodium silicate solution, stir, obtaining the 0.6LpH value is 1.0, SiO
2The activated silicic acid of content 5.4%.This activated silicic acid is incubated 15 minutes at 30～40 ℃.To contain Al
2O
316.5% (4.50mol/L Al
3+), the polymerize aluminum chloride of basicity 65.0% is raw material, press the indicated proportional quantity in table 2 No.1～3, measure polymerize aluminum chloride and water earlier and mix, measure again with quantitative polymeric silicicacid, under quick magnetic agitation, in 2 minutes, will gather silicic acid and slowly add in the polymeric aluminum chlorides solution, stir then 10 minutes, or to contain Al
2O
36.7% (1.50mol/L Al
3+), the polymerize aluminum chloride of basicity 32.% is raw material, presses the indicated material proportional quantity in table 2 No.4～6, making volume is 0.6L, concentration polymeric aluminium-silicon chloride flocculant as shown in table 2.
The synthesizing formula of table 2 polymeric aluminium-silicon chloride flocculant and product composition
| ????No. | Basicity (%) | Polymerize aluminum chloride (mL) | Water (mL) | Polymeric silicicacid (mL) | Al in the product 2O 3????(％) | SiO in the product 2????(％) | The Si/Al mol ratio |
| ????1 | ?65.0 | ????400 | ???0 | ????200 | ????15.3 | ????1.8 | ??0.10 |
| ????2 | ?65.0 | ????400 | ??65 | ????135 | ????15.3 | ????1.2 | ??0.067 |
| ????3 | ?65.0 | ????400 | ?134 | ????66 | ????15.3 | ????0.6 | ??0.033 |
| ????4 | ?32.0 | ????400 | ?134 | ????66 | ????5.1 | ????1.8 | ??0.10 |
| ????5 | ?32.0 | ????400 | ?155 | ????45 | ????5.1 | ????1.2 | ??0.067 |
| ????6 | ?32.0 | ????400 | ?178 | ????22 | ????5.1 | ????0.6 | ??0.033 |
The prepared polymeric aluminium-silicon chloride flocculant of the present invention is applicable to that turbidity removal, the decolouring to, waste water handle, and is particularly suitable for the purifying treatment of low temperature and low turbidity water, has the efficiency of coagulation more excellent than polymerize aluminum chloride.
One of application example
With above example two in the coagulation turbidity removal that is used for the kaolin muddy water of the No.1～3 polymeric aluminium-silicon chloride flocculant products of preparation handle, contrast with polymerize aluminum chloride simultaneously.Raw water turbidity is 70NTU, pH value 7.38, and 13 ℃ of water temperatures, result is listed in table 3.
The coagulation turbidity removal effect of table 3 polymerized aluminium silicon chloride
| ????No. | Different dosages are (with Al 3+10 -5The mol/L meter) under, handles the residual turbidity (NTU) of back water | ||||
| ????2.0 | ????4.0 | ????6.0 | ????8.0 | ????10 | |
| ????1 | ????26 | ????7.7 | ????3.2 | ????2.6 | ????1.9 |
| ????2 | ????24 | ????9.1 | ????4.3 | ????2.7 | ????1.6 |
| ????3 | ????28 | ????11.1 | ????5.2 | ????2.8 | ????2.0 |
| Polymerize aluminum chloride | ????32 | ????12.3 | ????7.2 | ????4.9 | ????3.9 |
From above result as seen, the coagulation turbidity removal effect of polymeric aluminium-silicon chloride flocculant obviously is better than flocculant of polymeric aluminium chloride, and increases with silicone content, and coagulation effect is good more.Reach same or more excellent treatment effect, use polymeric aluminium-silicon chloride flocculant can save pharmaceutical quantities 15～20% than polymerize aluminum chloride.
Two of application example
With above example two in the coagulation turbidity removal decolouring that is used to contain humic acids and the muddy colored water of kaolin of prepared No.4～6 polymeric aluminium-silicon chloride flocculant products handle, contrast with flocculant of polymeric aluminium chloride simultaneously.Raw water turbidity is 30NTU, and colourity represents that with the 370nm light absorption value its value is 0.175.PH value 7.20,13 ℃ of water temperatures, result is listed in table 4.
The coagulate decoloring effect of table 4 polymerized aluminium silicon chloride
| ????No. | Different dosages are (with Al 3+10 -5The mol/L meter) under, handles the residue colourity of back water | |||
| ????2.0 | ????4.0 | ????6.0 | ????8.0 | |
| ????1 | ????0.162 | ????0.070 | ????0.030 | ????0.024 |
| ????2 | ????0.165 | ????0.071 | ????0.034 | ????0.028 |
| ????3 | ????0.168 | ????0.073 | ????0.037 | ????0.030 |
| Polymerize aluminum chloride | ????0.172 | ????0.085 | ????0.048 | ????0.042 |
From above result as seen, the coagulation decoloration usefulness of polymeric aluminium-silicon chloride flocculant also more obviously is better than flocculant of polymeric aluminium chloride.
The prepared polymeric aluminium-silicon chloride flocculant of the present invention not only has good efficiency of coagulation, and has good chemical stability, never degenerated in 6 months at least, and efficiency of coagulation is constant.With the prepared Al of the present invention
2O
3Content is 5.7%, SiO
2Content is that 1.5% polymeric aluminium-silicon chloride flocculant is an example, carries out the contrast of coagulation turbidity removal effect with flocculant of polymeric aluminium chloride after storing 6 months under 20～30 ℃ of room temperatures, the results are shown in table 5.
Table 5 is stored the coagulation turbidity removal effect of 6 months post polymerization aluminium-silicon chlorides
| ????No. | Different dosages are (with Al 3+10 -5The mol/L meter) under, handles the residual turbidity (NTU) of back water | ||||
| ????0.8 | ????1.2 | ????1.6 | ????2 | ????2.4 | |
| Polymerized aluminium silicon chloride | ????28 | ????15.7 | ????7.6 | ????6.8 | ????5.4 |
| Polymerize aluminum chloride | ????32 | ????18.2 | ????12.3 | ????9.6 | ????8.3 |
From above result as seen, through the polymeric aluminium-silicon chloride flocculant of 6 months long storage, its efficiency of coagulation still obviously is better than flocculant of polymeric aluminium chloride, shows that the polymeric aluminium-silicon chloride flocculant by prepared of the present invention has good chemical stability.
In sum, the polymeric aluminium-silicon chloride flocculant that the present invention is prepared had good efficiency of coagulation and chemical stability, and preparation technology is easy.Coagulate agent with the silicon of other prepared, aluminium complex type flocculation and compare, cheap and treatment efficiency is high.
Must point out, more because of the kind of raw materials used polymerize aluminum chloride of the present invention and water glass, need statement once more:
1 one kinds of high effective polymeric aluminium-silicon chloride flocculants, its effective ingredient is: Al
2O
34～17%, SiO
20.5～3.0%; Its basicity is 30～70%.Because of the difference of quality, polymerize aluminum chloride can contain a certain amount of sulfate radical, phosphate radical etc.
2 preparation technologies as polymeric aluminium-silicon chloride flocculant as described in 1, this technology comprise earlier the water glass activated polymerization are obtained having the polymeric silicicacid of high-polymerization degree; And then polymeric silicicacid is incorporated in the polymerize aluminum chloride, finally obtain stable polymeric aluminium-silica flocculation agent.
3 according to 2 described preparation technologies, it is characterized in that water glass is the water glass of modulus 1.6～3.9.
4 according to 2 described preparation technologies, it is characterized in that earlier water glass being activated to pH value 1～2, SiO
2The polymeric silicicacid of concentration≤6.0%, this poly-silicic acid was 30～40 ℃ of following polymerizations (activation) 0～30 minute.The water glass activator can be hydrochloric acid, sulfuric acid and other mineral acid or acetic acid.
5 according to 2 described preparation technologies, and to it is characterized in that adopting with the aluminum hydroxide gel be raw material, with the transparent liquid or the solid polyaluminium chloride of the basicity 30～70% of high-temperature low-pressure prepared.
6 according to 1～5 described polymeric aluminium-silicon chloride flocculant and preparation technology thereof, it is characterized in that poly-silicic acid is joined in the polymerize aluminum chloride under room temperature normal pressure agitation condition lentamente, also comprises this order that poly-silicic acid is incorporated into polymerize aluminum chloride.Finally obtain polymeric aluminium-silicon chloride flocculant as stability and high efficiency as described in 1.
7 polymeric aluminium-silicon chloride flocculants according to 1～6 described preparation are widely used in turbidity removal, decolorization to, wastewater treatment or other adopts coagulation process to carry out the solid-liquid separation process.
Claims (8)
1 one kinds of high effective polymeric aluminium-silicon chloride flocculants, its effective ingredient is: Al
2O
34～17% (m/v), SiO
20.5～3.0% (m/v); Basicity is 30～70%; Density 1.10～1.30 grams per milliliters; PH value 1.30～2.70.
2 preparation technologies of polymeric aluminium-silicon chloride flocculant according to claim 1, this technology comprise earlier the water glass activated polymerization are obtained the polymeric silicicacid of high-polymerization degree; Then polymeric silicicacid is incorporated in the polymerize aluminum chloride, finally obtains stable polymeric aluminium-silicon chloride flocculant.
3 according to the described preparation technology of claim 2, it is characterized in that water glass is the liquid sodium silicate of modulus 1.6～3.9.
4 according to the described preparation technology of claim 2, it is characterized in that water glass is activated to pH value 1～2, SiO
2The polymeric silicicacid of concentration≤6.0% (m/v), this polymeric silicicacid polymerase 10～30 minute under room temperature (30-40 ℃) temperature, activator can be hydrochloric acid or sulfuric acid.
5 according to the described preparation technology of claim 2, and polymerize aluminum chloride is is raw material with the aluminum hydroxide gel, adopt that the basicity of high-temperature low-pressure polymerization preparation is 30～70%, concentration is the transparent liquid or the solid polyaluminium chloride of 6～17% (m/m).
6 according to described polymeric aluminium-silicon chloride flocculant of claim 1～5 and preparation technology thereof, it is characterized in that polymeric silicicacid is introduced in the polymerize aluminum chloride under the room temperature normal pressure, finally obtain polymeric aluminium-silicon chloride flocculant efficient according to claim 1, stable, high density.
7 processing steps according to claim 6, the preparation of polymerized aluminium silicon chloride, its feature comprises this order that polymeric silicicacid is incorporated into polymerize aluminum chloride.
8 polymeric aluminium-silicon chloride flocculants be used to feed water turbidity removal, decolouring with wastewater treatment according to the described preparation of claim 1～7, and other adopts the solid-liquid separation process of coagulation process.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98101425 CN1197038A (en) | 1998-04-24 | 1998-04-24 | High effective polymeric aluminium-silicon chloride flocculant and prepn. tech. thereof |
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|---|---|---|---|
| CN 98101425 CN1197038A (en) | 1998-04-24 | 1998-04-24 | High effective polymeric aluminium-silicon chloride flocculant and prepn. tech. thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100347098C (en) * | 2003-10-30 | 2007-11-07 | 同济大学 | Aluminium iron chloride of coagulant agent in polymorphism polymerization and preparation method |
| CN102249893A (en) * | 2010-12-13 | 2011-11-23 | 日照金禾博源生化有限公司 | Citric acid solution decolorizing method |
| CN103979655A (en) * | 2013-11-01 | 2014-08-13 | 季红军 | Sewage treatment agent and preparation method thereof |
| CN104787867A (en) * | 2015-05-04 | 2015-07-22 | 李练红 | Flocculant for river/lake water body original ecological restoration and application thereof |
| CN113896304A (en) * | 2021-10-22 | 2022-01-07 | 上海成宙化工有限公司 | High-efficiency water treatment flocculant and preparation method thereof |
| CN114149065A (en) * | 2021-12-27 | 2022-03-08 | 襄垣县万普净水材料有限公司 | Novel water purifying agent production reaction curing flash evaporation process |
| CN114214467A (en) * | 2021-12-10 | 2022-03-22 | 中粮崇左糖业有限公司 | Method for settling and clarifying filtered juice of sugarcane raw sugar factory |
| CN115838177A (en) * | 2022-07-27 | 2023-03-24 | 杭州萧山三江净水剂有限公司 | Preparation method of high-basicity polymerized aluminum silicon chloride and treatment method of papermaking wastewater containing low-concentration organic halide |
| CN117383574A (en) * | 2023-10-16 | 2024-01-12 | 北京万水净水剂有限公司 | Production process of composite polysilicate aluminum coagulant |
-
1998
- 1998-04-24 CN CN 98101425 patent/CN1197038A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100347098C (en) * | 2003-10-30 | 2007-11-07 | 同济大学 | Aluminium iron chloride of coagulant agent in polymorphism polymerization and preparation method |
| CN102249893A (en) * | 2010-12-13 | 2011-11-23 | 日照金禾博源生化有限公司 | Citric acid solution decolorizing method |
| CN102249893B (en) * | 2010-12-13 | 2014-01-08 | 日照金禾博源生化有限公司 | Citric acid solution decolorizing method |
| CN103979655A (en) * | 2013-11-01 | 2014-08-13 | 季红军 | Sewage treatment agent and preparation method thereof |
| CN103979655B (en) * | 2013-11-01 | 2015-08-26 | 浙江省农业科学院 | A kind of sewage treatment drug and preparation method thereof |
| CN104787867A (en) * | 2015-05-04 | 2015-07-22 | 李练红 | Flocculant for river/lake water body original ecological restoration and application thereof |
| CN113896304A (en) * | 2021-10-22 | 2022-01-07 | 上海成宙化工有限公司 | High-efficiency water treatment flocculant and preparation method thereof |
| CN114214467A (en) * | 2021-12-10 | 2022-03-22 | 中粮崇左糖业有限公司 | Method for settling and clarifying filtered juice of sugarcane raw sugar factory |
| CN114149065A (en) * | 2021-12-27 | 2022-03-08 | 襄垣县万普净水材料有限公司 | Novel water purifying agent production reaction curing flash evaporation process |
| CN115838177A (en) * | 2022-07-27 | 2023-03-24 | 杭州萧山三江净水剂有限公司 | Preparation method of high-basicity polymerized aluminum silicon chloride and treatment method of papermaking wastewater containing low-concentration organic halide |
| CN117383574A (en) * | 2023-10-16 | 2024-01-12 | 北京万水净水剂有限公司 | Production process of composite polysilicate aluminum coagulant |
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