CN100386267C - High efficiency composite flocculant, its preparation method and application - Google Patents

High efficiency composite flocculant, its preparation method and application Download PDF

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CN100386267C
CN100386267C CNB2005100308348A CN200510030834A CN100386267C CN 100386267 C CN100386267 C CN 100386267C CN B2005100308348 A CNB2005100308348 A CN B2005100308348A CN 200510030834 A CN200510030834 A CN 200510030834A CN 100386267 C CN100386267 C CN 100386267C
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water
composite flocculant
flocculant
coagulant aids
efficiency composite
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CNB2005100308348A
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Chinese (zh)
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CN1785836A (en
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王黎明
沈勇
丁颖
张惠芳
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上海工程技术大学
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Abstract

The present invention relates to a high efficiency composite flocculant, a preparing method and application thereof. The flocculant is composed of a flocculant and a coagulant aid, wherein the flocculant is mainly polymeric aluminum iron or polymeric aluminum. The coagulant aid mainly has two classes. One class is an inorganic substance, such as sodium silicate, calcium hydroxide, calcium carbonate, magnesium hydroxide, a macromolecule inorganic coagulant aid, etc. The other class is an organic substance, such as polyacrylamide, dodecyl dimethyl tertiary amine, dicyanodiamide, modified chitosan, etc. The high efficiency composite flocculant can be used for treating the printing and dyeing waste water, and the high efficiency composite flocculant is particularly suitable for non water soluble dispersed dye and paint difficult to remove.

Description

High efficiency composite flocculant, preparation method and application thereof

Technical field

The invention belongs to the techniques of Dyeing Wastewater Treatment field.Relate to composite type polymeric flocculant, preparation method and application, can be used for the processing of fabrics printing and dyeing waste water.

Background technology

Along with developing rapidly of dyestuffs industries, the dye species of whole world use has at present reached tens thousand of kinds, dyeing waste water mainly contains dyestuff, slurry, auxiliary agent, finish, soda acid, fiber impurity and inorganic salt etc., having characteristics such as complicated component, concentration height, colourity height, difficult degradation, is one of main harmful waste water of generally running into of China.The improvement of such waste water at first will solve the decolouring problem.Decoloring method commonly used at present has neutralisation, oxidation style, absorption method, reverse osmosis method, Coagulation Method etc.Advantages such as wherein, Coagulation Method is strong with its adaptability, and operational administrative is simple, initial cost and being widely used.But dyeing waste water is various in style, is applied to its coagulation effect of different dyeing waste waters with a kind of coagulating agent and has very big difference.Especially decolourings such as dispersed dye, coating still being lacked effective flocculation agent handles.Therefore, the combination dye molecular structure, by the further investigation to the mechanism of action of various flocculation agents, developing efficient composite flocculation agent is one of main direction of present coagulation technology development.

In coagulation process, chemical reactions such as hydrolysis, polymerization at first take place in flocculation agent in water, the hydrolytic polymerization product of generation again with water in particle generation static neutralization, intergranular build bridge, adhere to volume and the thick flocs unit of effect generation such as sweep and remove through precipitation again.More than several effects may produce simultaneously, certain effect may be the factor of dominating under different condition.The process control of coagulating both by to the screening of flocculation agent, flocculation reaction condition determine etc. make coagulating can reach best treatment effect with the dosage of minimum.Therefore, the general composite high-molecular flocculation agent that adopts when handling waste water, it can bring into play the advantage of several flocculation agents simultaneously, and it was both economical to make Coagulation Method be used for dyeing waste water, was suitable for again.

Polymeric flocculant is to have high molecular, can promote colloidal particle and other suspended particle to be condensed into the preparation that amorphous throw out precipitates.Polymeric flocculant can be divided into inorganic polymer flocculant, organic polymer coargulator and biopolymer flocculation agent.The toxicity that may exist owing to some organic polymer coargulator price is in addition used more prudent in water treatment than reasons such as costlinesses.At present, most widely used polymeric flocculant is high molecular aluminium salt (or molysite) and composite type inorganic polymer aluminium salt (or molysite) aspect water treatment, and polyaluminium salts (or molysite)-organic polymer compound system is used for water treatment and also more and more comes into one's own.

Aluminium system, iron are inorganic flocculating agent has decades as two big classes of inorganic flocculating agent developing history.It is slow that simple aluminium salt exists sedimentation speed, removes shortcomings such as chromatic effect difference, though and simple molysite settling velocity is fast, turbidity removal effect is good, molysite has very strong corrodibility.Therefore,, make it have the characteristics of general aluminium salt, molysite concurrently, become new research direction aluminium, the synthetic new polymkeric substance of iron copolymerization.From structural performance, polymeric ferric aluminum is a kind of polymeric flocculant that aluminium salt and molysite obtain by copolyreaction, relative molecular mass is bigger, has good decolorizing effect, in water-soluble dye wastewater is handled, certain application is arranged also, but just not obvious to decolorizing effects such as reluctant dispersed dye, coating.It is generally acknowledged that coating becomes colloidal with dispersed dye, be difficult for removing with general flocculation agent, must a kind of compound flocculation agent of preparation.This flocculation agent is to introduce a certain proportion of other metal ion in polymerization organic or inorganic polymer, makes it become the bigger polymerization plasma of molecular weight.By absorption coating, dispersed dye etc., make their colloidal stability obtain destroying, and then can make the coacervation of colloid precipitation.According to this principle, innovative point of the present invention is to introduce the flocculating polymer auxiliary agent in the ferro-aluminum flocculation agent, forms the bigger composite flocculant of molecular weight.Rationally compoundly in flocculation agent advance auxiliary agent, not only can accelerate flocculation rate, improve flocculating effect, and can also reduce the consumption of flocculation agent.Flocculant aid mainly rises and regulates pH value, basicity is provided, improve the flocculating effect of low-temperature and low turbidity and destroy the stability of wetting ability organic impurity, the effect of reduction coexistent impurity.

Summary of the invention

The purpose of this invention is to provide a kind of above-mentioned composite flocculant.

Another object of the present invention provides a kind of preparation method of above-mentioned composite flocculant.

Purpose of the present invention also provides a kind of application of above-mentioned composite flocculant, can be used for the processing of fabrics printing and dyeing waste water.The present invention adopts to introduce in aluminium, iron copolymer and is compounded to form flocculation agent such as inorganic and organic coagulant aidss such as water glass, inorganic polymer coagulant aids Z, polyacrylamide, dodecyl dimethyl tertiary amines, dyeing waste water is comprised that dispersed dye, reactive dyestuffs, matching stain, substantive dyestuff and coating waste-water handle, improve the flocculating decoloring effect of these dyestuffs in waste water, reduce the COD of dyeing waste water CrWith the BOD value, play the effect that purifies water.And the present invention is particularly outstanding to the effect of dispersed dye and coating waste-water processing, and decolorization rate of wastewater surpasses 85%, COD CrClearance greater than 75%.Composite type polymeric flocculant, preparation method and application can be used for the processing of fabrics printing and dyeing waste water.

The present invention is the method that adopts coagulation, with composite flocculant to the processing of decolouring of the dyestuff in the dyeing waste water and coating.Since such flocculation agent hydrolysate can with suspended substance colloidal solid generation compression double electric layer and charge neutrality effect in the water, make in the waste water between the suspended substance colloidal impurity " adhesion " and " bridge formation ", therefore in downward settling process, impurity particle in the water is carried out " sweeping network ", and make it to be removed.

The preparation method of composite flocculant of the present invention, be that aluminium, iron ion are prepared into the polymeric ferric aluminum flocculation agent earlier, then such flocculation agent and selected inorganic or organic polymer coagulant aids o'clock are refluxed in 40 ℃～70 ℃ of controlled temperature and pH=3～5 in reactor, stirred 1～3 hour the promptly compound composite high-molecular flocculation agent that is prepared into fast.

High efficiency composite flocculant of the present invention can be expressed as: X+Y.Wherein, X is a flocculation agent, and this flocculation agent is mainly polymeric ferric aluminum or poly-aluminium.Y is a coagulant aids, mainly contains two big classes, and a class is an inorganics as water glass, the inorganic coagulant aids Z of calcium hydroxide, lime carbonate, magnesium hydroxide or polymer etc.; Another kind of is organism as polyacrylamide, dodecyl dimethyl tertiary amine, Dyhard RU 100 or modified chitosan etc.Utilize these coagulant aidss and polymeric ferric aluminum, poly-reactive aluminum or the compound composite flocculant that is prepared into higher stability.Wherein the apparent in view coagulant aids of effect is the composite flocculant of inorganic coagulant aids Z of polymer and organism dodecyl dimethyl tertiary amine.

Special recommendation inorganic polymer coagulant aids Z of the present invention, it is to adopt chemical reagent such as inorganic sodium, is dissolved in the distilled water, is adjusted to required pH value with acid, under 50～60 ℃, back flow reaction 30～45 minutes is formed.Its feature is to accelerate the formation of flocs unit, and makes it become thick, closely knit, and also has good cohesion under low water temperature, low basicity condition.Inorganic polymer coagulant aids Z primary structure is as follows:

Wherein: n=5～15.

The AlO that its energy and polymeric ferric aluminum hydrolysis generate 4Al 12(OH) 24 7+And Fe 3+Be compounded to form the macromolecule flocculation agent of wire, branch's chain or spherical particle, with effects such as suspended substance in the water and colloidal solid generation compression double electric layer, charge neutrality, " bridge formations ", impurity particle in the water is carried out " sweeping network ", and make it to remove, particularly particularly evident to the decolorizing effect of coating and dispersed dye.

The preparation method of composite type polymeric flocculant of the present invention specifically can be divided into two processes:

1, the preparation of polymeric ferric aluminum flocculation agent

In water, the pH value is that aluminum chloride and ferric sulfate weight ratio are 1: 0.5～1.5 under 2～4 and 40 ℃～70 ℃ conditions, backflow stirring reaction 0.5～2 hour; Described water is distilled water preferably.

2, the preparation of composite high-molecular flocculation agent

In distilled water, under pH=3～5 and 40～70 ℃, flocculation agent and coagulant aids reflux and stirred 1～3 hour, compoundly obtain pale brown look composite flocculant; The weight ratio of polymeric ferric aluminum and coagulant aids is 1: 0.03～1.0.

Described coagulant aids can for inorganics as water glass, calcium hydroxide, lime carbonate, magnesium hydroxide or above-mentioned polymer inorganic coagulant aids etc.; Or organism, as: polyacrylamide, dodecyl dimethyl tertiary amine, Dyhard RU 100 and modified chitosan etc.

The inorganic coagulant aids of described polymer is in the aqueous solution, and water glass and silicon oxide weight ratio are 2: 0.8～1.2, regulates pH=3～4 with dilute sulphuric acid, dilute hydrochloric acid or acetic acid, and backflow, stirring reaction are 30～45 minutes under 50～60 ℃; Described water is distilled water preferably.

Restrain silicon oxide as restraining water glass, 10 with 20, be dissolved in 100 ml distilled waters, regulate pH=3～4 with dilute sulphuric acid, dilute hydrochloric acid or acetic acid, backflow, stirring reaction are 30～45 minutes under 50～60 ℃, promptly obtain the coagulant aids of n=8.

Composite flocculant preparation method of the present invention is easy, and cost is low, and is easy to use, not only water-soluble dye commonly used is had certain flocculating decoloring effect, and non-water-soluble dispersed dye and coating etc. are also had good adsorption bleaching ability.Composite flocculant A, the B of especial manufacture of the present invention and C are as the new type compound flocculation agent, both had aluminum ion and iron ion compression double electric layer and electrically neutral effect, the adsorption bridging, the volume that have coagulant aids are again swept function, can remove the contaminant particles in the waste water effectively.In pH value 5～8 scopes, settling time 2～3h has flocculating effect preferably to water-soluble dye in the dyeing waste water and the dispersed dye that are difficult to remove and coating when consumption is 100～150ppm.Especially obvious especially to dispersed dye and coating effect, its colourity percent of decolourization 〉=85%, the clearance of CODcr 〉=75%.

Embodiment:

Will be further understood that the present invention by following embodiment, but can not limit content of the present invention.

The preparation of embodiment 1 composite type inorganic polymer flocculating agent A

1, the preparation of polymeric ferric aluminum flocculation agent

Get aluminum chloride 30 grams respectively in 1: 0.7 ratio, ferric sulfate 21 grams place reaction flask, add the distilled water of 400mL, and at 50 ℃～60 ℃, the pH value is a backflow stirring reaction 0.5～1 hour under 2～3 conditions.

2, the preparation of coagulant aids

With 20 gram water glass, 10 gram silicon oxide, be dissolved in 100 ml distilled waters, regulate pH=3～4 with sulfuric acid or hydrochloric acid, backflow, stirring reaction are 30～45 minutes under 50～60 ℃, promptly obtain coagulant aids.(n＝8)。

3, the polymeric ferric aluminum flocculation agent becomes flocculating agent A with coagulant aids Z prepared in reaction

The synthetic polymeric ferric aluminum is placed reaction flask,, under the condition of pH=3～4, slowly add coagulant aids (inorganic macromolecule compound n=8) 0.9 gram, reflux and stirred 1～1.5 hour at 40 ℃～50 ℃.After finishing, reaction promptly obtains pale brown look transparent composite flocculant A.

The preparation of embodiment 2 composite type polymeric flocculant B

1, the preparation of polymeric ferric aluminum flocculation agent

Get aluminum chloride 20 grams respectively in 1: 0.7 ratio, ferric sulfate 14 grams place reaction flask, add the distilled water of 270mL, and at 50 ℃～60 ℃, the pH value is a backflow stirring reaction 0.5～1 hour under 2～3 conditions.

2, polymeric ferric aluminum flocculation agent and coagulant aids dodecyl dimethyl tertiary amine are compounded to form flocculating agent B the synthetic polymeric ferric aluminum are placed reaction flask, at 40 ℃～50 ℃, under the condition of pH=3～4, slowly add coagulant aids dodecyl dimethyl tertiary amine 20 grams, reflux and stirred 1.5～2 hours.Promptly obtain flaxen composite flocculant B after compound the finishing.

The preparation of embodiment 3 composite inorganics-organic polymer coargulator C

1, the preparation of composite type inorganic polymer flocculating agent A

34 gram polymeric ferric aluminums are placed reaction flask, add the distilled water of 270mL,, under the condition of pH=3～4, slowly add coagulant aids (inorganic macromolecule compound n=8) 2 grams, reflux and stirred 1～1.5 hour at 40 ℃～50 ℃.After finishing, reaction promptly gets pale brown look transparent composite flocculant A.

2, flocculating agent A and dodecyl dimethyl tertiary amine are compounded to form flocculation agent C

The synthetic flocculating agent A is placed reaction flask, under 50～60 ℃ condition, slowly add dodecyl dimethyl tertiary amine 20 grams, reflux and stirred 1.5～2 hours.Can obtain pale brown look composite flocculant C.

The application of embodiment 4 composite flocculants in water-soluble dye wastewater

The consumption of composite flocculant:

Embodiment 1 flocculating agent A 100ppm

Embodiment 2 flocculating agent B 150ppm

Embodiment 3 flocculation agent C 120ppm

Treatment process:

With volumetric molar concentration is composite flocculant A, B, the C of 0.36mol/L, join respectively by above-mentioned consumption in the dyeing waste waters such as Xylene Red 3R dyestuff, Reactive blue X-BR dyestuff and direct acid blue 5B dyestuff (waste strength is 0.04g/L), stirred 10～15 minutes, under the condition of pH=5～8, its percent of decolourization is measured in sedimentation 2～3 hours then.

Result sees Table 1.

Table 1 flocculation agent is to the flocculating decoloring effect of water-soluble dye wastewater

The application of embodiment 5 composite flocculants in dispersed dye and coating waste-water

The consumption of composite flocculant:

Embodiment 1 flocculating agent A 75～100ppm

Embodiment 2 flocculating agent B 100～150ppm

Embodiment 3 flocculation agent C 100～120ppm

Treatment process:

With volumetric molar concentration is composite flocculant A, B, the C of 0.4mol/L, join respectively by above-mentioned consumption that (waste strength is 0.03～0.04g/L) in the blue waste water of EX-SF DISPERSE BLUE EX-SF 300 HGL dyestuff and coating, stirred 10～15 minutes, under the condition of pH=5～8, its percent of decolourization is measured in sedimentation 3 hours then.

Result sees Table 2.

Table 2 flocculation agent is to the flocculating decoloring effect of dispersed dye and coating waste-water

Embodiment 6 coagulant aids Z are to the influence of dispersed dye and coating waste-water decoloration performance

Change water glass and silicon oxide consumption, can obtain multi-form coagulant aids: n respectively and be respectively 5,8,12.

Coagulant aids Z (n=5,8,12) and polymeric ferric aluminum reaction are formed composite flocculant A, and be used for the decolouring processing of dispersed dye and coating waste-water.

Treatment process:

With volumetric molar concentration is the composite flocculant A of 0.4mol/L, consumption is that 75～100ppm joins respectively that (waste strength is 0.03～0.04g/L) in the blue waste water of EX-SF DISPERSE BLUE EX-SF 300 HGL dyestuff and coating, stirred 10～15 minutes, under the condition of pH=5～8, its percent of decolourization is measured in sedimentation 3 hours then.

Result sees Table 3.

Table 3 flocculation agent is to the flocculating decoloring effect of dispersed dye and coating waste-water

COD after embodiment 7 dispersed dye and coating are handled with flocculating agent A CrValue changes

Treatment process:

In strongly acidic solution, accurately add excessive potassium bichromate standardized solution, reflux, with reducing substances (being mainly organism) oxidation in dispersed dye and the coating waste-water sample (the waste water sample amount of getting must not be less than 5ml), excessive potassium bichromate is made indicator with phenanthroline ion, with ferrous ammonium sulphate standardized solution residual titration, calculate the water sample chemical oxygen demand (COD) according to consumption potassium bichromate standardized solution amount, calculate COD then CrClearance:

COD CrClearance (%)=(COD Cr0-COD Cr1)/COD Cr0* 100%

Result sees Table 4.

COD before and after table 4 dispersed dye and coating waste-water are handled CrValue

Claims (7)

1. a high efficiency composite flocculant is characterized in that being composited by flocculation agent and coagulant aids,
Wherein: flocculation agent is a polymeric ferric aluminum; Coagulant aids is dodecyl dimethyl tertiary amine or the inorganic coagulant aids of polymer with following structural formula:
Wherein: n=5～15; Wherein the weight ratio of aluminium, iron and coagulant aids is 1: 0.5～1.5: 0.03～1.
2. the preparation method of a high efficiency composite flocculant as claimed in claim 1 is characterized in that being obtained by following two one step process:
(1) in water and under 40 ℃～70 ℃, the weight ratio of aluminum chloride and ferric sulfate is that 1: 0.5～1.5 o'clock, pH value are back flow reaction acquisition in 0.5～2 hour polymeric ferric aluminum flocculation agent under 2～4 conditions;
(2) with the polymeric ferric aluminum of (1) and coagulant aids under the condition of 40 ℃～70 ℃ and pH=3～5, refluxing to stir obtained pale brown look transparent composite flocculant in 1～3 hour; Wherein: the weight ratio of polymeric ferric aluminum and coagulant aids is 1: 0.03～1.0;
Described flocculation agent and coagulant aids are according to claim 1.
3. the preparation method of a high efficiency composite flocculant as claimed in claim 2, it is characterized in that the inorganic coagulant aids of described polymer is in the aqueous solution, the weight ratio of sodium silicate and silicon oxide is that 2: 0.8～1.2 o'clock usefulness dilute sulphuric acid, dilute hydrochloric acid or acetic acid are regulated pH=3～4, and backflow, stirring reaction are 30～45 minutes under 50～60 ℃.
4. the preparation method of a high efficiency composite flocculant as claimed in claim 2 is characterized in that described water is distilled water.
5. the purposes of a kind of high efficiency composite flocculant as claimed in claim 1 is characterized in that being used for the flocculation decoloration processing of dyeing waste water.
6. the purposes of a kind of high efficiency composite flocculant as claimed in claim 5 is characterized in that described dyeing waste water is the waste water of the water-soluble dye wastewater of matching stain, reactive dyestuffs and substantive dyestuff; It perhaps is the water-insoluble dyeing waste water that is difficult to remove of dispersed dye or coating waste-water.
7. the purposes of a kind of high efficiency composite flocculant as claimed in claim 6, it is characterized in that with volumetric molar concentration being that the described composite flocculant of 0.3～0.4mol/L joins in the dyeing waste water, stirred 10～15 minutes, under the condition of pH=5～8, sedimentation 3 hours.
CNB2005100308348A 2005-10-28 2005-10-28 High efficiency composite flocculant, its preparation method and application CN100386267C (en)

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