CN104692510A - Preparation method for solid polymer ferric sulfate zinc flocculant - Google Patents
Preparation method for solid polymer ferric sulfate zinc flocculant Download PDFInfo
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Abstract
The invention relates to a preparation method for solid polymer ferric sulfate zinc flocculant. The preparation method comprises the steps that firstly, solid seven-hydrate ferrous sulfate is acidized through concentrated sulfuric acid; secondly, sodium chlorate is added into the mixture and stirred slowly so that tan uniform liquid can be formed; thirdly, solid zinc sulfate is added into the liquid and mixed with the liquid to be uniform, and solid powdery zinc sulfate is added again and stirred slowly to be completely dissolved; afterwards, carbon oxidation materials are added so that the curing rate of the flocculant can be increased, and water bath heating is performed; finally, dry heating and room-temperature curing are performed through an electric jacket, so the faint yellow solid polymer ferric sulfate zinc flocculant can be obtained in a short time. According to the preparation method, none of waste liquid, waste residue and waste gas are produced in the production process; the curing rate of the product is high, mass distribution is uniform, the content of flocculation active components is high, and the flocculation effect is good, and therefore the preparation method can be applied to treatment for industrial waste water, domestic sewage, source water and the like.
Description
Technical field
The present invention relates to the technical field of water treatment water purification agent, be specifically related to a kind of preparation method of solid ferric polysulfate zinc flocculation agent.
Background technology
Flocculation is preconditioning technique important in water technology unit operation, in colloidal solid removal, play the part of important effect.Flocculation mainly relies on some chemical substance with flocculating properties of adding, and has charge neutrality, adsorption bridging, net catch volume and the several functions such as to sweep.The current this kind of chemical substance be widely adopted mainly includes machine polymeric flocculant and inorganic polymer flocculant.Inorganic polymer flocculant mainly comprises the large class of iron system and aluminium system two, and wherein polymerize aluminum chloride and bodied ferric sulfate are Typical Representatives.They have different flocculating properties in water treatment applications.
There is potential toxicity and secondary pollution problem in AlSnSi alloy, and presents the shortcomings such as flocculation volume is little, loose, sedimentation is slow, and then caused the development of iron-based flocculation agent, and the iron-based flocculation agent that research and development usefulness is high becomes important study hotspot already.Iron-based flocculation agent, in application process, finds the problems such as liquid flocculation agent stability relative mistake, communications and transportation inconvenience, which has limited the propagation and employment of iron-based flocculation agent.
Prepare the problem that solid flocculant can solve liquid flocculation agent unstable and transport inconvenience, promote applying of iron-based flocculation agent.The preparation of the solid silicic acid iron-based flocculation agent applied in the market operates relative complex because the unstable of silicic acid sill result in preparation technology; Other solid flocculant is also is mostly to be obtained through spraying dry by liquid product or add other auxiliary agent such as diatomite, clay and sodium bentonite, adds energy consumption and potentially reduces flocculation activity composition.
Summary of the invention
For the problems referred to above that prior art exists, the object of this invention is to provide the synthetic method of the solid ferric polysulfate zinc flocculation agent that the preparation of a kind of technique is simple, usefulness is high.
For realizing the object of the invention, the present invention adopts following technical scheme: a kind of preparation method of solid ferric polysulfate zinc flocculation agent, specifically comprises the steps:
S1: under normal temperature condition, mixes the vitriol oil of 3 ~ 6 ml 98% with iron vitriol, and moderate-speed mixer is to forming homogeneous paste mixture;
S2: slowly drip sodium chlorate in the pasty mixture of the vitriol oil of iron vitriol and 3 ~ 6 ml 98%, low rate mixing carries out oxidizing reaction;
S3: to be mixed evenly after, add pressed powder zinc sulfate, by Fe/Zn mol ratio 8:1 ~ 3:2, slowly stir and pressed powder zinc sulfate is fully dissolved;
S4: after pressed powder zinc sulfate dissolves completely, add oxidation of coal material or distilled water that 10 ~ 20 ml concentration are 8 ~ 32 mg/L, heating in water bath 40 ~ 60 min, the polyreaction and moderate-speed mixer is hydrolyzed, the temperature of water-bath is 20 ~ 80 DEG C;
S5: in water-bath process, slowly adds 2.01 ~ 4.035g sodium carbonate solid powder:, guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtains flocculation agent first product;
S6: adopt electric mantle at the temperature of 80 DEG C ~ 100 DEG C, heat 5 ~ 10 minutes to flocculation agent first product is micro-boil, low rate mixing 1 ~ 2 min minute after cooling, after leaving standstill slaking 6-72h, can obtain mass distribution uniform faint yellow solid bodied ferric sulfate zinc flocculation agent.
As optimization, the oxidation of coal material in described S4 is graphene oxide.
As optimization, leaving standstill the curing time in described S6 is 6-12h.
Relative to prior art, tool of the present invention has the following advantages:
(1) main raw material that product preparation of the present invention uses is titanium dioxide industry byproduct, and raw material sources are extensive, low production cost; The preparation technology's flow process adopted is simple, easy to operate, easy to control, energy consumption is low, and short period of time normal temperature slaking can form the uniform solid flocculant of mass distribution.
(2) just can obtain solid flocculant without the need to adding the auxiliary agents such as such as clay, diatomite, sodium bentonite, improve the active constituent content of flocculation agent; The present invention adds solid sodium carbonate powder and regulates flocculation agent basicity, and the oxidation of coal material of the low levels of interpolation has the advantage accelerating curing speed, can significantly improve product preparation efficiency.
(3) whole preparation process is without the generation of waste liquid, waste residue, waste gas, more environmental protection.
(4) what prepared by the present invention is a kind of solid flocculant, is faint yellow solid, soluble in water; Under normal temperature, stable chemical nature, for a long time storage is never degenerated, and compares liquid product and can to store in a long time and flocculating property is stablized, be convenient to transport.
(5) it is convenient that the solid flocculant that prepared by the present invention is applied, and both directly can add solid phase prod, and also add use again after dissolvable solid product.Product is applicable to process various water bodies, such as source water, trade effluent and sanitary sewage.Product flocculation mark sheet present alumen ustum formation speed is fast, residual turbidity is low, COD, TOC, NH
4-N clearance and percent of decolourization high.
Embodiment
Term in the present invention, rapid stirring refers to that stirring velocity is greater than 200 rpm/min, moderate-speed mixer refers to that stirring velocity is 100-200 rpm/min, and low rate mixing refers to that stirring velocity is 100-50 rpm/min, slowly stirs and refers to that stirring velocity is less than 50 rpm/min.
Micro-boiling refers to that fluid surface starts state when there are small bubbles.
embodiment 1
A preparation method for solid ferric polysulfate zinc flocculation agent, under normal temperature condition, mixed with 54.3 g titanium dioxide industry byproduct iron vitriols by the vitriol oil of 3 ml 98%, moderate-speed mixer mixture is to forming uniform mashed prod; Then slowly drip 10.85 ml sodium chlorate (concentration 3M) low rate mixings and carry out fully oxidized reaction; After question response stirs mutually, by Fe/Zn mol ratio 2:1, add pressed powder zinc sulfate, slowly stir and make it dissolve completely; Add the oxidation of coal material solution that 10 ml concentration are 16 mg/L; Heating in water bath is hydrolyzed polyreaction, and moderate-speed mixer, bath temperature is 60 DEG C, and heat-up time is 40 min; In water-bath process, slowly add 2.69 g sodium carbonate solid powder, and guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtain liquid flocculation agent first product; At 80 DEG C ~ 100 DEG C temperature, electric mantle is heated to that liquid flocculation agent first product is micro-to boil, low rate mixing 2 min minute after cooling, stores Vandyke brown liquid flocculant product; Leave standstill slaking 6-12h, the uniform faint yellow gluey solid ferric polysulfate zinc product of mass distribution can be obtained.
embodiment 2
A preparation method for solid ferric polysulfate zinc flocculation agent, under normal temperature condition, mixed with 54.3 g titanium dioxide industry byproduct iron vitriols by the vitriol oil of 5.3 ml 98%, moderate-speed mixer mixture is to forming uniform mashed prod; Then slowly drip 10.85 ml sodium chlorate (concentration 3M) low rate mixings and carry out fully oxidized reaction; After question response stirs mutually, by Fe/Zn mol ratio 8:1, add pressed powder zinc sulfate, slowly stir and make it dissolve completely; Add the oxidation of coal material solution that 15ml concentration is 16 mg/L; Heating in water bath is hydrolyzed polyreaction, and moderate-speed mixer, bath temperature is 30 DEG C, and heat-up time is 50 min; In water-bath process, slowly add 2.69 g sodium carbonate solid powder, and guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtain liquid flocculation agent first product; At 80 DEG C ~ 100 DEG C temperature, electric mantle is heated to that liquid flocculation agent first product is micro-to boil, low rate mixing 2 min minute after cooling, stores Vandyke brown liquid flocculant product; Leave standstill slaking 24-48h, the uniform faint yellow gluey solid ferric polysulfate zinc product of mass distribution can be obtained.
embodiment 3
A preparation method for solid ferric polysulfate zinc flocculation agent, under normal temperature condition, mixed with 54.3 g titanium dioxide industry byproduct iron vitriols by the vitriol oil of 4.5ml 98%, moderate-speed mixer mixture is to forming uniform mashed prod; Then slowly drip 10.85 ml sodium chlorate (concentration 3M) low rate mixings and carry out fully oxidized reaction; After question response stirs mutually, by Fe/Zn mol ratio 6:1, add pressed powder zinc sulfate, slowly stir and make it dissolve completely; Add the oxidation of coal material solution that 18 ml concentration are 16 mg/L; Heating in water bath is hydrolyzed polyreaction, and moderate-speed mixer, bath temperature is 60 DEG C, and heat-up time is 40 min; In water-bath process, slowly add 3.05g sodium carbonate solid powder, and guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtain liquid flocculation agent first product; At 80 DEG C ~ 100 DEG C temperature, electric mantle is heated to that liquid flocculation agent first product is micro-to boil, low rate mixing 2 min minute after cooling, stores Vandyke brown liquid flocculant product; Leave standstill slaking 48-72h, the uniform faint yellow gluey solid ferric polysulfate zinc product of mass distribution can be obtained.
embodiment 4
A preparation method for solid ferric polysulfate zinc flocculation agent, under normal temperature condition, mixed with 54.3 g titanium dioxide industry byproduct iron vitriols by the vitriol oil of 5ml 98%, moderate-speed mixer mixture is to forming uniform mashed prod; Then slowly drip 10.85 ml sodium chlorate (concentration 3M) low rate mixings and carry out fully oxidized reaction; After question response stirs mutually, by Fe/Zn mol ratio 2:1, add pressed powder zinc sulfate, slowly stir and make it dissolve completely; Add the oxidation of coal material solution that 20ml concentration is 16 mg/L; Heating in water bath is hydrolyzed polyreaction, and moderate-speed mixer, bath temperature is 60 DEG C, and heat-up time is 40 min; In water-bath process, slowly add 2.01g sodium carbonate solid powder, and guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtain liquid flocculation agent first product; At 80 DEG C ~ 100 DEG C temperature, electric mantle is heated to that liquid flocculation agent first product is micro-to boil, low rate mixing 1 min minute after cooling, stores Vandyke brown liquid flocculant product; Standing slaking is less than 6h, can obtain the uniform faint yellow gluey solid ferric polysulfate zinc product of mass distribution.
embodiment 5
A preparation method for solid ferric polysulfate zinc flocculation agent, under normal temperature condition, mixed with 54.3 g titanium dioxide industry byproduct iron vitriols by the vitriol oil of 6ml 98%, moderate-speed mixer mixture is to forming uniform mashed prod; Then slowly drip 10.85 ml sodium chlorate (concentration 3M) low rate mixings and carry out fully oxidized reaction; After question response stirs mutually, by Fe/Zn mol ratio 3:2, add pressed powder zinc sulfate, slowly stir and make it dissolve completely; Add the oxidation of coal material solution that 20 ml concentration are 16 mg/L; Heating in water bath is hydrolyzed polyreaction, and moderate-speed mixer, bath temperature is 60 DEG C, and heat-up time is 40 min; In water-bath process, slowly add 2.69 sodium carbonate solid powder, and guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtain liquid flocculation agent first product; At 80 DEG C ~ 100 DEG C temperature, electric mantle is heated to that liquid flocculation agent first product is micro-to boil, low rate mixing 2 min minute after cooling, stores Vandyke brown liquid flocculant product; Standing slaking is less than 6h, can obtain the uniform faint yellow gluey solid ferric polysulfate zinc product of mass distribution.
embodiment 6
A preparation method for solid ferric polysulfate zinc flocculation agent, under normal temperature condition, mixed with 54.3 g titanium dioxide industry byproduct iron vitriols by the vitriol oil of 5.32ml 98%, moderate-speed mixer mixture is to forming uniform mashed prod; Then slowly drip 10.85 ml sodium chlorate (concentration 3M) low rate mixings and carry out fully oxidized reaction; After question response stirs mutually, by Fe/Zn mol ratio 2:1, add pressed powder zinc sulfate, slowly stir and make it dissolve completely; Add the oxidation of coal material solution that 12 ml concentration are 8 mg/L; Heating in water bath is hydrolyzed polyreaction, and moderate-speed mixer, bath temperature is 60 DEG C, and heat-up time is 60 min; In water-bath process, slowly add 2.69 sodium carbonate solid powder, and guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtain liquid flocculation agent first product; At 80 DEG C ~ 100 DEG C temperature, electric mantle is heated to that liquid flocculation agent first product is micro-to boil, low rate mixing 2 min minute after cooling, stores Vandyke brown liquid flocculant product; Standing slaking is less than 12h, can obtain the uniform faint yellow gluey solid ferric polysulfate zinc product of mass distribution.
embodiment 7
A preparation method for solid ferric polysulfate zinc flocculation agent, under normal temperature condition, mixed with 54.3 g titanium dioxide industry byproduct iron vitriols by the vitriol oil of 6ml 98%, moderate-speed mixer mixture is to forming uniform mashed prod; Then slowly drip 10.85 ml sodium chlorate (concentration 3M) low rate mixings and carry out fully oxidized reaction; After question response stirs mutually, by Fe/Zn mol ratio 2:1, add pressed powder zinc sulfate, slowly stir and make it dissolve completely; Add the oxidation of coal material solution that 14ml concentration is 32 mg/L; Heating in water bath is hydrolyzed polyreaction, and moderate-speed mixer, bath temperature is 80 DEG C, and heat-up time is 40 min; In water-bath process, slowly add 4.035 sodium carbonate solid powder, and guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtain liquid flocculation agent first product; At 80 DEG C ~ 100 DEG C temperature, electric mantle is heated to that liquid flocculation agent first product is micro-to boil, low rate mixing 2 min minute after cooling, stores Vandyke brown liquid flocculant product; Standing slaking is less than 6h, can obtain the uniform faint yellow gluey solid ferric polysulfate zinc product of mass distribution.
coagulation performance is tested:adopt its coagulation performance of flocculation agent that the checking of beaker coagulation test adopts the inventive method to prepare.
The concrete operations of coagulation test are: under room temperature condition, adopt six agitators to carry out coagulation test, dispensing and timing.Coagulation experiment process is: deposit the former water of 1L process in the circular beaker of 1L.
Coagulation process condition is set as: rapid stirring speed 250 rpm, rapid stirring time 2 min, moderate-speed mixer speed 150 rpm, moderate-speed mixer time 5 min, low rate mixing speed 40 rpm, low rate mixing time 10 min.After coagulation stirs, water sample leaves standstill 30 min, gets 2 centimeters supernatant liquors under liquid level, carries out water sample analysis fast.
Coagulation experiment is carried out to coagulating agent prepared by embodiment 1-4.Result shows: the sanitary sewage of coagulation 200 NTU and 400 mg/L COD, residual turbidity and COD clearance be less than respectively 5 NTU with between 85%-75%; Coagulation 0.054 UV
254cm
-1slightly-polluted raw water, remaining UV
254between 0.020-0.030 cm
-1, residual turbidity is less than 2 NTU; Coagulation 250 NTU simulates kaolin solution, and residual turbidity is less than 0.65 NTU, standard deviation (STD) 0.04.Wherein, as standing slaking 6-12h, effect is the most desirable.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (3)
1. a preparation method for solid ferric polysulfate zinc flocculation agent, is characterized in that, specifically comprises the steps:
S1: under normal temperature condition, mixes the vitriol oil of 3 ~ 6 ml 98% with iron vitriol, and moderate-speed mixer is to forming homogeneous paste mixture;
S2: slowly drip sodium chlorate in the pasty mixture of the vitriol oil of iron vitriol and 3 ~ 6 ml 98%, low rate mixing carries out oxidizing reaction;
S3: to be mixed evenly after, add pressed powder zinc sulfate, by Fe/Zn mol ratio 8:1 ~ 3:2, slowly stir and pressed powder zinc sulfate is fully dissolved;
S4: after pressed powder zinc sulfate dissolves completely, add oxidation of coal material or distilled water that 10 ~ 20 ml concentration are 8 ~ 32 mg/L, heating in water bath 40 ~ 60 min, the polyreaction and moderate-speed mixer is hydrolyzed, the temperature of water-bath is 20 ~ 80 DEG C;
S5: in water-bath process, slowly adds 2.01 ~ 4.035g sodium carbonate solid powder:, guarantee that moderate-speed mixer is to liquid bubble completely dissolve, obtains flocculation agent first product;
S6: adopt electric mantle at the temperature of 80 DEG C ~ 100 DEG C, heat 5 ~ 10 minutes to flocculation agent first product is micro-boil, low rate mixing 1 ~ 2 min minute after cooling, after leaving standstill slaking 6-72h, can obtain mass distribution uniform faint yellow solid bodied ferric sulfate zinc flocculation agent.
2. the preparation method of solid ferric polysulfate zinc flocculation agent as claimed in claim 1, it is characterized in that, the oxidation of coal material in described S4 is graphene oxide.
3. the preparation method of solid ferric polysulfate zinc flocculation agent as claimed in claim 1 or 2, is characterized in that, leaving standstill the curing time in described S6 is 6-12h.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109174058A (en) * | 2018-09-18 | 2019-01-11 | 渤海大学 | The preparation method of secondary chlorine white clay adsorbing material for depth removal complex state chromium |
CN110723774A (en) * | 2019-10-16 | 2020-01-24 | 山西大学 | Polymeric copper sulfate and iron inorganic composite water purifying agent and preparation method and application thereof |
CN110819806A (en) * | 2019-11-01 | 2020-02-21 | 郴州丰越环保科技有限公司 | Preparation method for preparing zinc iron sulfate flocculating agent from germanium extraction liquid |
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JP2011131167A (en) * | 2009-12-24 | 2011-07-07 | Daiyanitorikkusu Kk | Flocculation treatment method of waste water |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109174058A (en) * | 2018-09-18 | 2019-01-11 | 渤海大学 | The preparation method of secondary chlorine white clay adsorbing material for depth removal complex state chromium |
CN110723774A (en) * | 2019-10-16 | 2020-01-24 | 山西大学 | Polymeric copper sulfate and iron inorganic composite water purifying agent and preparation method and application thereof |
CN110819806A (en) * | 2019-11-01 | 2020-02-21 | 郴州丰越环保科技有限公司 | Preparation method for preparing zinc iron sulfate flocculating agent from germanium extraction liquid |
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