CN101215031A - Method for preparing clay composite flocculant - Google Patents
Method for preparing clay composite flocculant Download PDFInfo
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- CN101215031A CN101215031A CNA2007103008984A CN200710300898A CN101215031A CN 101215031 A CN101215031 A CN 101215031A CN A2007103008984 A CNA2007103008984 A CN A2007103008984A CN 200710300898 A CN200710300898 A CN 200710300898A CN 101215031 A CN101215031 A CN 101215031A
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- clay
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- flocculating agent
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Abstract
The invention belongs to the technical field of water curing medicine, in particular to a process for preparing a clay complex flocculating agent. In a certain condition, purify modified clay and Al-hydroxy-polymerization solution to make reaction to prepare 1 clay complex flocculating agent, the invention further adopt acid pickle from clay modification to prepare 2 clay complex flocculating agent, (1) clay purification is, clay mineral and water is marinated (1-48h) according to solid-to-liquid ratio (0.1-2): (1-20), then add sodium pyrophosphate of which the weight is equivalent to that of clay raw mineral, stir and scatter the clay (1-3h), then stew and precipitate the clay (1-48h), take the upper layer suspension, filter, wash and dry the upper layer suspension, then achieve clay with purity quotient up to 99 percent, which are SiO2 50-53%, Al2O3 3.5-5%, Fe2O3 2-3%, FeO 0.1-0.4%, CaO 4-6%, MgO 18-25%, (2) clay modification is, <1> skive and sift out purified clay, add hydrochloric acid to proceed acid modification, then filter clay, further wash, filter and dry the modified clay after acid modifying the filtered solid matter, then use sulphuric acid to adjust pH value to make the clay to be modified clay of hydroxide radical metallic ion solution, then proceed aging and polymerization in a constant temperature, and further dry, burn, skive and sift out the clay to make 1 clay complex flocculating agent, <2> use filtrate after being filtered and filtrate after being washed in <1> to form mixed filtrate, then use the mixed filtrate to prepare poly silicic acid solution, and further prepare 2 clay complex flocculating agent with aging in a constant temperature.
Description
Technical field
The present invention the invention belongs to the water treatment agent technical field, relates in particular to a kind of preparation method of clay composite flocculant.
Background technology
As everyone knows, present method of wastewater treatment has multiple, mainly contains physics biochemistry, ion-exchange, absorption, chemical oxidation, electrodialysis and Coagulation Method etc.Coagulation Method is to generally believe a kind of not only economy but also easy important method that improves water treatment efficiency at present both at home and abroad.Show according to pertinent data: in the wastewater treatment of domestic and international multiple industry, Coagulation Method water treatment ratio accounts for 55%～75%; Tap water industry almost 100% uses Coagulation Method as the water purification means.
But traditional flocculant can not satisfy more and more high-level water treatment market demand at aspects such as economy, securities, utilize discarded metals such as aluminium, iron and depleted hydrochloric acid, sulfuric acid to prepare various inorganic type flocculation agents, its Costco Wholesale is no doubt very low, but contain a large amount of heavy metals and other objectionable impurities in depleted metal-salt and the spent acid, seriously jeopardize ecological safety, human health and ecosystem health are constituted a serious threat.
And the organic polymer coargulator synthesis material mainly is non-renewable resources such as oil, degraded by environmental microorganism or recycle unrealistic in the use back, be unfavorable for Sustainable development human and society, do not conform to the environmental protection concept of Green Chemistry and industrial ecology.
For trying to achieve safer flocculation agent, the researchist has attempted many new ways in the hope of ideal results.The process of flocculation agent development is not difficult to find out in the world wide, its development trend be by low molecule to polymer, from single type to compound.Be that raw material is developed novel organic polymer coargulator becomes research with alternative existing traditional flocculant focus with natural organic high-molecular, microorganism in recent years.But the screening of existing microbial bacterial, cultivate, fermentation and extract the method for agglutinating matter and production process complexity, production cost too high, only rest on laboratory stage, the report of implementing extensive industrialization does not at home and abroad almost have.
Restriction novel flocculant mass market key in application is the quality of product at present, the content that comprises five aspects: production cost, transportation cost, use cost, treatment effect and mud subsequent disposal etc., wherein the production cost of novel flocculant plays a decisive role.
Consider based on the market requirement and environmental protection industry characteristics; development, development of new economy, nontoxic, flocculating property is high, non-secondary pollution, environmentally friendly, cheap composite flocculant are the task of top priority; provide new approaches to the development that promotes flocculation agent research, significant to environmental protection work on higher level.
Summary of the invention
In order to overcome the deficiency of existing inorganic flocculating agent and organic floculant and composite flocculation agent, the invention provides a kind of more efficiently, more inexpensive, easy to operate, non-secondary pollution, environmentally friendly, to the preparation method of the harmless clay composite flocculant of HUMAN HEALTH.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of clay composite flocculant, its special character is: under certain conditions with purification modified clay and hydroxy aluminum solion polymerization reaction take place preparation 1
#Clay composite flocculant; Also utilize the spent acid solution preparation 2 of clay alteration
#Clay composite flocculant:
(1) clay is purified and is: former clay pit and water are pressed solid-to-liquid ratio (0.1-2): (1-20) soak (1-48h), add the trisodium phosphate that is equivalent to clay raw ore weight (0.5-2%) again, dispersed with stirring (1-3h), staticly settle (1-48h) again, get upper strata suspension, suction filtration, washing, drying get final product to such an extent that purity reaches 99% clay, i.e. SiO
250-53%, Al
2O
33.5-5%, Fe
2O
32-3%, FeO 0.1-0.4%, CaO 4-6%, MgO 18-25%.
(2) clay alteration is:
1. the clay after will purifying grinds and sieves, add hydrochloric acid and carry out sour modification, acid modification after-filtration, the further washing and filtering oven dry of modified clay after solid substance acid after filtering changed, regulate pH value to 4～4.5 with sulfuric acid again, make it become hydroxy metal solion modified clay, again it is carried out 90 ℃ of constant temperature slaking polymerizations after, further oven dry, roasting, grind, sieve, make 1
#Clay composite flocculant;
2. the washing and filtering liquid formation hybrid filtering liquid to the filtered liquid after filtering and 1. is made into poly-silicate solution again, and further the constant temperature slaking makes 2
#Clay composite flocculant.
In the preparation method of above-mentioned a kind of clay composite flocculant, in clay alteration, when temperature of reaction be 60 ℃, reaction times be 10h, when concentration of hydrochloric acid is 15%, the solubility rate of the magnesium in the clay is 38.9%, at this moment, the specific surface area maximum of modified clay;
In the preparation method of above-mentioned a kind of clay composite flocculant, be feedstock production 2 with the spent acid solution of clay alteration
#The top condition of clay composite flocculant is: choosing activation pH value is 4.5, the active silicic acid of soak time 40min and the spent acid solution of clay alteration, and 1: 1 by volume, under 40 ℃ of constant temperature, slaking reaction 4.5h.
The present invention has the following advantages:
1. economic performance is good.Clay composite flocculant of the present invention, has good flocculating effect, its reason is in the flocculation pollutants in waste water, be rich in the mixture subsequently that polyhydric performance net is caught and the characteristic of building bridge makes that molecule and contaminants form big flocs unit in the water body, because molecular weight variation range big (from several thousand to hundreds of thousands of dalton) just in time satisfies the complicated diversified characteristics of contaminant molecule in the treating water.Again because the molecular weight height of mixture, floc settlement speed is faster than existing like product, show: compare when handling high-concentration waste water with polymerize aluminum chloride in the prior art (PAC), injected volume of the present invention is about the 30%-40% of PAC, in other words, its flocculating effect be equivalent to flocculant poly aluminum chloride in the prior art 2.5-3 doubly.Sludge yield is low, the mud compact structure, and moisture content is few, helps the subsequent disposal of mud.Cost is low, and " refuse " utilizes again.Carry out innoxious, recycling.
2. cost performance height.For industrial sewage or domestic sewage treating, emphasis is considered the economic benefit of water conditioner, and the flocculation agent raw materials cost accounts for the major portion of its total cost.Glue the scholar in the prescription of the present invention as main raw material, cost-effectivenes price ratio height.
3. superior product quality.The present invention is synthetic by above-mentioned prescription and manufacture craft by modified clay and inorganic flocculation salt, flocculation salt (aluminium, the iron etc.) ionic concn of handling free state in the water body of back reduces greatly, therefore, the probability of small organic contamination deposits yields free radical reduces greatly in flocculation salt (aluminium, iron etc.) the ionic catalysis water body, and " three cause material " of handling in the water body of back reduces greatly.
4. good stability of products, storage period is long.The stability quality is related to the period of storage and the result of use of product, and the storage period of existing commercially available inorganic one inorganic, inorganic-organic composite type flocculation agent is short, is generally about 1 month, and the shelf-time is long then can gelling to be occurred and lose flocculation activity.More than 12 months, this will play an important role in the commercialization process of product by the period of storage of the flocculation agent of the inventive method preparation.
5. environmentally friendly, non-secondary pollution.The present invention is because the employing modified clay is a raw material, and flocculation agent is easy to by the microbiological deterioration in the environment after implementing, and is environmentally friendly, the non-secondary pollution problem.In addition, the present invention also has the pollutent functions such as waste water that removal contains the high density heavy metal.
6. wide adaptability.Comprise paper industry waste water, beer production sewage, glutamate production sewage etc., be particularly suitable for the processing of high-concentration sewage; These sewage pollution loads are high, the additive method processing cost is higher, difficulty is big, uses this flocculation agent can reduce pollution load greatly, reduce cost for follow-up other treatment process by chemical enhanced flocculation process.
7. convenient, can implement industrialization.The inventive method is not high to equipment requirements, the reaction conditions gentleness, and making processes is simple, and different according to process object and sewage character can suitably be adjusted its prescription in described scope, handle target contaminant with maximum efficiency ground; And workable, be easy to carry out industrialization, obtain economic profit, post simultaneously creates more jobs; Emphasize whipping process and temperature controlling method in the preparation process, guaranteed that preparation process carries out fast smoothly, shortened reaction time greatly.
8. have initiative.The present invention is clay and the compound development flocculation agent of inorganic salt first, known to the contriver, does not find worldwide to have the development and the application of like product at present as yet.
9. market outlook are wide.The harmless treatment of trade effluent (making waste water etc. as dyeing and printing sewage, brewage waste water, monosodium glutamate) and recycling are difficult point and the emphasis in the water treatment industry always.Prescription of the present invention is according to the characteristics of sewage, and emphasis is in conjunction with the moiety and the discharging characteristics of sewage, within the specific limits, reduce the ratio of starch targetedly, improve the ratio of inorganic flocculation salt, make the economic performance of product better, in the hope of on market, establishing price advantage.
Description of drawings
Accompanying drawing 1 is preparation method's process flow sheet of clay composite flocculant of the present invention
Embodiment 1:
The clay pit that the present invention selects for use is taken from Jiangxi Province clay pit factory.Raw ore mainly contains three kinds of materials and forms: clay, talcum and quartz.Content through its medium clay soil of quantitative analysis is about 28%, and is quartzy 67%, talcum 2%, other 1%, the content of clay in raw ore is not very high, therefore for improving the result of use of clay, the present invention carries out purification processes to it earlier.
Preparation technology of the present invention is referring to Fig. 1, and clay is purified and adopted mechanical mixing method, during purification, is that 1: 10 amount was soaked in water 24 hours with the clay of 1000kg by solid-to-liquid ratio, treat its soak loose after, add the trisodium phosphate that is equivalent to clay weight 1%, with stirrer dispersed with stirring 2h, staticly settle.Top suspension is poured out, used the vacuum pump suction filtration, filter cake is put into baking oven dry, grinding gets final product to such an extent that purity reaches 99% clay, i.e. SiO
250-53%, Al
2O
33.5-5%, Fe
2O
32-3%, FeO 0.1-0.4%, CaO 4-6%, MgO 18-25%.Clay grinding after purifying is sieved, add hydrochloric acid and carry out sour modification, acid modification after-filtration, the further washing and filtering oven dry of modified clay after solid substance acid after filtering changed, regulate pH value with sulfuric acid again, make it become hydroxy metal solion modified clay, again it is carried out constant temperature slaking polymerization after, further oven dry, roasting, grind, sieve, make 1
#Clay composite flocculant.
Embodiment 2:
The clay pit that the present invention selects for use is taken from Jiangxi Province clay pit factory.Raw ore mainly contains three kinds of materials and forms: clay, talcum and quartz.Content through its medium clay soil of quantitative analysis is about 28%, and is quartzy 67%, talcum 2%, other 1%, the content of clay in raw ore is not very high, therefore for improving the result of use of clay, the present invention carries out purification processes to it earlier.
Preparation technology of the present invention is referring to Fig. 1, and clay is purified and adopted mechanical mixing method, during purification, is that 1: 10 amount was soaked in water 24 hours with the clay of 1000kg by solid-to-liquid ratio, treat its soak loose after, add the trisodium phosphate that is equivalent to clay weight 1%, with stirrer dispersed with stirring 2h, staticly settle.Top suspension is poured out, used the vacuum pump suction filtration, filter cake is put into baking oven dry, grinding gets final product to such an extent that purity reaches 99% clay, i.e. SiO
250-53%, Al
2O
33.5-5%, Fe
2O
32-3%, FeO 0.1-0.4%, CaO 4-6%, MgO 18-25%.Clay after purifying ground sieves, add hydrochloric acid and carry out sour modification, sour modification after-filtration, to the filtered liquid after filtering and in washing and filtering liquid form hybrid filtering liquid, be made into poly-silicate solution again, further, make 2 40 ℃ of constant temperature slaking 4h reactions
#Clay composite flocculant.
The present invention prepares flocculation agent with modified clay and hydroxy aluminum ion generation polymerization, at home and abroad still belongs to the first time, and this has not only opened up a kind of new approach for the application of clay, and has expanded the flocculation agent method of production.The utilization of modified clay spent acid solution, the improvement that had both solved spent acid solution has reached the purpose that turns waste into wealth again.
The centrifugal settling of clay raw ore disperses the preferable processing condition of purification to be: former clay pit and water are soaked 24h by solid-to-liquid ratio at 1: 10, add the trisodium phosphate that is equivalent to clay raw ore weight 1% again, dispersed with stirring 2h staticly settles 24h again, get final product the higher clay of purity.
In clay alteration, temperature of reaction, concentration of hydrochloric acid and reaction times are the principal elements that influences magnesium solubility rate in the clay, and along with the growth in temperature of reaction, concentration of hydrochloric acid and reaction times, the magnesium solubility rate increases.When temperature of reaction be 60 ℃, reaction times be 10h, when concentration of hydrochloric acid is 15%, the solubility rate of the magnesium in the clay is 38.9%, at this moment, the specific surface area maximum of modified clay.
After the dyeing waste water flocculation treatment, the processing condition that its dyestuff reclaims stir 3min for to add a certain amount of vitriol oil at dyeing waste water fast with 800r/min, stir 5min with the 260r/min middling speed, stir 5min at a slow speed with 50r/min, quiet heavy 20min.
With modified clay, poly-oxyaluminum ion is raw material synthetic 1
#The top condition of flocculation agent is: select 15%HCl for use, and 60 ℃ of constant temperature, the modified clay that modification 12h particle diameter is less and is the poly-oxyaluminum solion for preparing under 4～4.5 conditions in the pH value by solid-liquid volume ratio 1: 5, under 40 ℃ of constant temperature, polyreaction 24h.
1
#Flocculation agent flocculating effect top condition: the pH value is 6.34, and dosage is 1.5g/L, and the COD clearance reaches, and chroma removal rate reaches 98%.
1
#The simultaneous test of other flocculation agent such as flocculation agent and poly-aluminium as can be known, 1
#The pH scope of application of flocculation agent is big, and settling velocity is fast, and treatment effect is good.
Through scanning electron microscope and Infrared spectroscopy as can be known, 1
#Flocculation agent has porous by forming through modification and polyreaction, the modified clay of poly-hydroxy, excellent adsorption and contain the muriate of aluminium, magnesium, iron, calcium and comparatively the jelly of complicated polyhydroxylated polymer form.
1
#The flocculation mechanism of flocculation agent mainly contains two aspects: the one, modified clay and react with the hydroxy aluminum ion in generate the hydroxyl adsorption of complex compound; The 2nd, the throwing out of aluminium salt, magnesium salts, molysite, calcium salt.
Spent acid solution with clay alteration is a feedstock production 2
#The top condition of flocculation agent is: choosing activation pH value is 4.5, the active silicic acid of soak time 40min and the spent acid solution of clay alteration, and 1: 1 by volume, under 40 ℃ of constant temperature, slaking reaction 4.5h.
2
#Flocculation agent flocculating effect top condition: the pH value is 7.12, and best dosage is 1ml/100ml, and the COD clearance reaches, and chroma removal rate reaches more than 98%.
From 2
#Flocculation agent trial state at the scene sees that pH value subject range is bigger, and its treatment process is simple, does not need strict whipping device, and processing costs is low; The expense of recycling thioxine dyes and wastewater treatment appropriate litigation fees, to COD, colourity, turbidity removal rate height, it is neutral that processed waste water is, and using value is preferably arranged.
Claims (3)
1. the preparation method of a clay composite flocculant, its feature part is: prepare 1 with purification modified clay and hydroxy aluminum solion polymerization reaction take place under certain conditions
#Be stained with composite flocculation agent; Also utilize the spent acid solution preparation 2 of clay alteration
#Clay composite flocculant:
(1) clay is purified and is: former clay pit and water are pressed solid-to-liquid ratio (0.1-2): (1-20) soak (1-48h), add the trisodium phosphate that is equivalent to clay raw ore weight (0.5-2%) again, dispersed with stirring (1-3h), staticly settle (1-48h) again, get upper strata suspension, suction filtration, washing, drying get final product to such an extent that purity reaches 99% clay, i.e. SiO
250-53%, Al
2O
33.5-5%, Fe
2O
32-3%, FeO 0.1-0.4%, CaO 4-6%, MgO 18-25%.
(2) clay alteration is:
1. the clay after will purifying grinds and sieves, add hydrochloric acid and carry out sour modification, acid modification after-filtration, the further washing and filtering oven dry of modified clay after solid substance acid after filtering changed, regulate pH value to 4～4.5 with sulfuric acid again, make it become hydroxy metal solion modified clay, again it is carried out 90 ℃ of constant temperature slaking polymerizations after, further oven dry, roasting, grind, sieve, make 1
#Clay composite flocculant;
2. the washing and filtering liquid formation hybrid filtering liquid to the filtered liquid after filtering and 1. is made into poly-silicate solution again, and further the constant temperature slaking makes 2
#Clay composite flocculant.
2. the preparation method of a kind of clay composite flocculant according to claim 1, its feature part is: in clay alteration, when temperature of reaction be 60 ℃, reaction times be 10h, when concentration of hydrochloric acid is 15%, the solubility rate of the magnesium in the clay is 38.9%, at this moment, the specific surface area maximum of modified clay;
3. the preparation method of a kind of clay composite flocculant according to claim 1, its feature part is: the spent acid solution with clay alteration is a feedstock production 2
#The top condition of clay composite flocculant is: choosing activation pH value is 4.5, the active silicic acid of soak time 40min and the spent acid solution of clay alteration, and 1: 1 by volume, under 40 ℃ of constant temperature, slaking reaction 4.5h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007103008984A CN101215031A (en) | 2007-12-28 | 2007-12-28 | Method for preparing clay composite flocculant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007103008984A CN101215031A (en) | 2007-12-28 | 2007-12-28 | Method for preparing clay composite flocculant |
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| CN101215031A true CN101215031A (en) | 2008-07-09 |
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|---|---|---|---|
| CNA2007103008984A Pending CN101215031A (en) | 2007-12-28 | 2007-12-28 | Method for preparing clay composite flocculant |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318984A (en) * | 2013-07-01 | 2013-09-25 | 中国地质大学（武汉） | Method for treating polymer flooding oil-extraction wastewater by employing organic modified sepiolite |
| CN103771572A (en) * | 2014-02-12 | 2014-05-07 | 重庆大学 | Preparation method of polymerization chlorination zinc iron sulfate flocculating agent |
| CN104148007A (en) * | 2014-07-18 | 2014-11-19 | 大连理工大学 | Preparation method and application of multifunctional material for water treatment |
| CN107162133A (en) * | 2017-05-26 | 2017-09-15 | 贵州美瑞特环保科技有限公司 | A kind of oil gas field sewage functionalization chitin composite flocculant and preparation method thereof |
| CN110316835A (en) * | 2019-07-03 | 2019-10-11 | 合山市春旭环保科技有限责任公司 | A kind of high efficiency composition high polymer coagulant and preparation method thereof |
| CN113231192A (en) * | 2021-06-16 | 2021-08-10 | 江西省矿产资源保障服务中心 | Beneficiation method for silicon dioxide in silicon-planted ore |
-
2007
- 2007-12-28 CN CNA2007103008984A patent/CN101215031A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318984A (en) * | 2013-07-01 | 2013-09-25 | 中国地质大学（武汉） | Method for treating polymer flooding oil-extraction wastewater by employing organic modified sepiolite |
| CN103318984B (en) * | 2013-07-01 | 2014-06-11 | 中国地质大学（武汉） | Method for treating polymer flooding oil-extraction wastewater by employing organic modified sepiolite |
| CN103771572A (en) * | 2014-02-12 | 2014-05-07 | 重庆大学 | Preparation method of polymerization chlorination zinc iron sulfate flocculating agent |
| CN103771572B (en) * | 2014-02-12 | 2015-02-11 | 重庆大学 | Preparation method of polymerization chlorination zinc iron sulfate flocculating agent |
| CN104148007A (en) * | 2014-07-18 | 2014-11-19 | 大连理工大学 | Preparation method and application of multifunctional material for water treatment |
| CN107162133A (en) * | 2017-05-26 | 2017-09-15 | 贵州美瑞特环保科技有限公司 | A kind of oil gas field sewage functionalization chitin composite flocculant and preparation method thereof |
| CN110316835A (en) * | 2019-07-03 | 2019-10-11 | 合山市春旭环保科技有限责任公司 | A kind of high efficiency composition high polymer coagulant and preparation method thereof |
| CN110316835B (en) * | 2019-07-03 | 2022-03-29 | 合山市春旭环保科技有限责任公司 | High-efficiency composite polymeric flocculant and preparation method thereof |
| CN113231192A (en) * | 2021-06-16 | 2021-08-10 | 江西省矿产资源保障服务中心 | Beneficiation method for silicon dioxide in silicon-planted ore |
| CN113231192B (en) * | 2021-06-16 | 2022-05-27 | 江西省矿产资源保障服务中心 | Beneficiation method for silicon dioxide in silicon-planted ore |
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Open date: 20080709 |