CN109354145A - A method of organic waste water modification flocculant is prepared with diatomite - Google Patents

A method of organic waste water modification flocculant is prepared with diatomite Download PDF

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Publication number
CN109354145A
CN109354145A CN201811404528.XA CN201811404528A CN109354145A CN 109354145 A CN109354145 A CN 109354145A CN 201811404528 A CN201811404528 A CN 201811404528A CN 109354145 A CN109354145 A CN 109354145A
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China
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flocculant
diatomite
waste water
added
modified
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CN201811404528.XA
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Chinese (zh)
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冯权莉
张评
唐光明
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5281Installations for water purification using chemical agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F2001/007Processes including a sedimentation step
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/06Controlling or monitoring parameters in water treatment pH
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/08Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention discloses a kind of methods for preparing organic waste water modification flocculant with diatomite, belong to organic wastewater processing technology field.The method of the invention extracts SiO using diatomite as raw material2Metasilicate pentahydrate sodium is synthesized, then prepares polymeric aluminium ferrum silicate, and polymeric aluminium ferrum silicate (PAFCSC) flocculant of preparation is modified to obtain modified flocculant using carboxymethyl starch (CMS).The present invention prepares flocculant with diatomite and meets requirement to comprehensive utilization of natural resources, and, it is all very big in China or even All Around The World to the demand of flocculant at present, aluminium system and iron-based flocculating agent occupy very big market with its good treatment effect and low cost, therefore prepare PAFCS flocculant using diatomite and have very big economic significance and social effect.

Description

A method of organic waste water modification flocculant is prepared with diatomite
Technical field
The present invention relates to a kind of methods for preparing organic waste water modification flocculant with diatomite, belong to organic wastewater processing Technical field.
Background technique
Diatomite is a kind of siliceous rock, it is mainly made of the remains of ancient times diatom, is a kind of biogenic silicon Matter sedimentary rock.Its chemical component is with SiO2Based on, SiO can be used2·nH2O indicate, mineralogical composition be opal and its mutation, and Contain a small amount of Al2O3, Fe2O3, CaO, MgO, K2O, Na2O, P2O5 and organic matter.It is mainly distributed on China, the U.S., Japan, pellet The states such as wheat, France, about 3.2 hundred million tons of China's diatomite reserves, prospective reserves is concentrated mainly on East China and northeast ground up to more than 20 hundred million tons Area, wherein larger, reserves it is more have Linjiang city, proven reserve accounts for first, Asia at present, Zhejiang, Yunnan, Shandong, Sichuan etc. save, though distribution is wide, high-quality soil concentrates merely on Changbai Mountain area, and most of other mineral deposits are 3 ~ 4 grades Soil, due to impurity content height, cannot direct deep processing and utilization,.
Diatomite is a physico-chemical process sewage disposal technology, efficient modification infusorial earth sewage in processing organic sewage technology Inorganic agent is the key that the technology, and the present invention directly prepares high performance polymeric aluminium ferrum silicate flocculant by raw material of diatomite, And processing is modified to it using cheap and easy to get, environmentally protective starch, the processing capacity to organic wastewater is improved, this basis The process flow and process facility of upper cooperation, technology can realize purpose that is efficient, stable and inexpensively handling organic wastewater.
" protection environment, handle three-waste pollution " is the eternal topic in China or even the world.The pollution of waste water is also in China Extremely serious, many restrictions have also been made to the discharge of wastewater of enterprise in national policy, however the cost of water treatment of great number, cause very Multiple enterprises stealthily sewage effluent the phenomenon that, bring huge harm to environment.It is how more efficient, to handle these at low cost useless How water produces the water process reagent of high performance cheap, is an important topic for alleviating contaminated wastewater.
Summary of the invention
The purpose of the present invention is to solve the deficiency that the prior art utilizes diatomite, provides and a kind of prepared with diatomite The method of organic wastewater modified flocculant, specifically includes the following steps:
A method of organic waste water modification flocculant is prepared with diatomite, which is characterized in that specifically includes the following steps:
(1) polymeric aluminium ferrum silicate is prepared with diatomite: SiO is extracted from diatomite2, with the SiO of extraction2Prepare waterglass, water Glass adds aluminum sulfate after being diluted with distilled water and polymeric aluminium ferrum silicate is made in ferric sulfate;
(2) modified carboxymethyl starch (CMS) is added in the ratio of 0.002g/ mL ~ 0.020g/ mL and is prepared with diatomite Polymer aluminium silicate ferrous solution in, then in 0.0005g/mL ~ 0.010g/mL ratio be added initiator potassium persulfate, in magnetic It is sufficiently mixed under power stirring, reacts 1min ~ 30min under microwave condition, by acquired solution water bath method, abundant drying is simultaneously ground It is CMS-PAFCS modified flocculant at dark gray powder shape.
Dioxide-containing silica is 70%-96%, iron oxide content 0.5%-1.5%, oxygen in raw material diatomite of the present invention Change aluminium content is 1%-6%.
The carboxymethyl starch of modification of the present invention the preparation method comprises the following steps: by 6g~12g soluble starch be added 10mL~ In the ethyl alcohol of 20 mL, it is put into and 30 DEG C~40 DEG C is sufficiently stirred and be heated in heated at constant temperature magnetic agitation water-bath, be then added The NaOH solid of 2.5g~3.5g after continuing 40~50min of stirring, sequentially adds 10-15ml dissolved with mono- chlorine of 7.0g~7.5g The aqueous isopropanol of acetic acid and the NaOH solid of 2.5g~3.5g increase temperature to 45 DEG C, sufficiently react 100min~120min Afterwards, it is neutralized to neutrality with acetum, filters and is washed with 80% ethanol solution to no Cl-, by the solid after filtration washing Substance is dry under the conditions of 55 DEG C~65 DEG C, and required modified material carboxymethyl starch can be obtained.
Microwave condition of the present invention is 100W ~ 600W.
The organic wastewater modified flocculant of the method for the invention preparation is for handling organic wastewater: adjusting wastewater pH into Property or alkalinity, according to 0.1g/L~1.6g/L additive amount be added CMS-PAFCS flocculant be sufficiently stirred, flocculation sedimentation 5min~ 60in, supernatant are treated waste water.
Aluminium of the present invention, iron-based flocculating agent are introduced made of hydroxyl in silicic acid acid aluminium, iron molecule race reticular structure Inorganic polymer flocculant by bridge formation, is crosslinked and particle in waste water is promoted to flocculate the effects of adherency, aluminium, iron ion institute It is positively charged and can effectively neutralize the negative particles in water, the Zeta potential of colloid is reduced, micelle stability is destroyed, so that glue Group forms flocculation sedimentation by collision, and the precipitation surface product formed is big, there is stronger adsorption capacity.
Beneficial effects of the present invention:
(1) inorganic-organic hybrid high polymer coagulant has both the advantage of the two simultaneously, has affected by environment small, and wadding body is big, PH wide adaptation range, it is cheap the advantages that.
(2) high temperature being generated by microwave method to activate diatomite, being heated compared to electric furnace, heating efficiency is mentioned Height, and can be energy saving.
(3) modified flocculant is prepared using diatomite, diatomite utilization rate, and prepared flocculant pair can be improved Waste water has preferable treatment effect, preferably realizes the conversion of natural resources.
Specific embodiment
The present invention is described in further details with specific embodiment below, but protection scope of the present invention is not limited to institute State content.
Embodiment 1
A method of organic waste water modification flocculant being prepared with diatomite, specifically includes the following steps:
(1) polymeric aluminium ferrum silicate is prepared with diatomite: SiO is extracted from diatomite2, optimum process condition are as follows: m diatomite: m carbon Sour sodium is 1: 1.1,750 DEG C of maturing temperature, 1.8 h of calcining time, carries out acidleach with the hydrochloric acid of 3.0 mol/L;It is molten When glue-gel bath temperature is 94 DEG C, SiO2Yield be 84% or so;With the SiO of extraction2Prepare waterglass, dry method and wet Method;Waterglass is diluted to SiO with distilled water2Content is 3%, adjusts pH to 6 with 20% sulfuric acid acidification and polymerize instead It answers, adds aluminum sulfate (Al2(SO4) and ferric sulfate (Fe2(SO4) polymeric aluminium ferrum silicate is made, then pH to 2 is adjusted, wherein n (Al): n(Fe): n(Si)=5: 2: 1.
(2) preparation of CMS: the ethyl alcohol of 6g soluble starch and 10mL is added in the beaker of 250mL, is put into constant temperature and is added It is sufficiently stirred in pyromagnetic force stirring water-bath and is heated to 30 DEG C, 2.5gNaOH solid is then added, continued after stirring 40min, The NaOH solid for sequentially adding aqueous isopropanol and 2.5g of the 10ml dissolved with 7.0g chloroacetic acid increases temperature to 55 DEG C, fills After dividing reaction 100min, it is neutralized to neutrality with acetum, filters and is simultaneously washed with 80% ethanol solution to no Cl-, will filter Solid matter after washing is dry under the conditions of 60 DEG C, and required modified material CMS can be obtained.
(3) modified carboxy methyl starch (CMS) is added to the polymerization silicon prepared with diatomite in the ratio of 0.002g/ mL In sour ferro-aluminum solution, the diatomite material feature of polymeric aluminium ferrum silicate is prepared are as follows: dioxide-containing silica range is 70%, iron oxide Content range is 0.5%, and alumina content range is 1%;Initiator potassium persulfate 0.0005g/L is added, under magnetic stirring It is sufficiently mixed, then pours into mixed liquor in the conical flask of 250mL, be grafted 60min under 100W microwave condition, by acquired solution Water bath method is sufficiently dried and is ground into powder in thermostatic drying chamber, as gained CMS-PAFCS modified flocculant.
The CMS-PAFCS modified flocculant that the present embodiment is prepared is for handling organic wastewater, below with Amoxicillin For waste water, process conditions are as follows: under the conditions of influent waste water concentration is 600mg/L or so, adjusting wastewater pH to neutral or alkali Property, CMS-PAFCS flocculant, which is added, according to the additive amount of 0.1g/L is sufficiently stirred, flocculation sedimentation 60min, and supernatant is to handle Waste water afterwards;Wastewater COD removal rate can reach 68% or more.
Embodiment 2
A method of organic waste water modification flocculant being prepared with diatomite, specifically includes the following steps:
(1) polymeric aluminium ferrum silicate is prepared with diatomite: SiO is extracted from diatomite2, with the SiO of extraction2Prepare waterglass, water Glass adds aluminum sulfate after being diluted with distilled water and polymeric aluminium ferrum silicate is made in ferric sulfate, and actual conditions are the same as embodiment 1.
(2) preparation of CMS: the ethyl alcohol of 9g soluble starch and 15mL is added in the beaker of 250mL, is put into constant temperature and is added It is sufficiently stirred in pyromagnetic force stirring water-bath and is heated to 35 DEG C, 3gNaOH solid is then added, continued after stirring 45min, according to The NaOH solid of the secondary aqueous isopropanol that 12.5ml is added dissolved with 7.25g chloroacetic acid and 3g increases temperature to 60 DEG C, sufficiently After reacting 110min, it is neutralized to neutrality with acetum, filters and is washed with 80% ethanol solution to no Cl-, by diafiltration Solid matter after washing is dry under the conditions of 60 DEG C, and required modified material CMS can be obtained.
(3) modified carboxy methyl starch (CMS) is added to the polymerization silicon prepared with diatomite in the ratio of 0.011g/ mL In sour ferro-aluminum solution, the diatomite material feature of polymeric aluminium ferrum silicate is prepared are as follows: dioxide-containing silica range is 88%, iron oxide Content range is 1%, and alumina content range is 3.5%.Initiator potassium persulfate 0.00525g/mL is added, in magnetic agitation Under be sufficiently mixed, then mixed liquor is poured into the conical flask of 250mL, is grafted 30min under 350W microwave condition, gained is molten Liquid water bath method is sufficiently dried and is ground into powder in thermostatic drying chamber, as gained CMS-PAFCS modified flocculant.
The CMS-PAFCS modified flocculant that the present embodiment is prepared is for handling organic wastewater, below with Amoxicillin For waste water, process conditions are as follows: under the conditions of influent waste water concentration is 700mg/L or so, adjusting wastewater pH to neutral or alkali Property, CMS-PAFCS flocculant, which is added, according to the additive amount of 0.85g/L is sufficiently stirred, flocculation sedimentation 33min, and supernatant is to locate Waste water after reason;Wastewater COD removal rate can reach 76% or more, and treated waste strength is 100mg/L hereinafter, reaching National emission standard.
Embodiment 3
A method of organic waste water modification flocculant being prepared with diatomite, specifically includes the following steps:
(1) polymeric aluminium ferrum silicate is prepared with diatomite: SiO is extracted from diatomite2, with the SiO of extraction2Prepare waterglass, water Glass adds aluminum sulfate after being diluted with distilled water and polymeric aluminium ferrum silicate is made in ferric sulfate, and actual conditions are the same as embodiment 1.
(2) preparation of CMS: the ethyl alcohol of 12g soluble starch and 20mL is added in the beaker of 250mL, constant temperature is put into It is sufficiently stirred in heating magnetic agitation water-bath and is heated to 40 DEG C, 3.5gNaOH solid is then added, continue to stir 50min Afterwards, sequentially add 15ml dissolved with 7.5g chloroacetic acid aqueous isopropanol and 3.5g NaOH solid, increase temperature to 65 DEG C, After sufficiently reaction 120min, it is neutralized to neutrality with acetum, filters and is washed with 80% ethanol solution to no Cl-, incited somebody to action Solid matter after filter washing is dry under the conditions of 60 DEG C, and required modified material CMS can be obtained.
(3) modified carboxy methyl starch (CMS) is added to the polymerization silicon prepared with diatomite in the ratio of 0.011g/ mL In sour ferro-aluminum solution, the diatomite material feature of polymeric aluminium ferrum silicate is prepared are as follows: dioxide-containing silica range is 96%, iron oxide Content range is 1.5%, and alumina content range is 6%.Initiator potassium persulfate 0.010g/mL is added, under magnetic stirring It is sufficiently mixed, then pours into mixed liquor in the conical flask of 250mL, be grafted 10min under 600W microwave condition, by acquired solution Water bath method is sufficiently dried and is ground into powder in thermostatic drying chamber, as gained CMS-PAFCS modified flocculant.
The CMS-PAFCS modified flocculant that the present embodiment is prepared is for handling organic wastewater, below with Amoxicillin For waste water, process conditions are as follows: under the conditions of influent waste water concentration is 800mg/L or so, adjusting wastewater pH to neutral or alkali Property, CMS-PAFCS flocculant, which is added, according to the additive amount of 1.6g/L is sufficiently stirred, flocculation sedimentation 10min, and supernatant is to handle Waste water afterwards;Wastewater COD removal rate can reach 87% or more.

Claims (5)

1. a kind of method for preparing organic waste water modification flocculant with diatomite, which is characterized in that specifically includes the following steps:
(1) polymeric aluminium ferrum silicate is prepared with diatomite: SiO is extracted from diatomite2, with the SiO of extraction2Prepare waterglass, water glass Glass adds aluminum sulfate after being diluted with distilled water and polymeric aluminium ferrum silicate is made in ferric sulfate;
(2) modified carboxymethyl starch is added in the ratio of 0.002g/ mL ~ 0.020g/ mL and is gathered with prepared by diatomite It closes in aluminium iron silicate solution, initiator potassium persulfate then is added in the ratio of 0.0005g/mL ~ 0.010g/mL, is stirred in magnetic force It mixes down and is sufficiently mixed, react 1min ~ 30min under microwave condition, by acquired solution water bath method, abundant drying is simultaneously ground into ash Black powder is CMS-PAFCS modified flocculant.
2. the method for preparing organic waste water modification flocculant with diatomite according to claim 1, it is characterised in that: raw silicon Dioxide-containing silica is 70%-96%, iron oxide content 0.5%-1.5%, alumina content 1%-6% in diatomaceous earth.
3. the method for preparing organic waste water modification flocculant with diatomite according to claim 1, it is characterised in that: modified Carboxymethyl starch the preparation method comprises the following steps: by 6g~12g soluble starch be added the mL of 10mL~20 ethyl alcohol in, be put into constant temperature and add It is sufficiently stirred in pyromagnetic force stirring water-bath and is heated to 30 DEG C~40 DEG C, the NaOH solid of 2.5g~3.5g is then added, after After 40~50min of continuous stirring, sequentially add aqueous isopropanol and 2.5g of the 10-15ml dissolved with 7.0g~7.5g chloroacetic acid~ The NaOH solid of 3.5g increases temperature to 45 DEG C, after sufficiently reaction 100min~120min, is neutralized to neutrality with acetum, It filters and is washed with 80% ethanol solution to no Cl-, the solid matter after filtration washing is done under the conditions of 55 DEG C~65 DEG C It is dry, required modified material carboxymethyl starch can be obtained.
4. the method for preparing organic waste water modification flocculant with diatomite according to claim 1, it is characterised in that: micro-strip Part is 100W ~ 600W.
5. the organic wastewater modified flocculant of claim 1 the method preparation is for handling organic wastewater, it is characterised in that: adjust Wastewater pH is saved to neutral or alkalinity, CMS-PAFCS flocculant is added according to the additive amount of 0.1g/L~1.6g/L and is sufficiently stirred, wads a quilt with cotton Retrogradation shallow lake 5min~60in, supernatant are treated waste water.
CN201811404528.XA 2018-11-23 2018-11-23 A method of organic waste water modification flocculant is prepared with diatomite Pending CN109354145A (en)

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CN112047422B (en) * 2020-09-16 2022-04-12 国投信开水环境投资有限公司 Production process of composite phosphorus removal agent for sewage treatment

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Application publication date: 20190219