CN108191019A - Iron chloride-chitosan compounding coagulation agent and preparation method thereof - Google Patents

Iron chloride-chitosan compounding coagulation agent and preparation method thereof Download PDF

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Publication number
CN108191019A
CN108191019A CN201810028534.3A CN201810028534A CN108191019A CN 108191019 A CN108191019 A CN 108191019A CN 201810028534 A CN201810028534 A CN 201810028534A CN 108191019 A CN108191019 A CN 108191019A
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China
Prior art keywords
chitosan
iron chloride
solution
preparation
coagulation agent
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CN201810028534.3A
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Chinese (zh)
Inventor
夏雄
侯青桐
许霞
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Changzhou Hua Yu Environmental Protection & Technology Co Ltd
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Changzhou Hua Yu Environmental Protection & Technology Co Ltd
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Priority to CN201810028534.3A priority Critical patent/CN108191019A/en
Publication of CN108191019A publication Critical patent/CN108191019A/en
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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
    • C02F1/5263Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
    • 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
    • C02F1/56Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/30Nature of the water, waste water, sewage or sludge to be treated from the textile industry

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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 iron chloride chitosan compounding coagulation agents and preparation method thereof.The preparation method of this compounding coagulation agent is:Iron chloride is dissolved in distilled water, is (25~100) according to Fe elements and chitosan mass ratio:1 ratio adds in chitosan, under condition of heating and stirring, adds in initiator, makes FeCl3Solution dissolves each other completely with chitosan, and after reacting 1~2 hour, it is 1.9~2.5 to adjust pH with lye, obtains a kind of crocus, transparent iron chloride chitosan compound coagulant.The present invention has the advantages that simple for process, short preparation period, at low cost, is not susceptible to dispersion phenomenon, and dosage is low during use.The iron chloride chitosan compound coagulant prepared by this method can be used for printing and dyeing, in the During Coagulation Process of textile waste.

Description

Iron chloride-chitosan compounding coagulation agent and preparation method thereof
Technical field
The present invention relates to water process built-up flocculant technical field, especially a kind of iron chloride-chitosan compounding coagulation Agent and preparation method thereof.
Background technology
The principal element for causing color degree of dyeing waste water higher is dyestuff.It is estimated that the annual Textile Dyes production in the whole world It is more than 40 ten thousand tons, is discharged during dyeing and printing process there are about 10%~20% dyestuff as waste water, into rivers and lakes, sea and the surface water In.Dyestuff in waste water can absorb light, reduce water transparency, influence aquatile and microorganism growth, be unfavorable for water body Self-cleaning, while easily cause visual pollution.The water body seriously polluted even influences whether the health of the mankind.
Flocculation is using one of most common critical process in waste water treatment process, and the advantage of flocculence is mainly manifested in base Build that expense is relatively low, technological process is simple and convenient to operate, high treating effect etc..It is used in dyeing wastewater now Inorganic flocculating agent is mainly aluminium salt inorganic flocculating agent and molysite inorganic flocculating agent, mainly includes low-molecular inorganic flocculant such as FeCl3, FeSO4, AlCl3, Al2(SO4)3Deng and inorganic polymer flocculant such as PAC, poly-ferric chloride (PFC), polymerised sulphur Sour iron (PFS) etc..
Chitosan and its derivative is all to have good flocculation, clarification.As the fining agent of beverage, suspension can be made Object flocculates rapidly, natural sedimentation, improves the yield of stoste;Using the adsorptivity of chitosan, have in terms of purification of water quality good Effect.
In built-up flocculant, the coordinative role between various flocculants and the processing effect to pollution factors different in dyeing waste water Fruit determines its high efficiency.Inorganic flocculating agent generally all has stronger absorption charge neutrality ability, but molecular weight is relatively low, to Obtaining big flco then needs to add a large amount of flocculant;And the organic polymer length generally all with big molecular weight and line style point Son amount structure, has the ability built bridge between very strong particle.Therefore iron chloride and chitosan are used in compounding, to take long benefit It is short, 1+1 is played in the treatment of waste water>2 effect can generate the floc sedimentation of bulk in a relatively short period of time, more preferable so as to reach Treatment effect.
Invention content
The technical problem to be solved by the present invention is to:Overcome deficiency in the prior art, it is multiple to provide a kind of iron chloride-chitosan With coagulant and preparation method thereof.
The technical solution adopted by the present invention to solve the technical problems is:A kind of iron chloride-chitosan compounding coagulation agent Preparation method has following steps:
(1), iron chloride solid and distilled water are taken by weight (1.6~1.7):(15~40) it mixes, stirs evenly, formed Yellow transparent solution;
(2), chitosan and distilled water are taken by weight 1:(900~1000) it mixes, stirs evenly, obtaining mass concentration is The chitosan solution of 1.0~1.1g/L;
(3), chitosan solution made from step (2) is added in yellow transparent solution made from step (1), chitosan The weight ratio of solution and yellow transparent solution is 1:The first mixed solution is made in (25~100);It is stirred in the heating of the first mixed solution Initiator is added in during mixing, stirs 1~2h, the second mixed solution is made;Initiator is solid;
(4), add in lye in the second mixed solution made from step (3), adjust the pH of the second mixed solution for 1.9~ 2.5, iron chloride-chitosan compounding coagulation agent is made after curing 2~3h.
Further, mixing speed is 100~500r/min in the step (3), and heating temperature is 75~90 DEG C.
Further, iron chloride solid is Iron(III) chloride hexahydrate in the step (1).
Further, initiator is sodium hydrogensulfite or potassium bisulfite in the step (3), and initiator addition is the 4~the 6 ‰ of one mixed solution quality.
Further, lye is sodium hydroxide solution in the step (4), sodium hydroxide solution molar concentration for 1~ 3mol/L。
A kind of iron chloride-chitosan compounding coagulation agent prepared according to above-mentioned preparation method.
The beneficial effects of the invention are as follows:Preparation process of the present invention is simple, the period is short, at low cost;Iron chloride-shell of preparation gathers Sugared compounding coagulation agent is not susceptible to dispersion phenomenon, and dosage is low during use;Iron chloride and chitosan are used in compounding, different coagulations Agent is learnt from other's strong points to offset one's weaknesses between each other, plays respective effect in the treatment of waste water, can generate the wadding of bulk in a relatively short period of time Group has good except total phosphorus effect and higher COD removal rates.
Specific embodiment
Presently in connection with preferred embodiment, the present invention is further illustrated.
Embodiment 1
A kind of preparation method of iron chloride-chitosan compounding coagulation agent has following steps:
(1), it weighs 1.6g iron chloride solids to be dissolved in 15ml distilled water, stirring is uniformly mixed it, forms crocus Clear solution;
(2), chitosan and distilled water are taken by weight 1:900 mixing, stir evenly, and it is 1.1g/L's to obtain mass concentration Chitosan solution;
(3), chitosan solution made from 35ml steps (2) is taken to be added in yellow transparent solution made from step (1), shell The weight ratio of glycan solution and yellow transparent solution is 1:25, the first mixed solution is made;In the first mixed solution heating stirring 0.3g initiators, mixing speed 200r/min are added in the process, and heating temperature is 75 DEG C, stirs 2h, and it is molten that the second mixing is made Liquid;
(4), 2mol/L lye is added in the second mixed solution made from step (3), adjusts the pH of the second mixed solution It is 2.0, iron chloride-chitosan compounding coagulation agent is made after curing 3h.
Embodiment 2
A kind of preparation method of iron chloride-chitosan compounding coagulation agent has following steps:
(1), it weighs 1.665g iron chloride solids to be dissolved in 30ml distilled water, stirring is uniformly mixed it, is formed orange Color clear solution;
(2), chitosan and distilled water are taken by weight 1:1000 mixing, stir evenly, and obtain mass concentration as 1.0g/L Chitosan solution;
(3), chitosan solution made from 25ml steps (2) is taken to be added in yellow transparent solution made from step (1), shell The weight ratio of glycan solution and yellow transparent solution is 1:50, the first mixed solution is made;In the first mixed solution heating stirring 0.45g initiators, mixing speed 200r/min are added in the process, and heating temperature is 85 DEG C, stirs 1.5h, and the second mixing is made Solution;
(4), 1mol/L lye is added in the second mixed solution made from step (3), adjusts the pH of the second mixed solution It is 2.1, iron chloride-chitosan compounding coagulation agent is made after curing 2.5h.
Embodiment 3
A kind of preparation method of iron chloride-chitosan compounding coagulation agent has following steps:
(1), it weighs 1.665g iron chloride solids to be dissolved in 37ml distilled water, stirring is uniformly mixed it, is formed orange Color clear solution;
(2), chitosan and distilled water are taken by weight 1:1000 mixing, stir evenly, and obtain mass concentration as 1.0g/L Chitosan solution;
(3), chitosan solution made from 13ml steps (2) is taken to be added in yellow transparent solution made from step (1), shell The weight ratio of glycan solution and yellow transparent solution is 1:75, the first mixed solution is made;In the first mixed solution heating stirring 0.3g initiators, mixing speed 200r/min are added in the process, and heating temperature is 80 DEG C, stirs 2h, and it is molten that the second mixing is made Liquid;
(4), 1mol/L lye is added in the second mixed solution made from step (3), adjusts the pH of the second mixed solution It is 2.3, iron chloride-chitosan compounding coagulation agent is made after curing 2h.
Embodiment 4
A kind of preparation method of iron chloride-chitosan compounding coagulation agent has following steps:
(1), it weighs 1.665g iron chloride solids to be dissolved in 40ml distilled water, stirring is uniformly mixed it, is formed orange Color clear solution;
(2), chitosan and distilled water are taken by weight 1:1000 mixing, stir evenly, and obtain mass concentration as 1.0g/L Chitosan solution;
(3), chitosan solution made from 10ml steps (2) is taken to be added in yellow transparent solution made from step (1), shell The weight ratio of glycan solution and yellow transparent solution is 1:100, the first mixed solution is made;In the first mixed solution heating stirring 0.3g initiators, mixing speed 200r/min are added in the process, and heating temperature is 90 DEG C, stirs 1.5h, and the second mixing is made Solution;
(4), 2mol/L lye is added in the second mixed solution made from step (3), adjusts the pH of the second mixed solution It is 2.5, iron chloride-chitosan compounding coagulation agent is made after curing 3h.
In order to prove beneficial effects of the present invention, iron chloride-chitosan compounding coagulation agent prepared by above-described embodiment 1-4 And single coagulant (FeCl3) handled with the textile printing and dyeing wastewater of Mr. Yu textile mills, 5 parts of dyeing waste waters are taken, are given up according to 1L The ratio of 4ml flocculants is added in water, by the compounding coagulation agent of the present invention or single coagulant (FeCl3) put into waste water, First quick stirring 1min, then 10min is mixed slowly under the rotating speed of 100r/min, static 20min under the rotating speed of 300r/min. Observe flco size, sinking speed and heavy mud amount during standing, Aspirate supernatant measures total tp removal rate, COD is gone after the completion of standing Except rate and percent of decolourization, test result is as shown in table 1.The assay method of wherein total tp removal rate uses National Standard Method, COD removal rates Assay method uses titration, and percent of decolourization is the measure that decolorizing effect is carried out using reactive blue stimulated dye wastewater.
Table 1 adds the effect of different compounding coagulation agent processing water
As can be seen from Table 1, during the iron chloride that prepared by the present invention-chitosan compounding coagulation agent processing textile printing and dyeing wastewater, Its total tp removal rate, which can reach 85%, COD removal rates, can reach more than 81%, percent of decolourization can reach 90% with On, dyeing waste water complies fully with after processing《Integrated wastewater discharge standard》Discharge standard in GB8978-2002.The present invention simultaneously During the iron chloride of preparation-chitosan compounding coagulation agent processing textile printing and dyeing wastewater, every process performance is superior to single coagulation Agent (FeCl3) process performance.
In addition, in order to prove beneficial effects of the present invention, the iron chloride-chitosan prepared using above-described embodiment 1-4 is multiple The waste water from dyestuff formed with coagulant for active red dye (M-3E) configuration carries out coagulating treatment, and the absorbance for measuring raw water is 11.6%.1L waste water is placed in every group of experiment in 5 1L test glasses respectively, by the coagulated agent prepared under different ratio respectively etc. Amount is added in five test glasses, and mixing time divides three phases, and a stage rotating speed is 300r/min, time 1min, second order It is 60r/min that section rotating speed, which is the stage rotating speed of 100r/min, time 10min, three, and time 20min takes supernatant after staticly settling Liquid carries out analysis measure, and the results are shown in Table 2.
Table 2. adds different compounding coagulation agents, the effect of various dose processing water
As can be seen from Table 2, when the dosage of flocculant be 4mL/L when, flocculating effect is best, percent of decolourization 80% with On, and built-up flocculant is better than single flocculant (FeCl3)。
In conclusion preparation process of the present invention is simple, the period is short, at low cost;The iron chloride of preparation-chitosan compounding coagulation Agent is not susceptible to dispersion phenomenon, and dosage is low during use;Iron chloride and chitosan are used in compounding, different coagulants are mutual Learn from other's strong points to offset one's weaknesses, play respective effect in the treatment of waste water, the floc sedimentation of bulk can be generated in a relatively short period of time, have good Remove total phosphorus effect and higher COD removal rates.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar can understand present disclosure and be implemented, and it is not intended to limit the scope of the present invention, all according to the present invention The equivalent change or modification that Spirit Essence is made should all cover within the scope of the present invention.

Claims (6)

1. a kind of preparation method of iron chloride-chitosan compounding coagulation agent, it is characterised in that:With following steps:
(1), iron chloride solid and distilled water are taken by weight (1.6~1.7):(15~40) it mixes, stirs evenly, form yellow Clear solution;
(2), chitosan and distilled water are taken by weight 1:(900~1000) it mixes, stirs evenly, it is 1.0 to obtain mass concentration The chitosan solution of~1.1g/L;
(3), chitosan solution made from step (2) is added in yellow transparent solution made from step (1), chitosan solution Weight ratio with yellow transparent solution is 1:The first mixed solution is made in (25~100);In the first mixed solution heating stirring mistake Initiator is added in journey, stirs 1~2h, the second mixed solution is made;
(4), lye is added in the second mixed solution made from step (3), the pH for adjusting the second mixed solution is 1.9~2.5, Iron chloride-chitosan compounding coagulation agent is made after curing 2~3h.
2. the preparation method of iron chloride according to claim 1-chitosan compounding coagulation agent, it is characterised in that:The step Suddenly mixing speed is 100~500r/min in (3), and heating temperature is 75~90 DEG C.
3. the preparation method of iron chloride according to claim 1-chitosan compounding coagulation agent, it is characterised in that:The step Suddenly iron chloride solid is Iron(III) chloride hexahydrate in (1).
4. the preparation method of iron chloride according to claim 1-chitosan compounding coagulation agent, it is characterised in that:The step Suddenly initiator is sodium hydrogensulfite or potassium bisulfite in (3), and initiator addition is 4~the 6 ‰ of the first mixed solution quality.
5. the preparation method of iron chloride according to claim 1-chitosan compounding coagulation agent, it is characterised in that:The step Suddenly lye is sodium hydroxide solution in (4), and sodium hydroxide solution molar concentration is 1~3mol/L.
6. a kind of iron chloride-chitosan compounding coagulation agent prepared according to claim 1-5 any one of them method.
CN201810028534.3A 2018-01-12 2018-01-12 Iron chloride-chitosan compounding coagulation agent and preparation method thereof Pending CN108191019A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1654497A (en) * 2005-01-14 2005-08-17 华南理工大学 Chitosan graft ternary polymerization polymeric flocculant and its preparation method and use
CN105712450A (en) * 2016-03-08 2016-06-29 佛山市聚成生化技术研发有限公司 Preparation method of chitosan composite flocculant and chitosan composite flocculant prepared through same
CN106006890A (en) * 2016-06-24 2016-10-12 佛山科学技术学院 Preparation method of chitosan coagulant
CN107175083A (en) * 2017-06-07 2017-09-19 成都信息工程大学 A kind of FeCl3Chitosan polymer and preparation method and application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1654497A (en) * 2005-01-14 2005-08-17 华南理工大学 Chitosan graft ternary polymerization polymeric flocculant and its preparation method and use
CN105712450A (en) * 2016-03-08 2016-06-29 佛山市聚成生化技术研发有限公司 Preparation method of chitosan composite flocculant and chitosan composite flocculant prepared through same
CN106006890A (en) * 2016-06-24 2016-10-12 佛山科学技术学院 Preparation method of chitosan coagulant
CN107175083A (en) * 2017-06-07 2017-09-19 成都信息工程大学 A kind of FeCl3Chitosan polymer and preparation method and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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Application publication date: 20180622

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