CN108585147A - A kind of preparation method of composite flocculant - Google Patents
A kind of preparation method of composite flocculant Download PDFInfo
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- CN108585147A CN108585147A CN201810423119.8A CN201810423119A CN108585147A CN 108585147 A CN108585147 A CN 108585147A CN 201810423119 A CN201810423119 A CN 201810423119A CN 108585147 A CN108585147 A CN 108585147A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/545—Silicon compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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Abstract
The present invention relates to flocculant technical fields, and in particular to a kind of preparation method of composite flocculant includes the following steps：To bentonite calcining, activation process, intercalation processing is then carried out, intercalation modifying bentonite is obtained；Aluminium-magnesium silicate, silane coupling agent, the progress of N hydroxylethyl acid amides is compound, obtain modified magnesium aluminium silicate；Modified magnesium aluminium silicate is compound with silicon tetrachloride, obtain compound system A；Intercalation modifying bentonite is added into compound system A, granulation obtains composite flocculation agent.The composite flocculant of the present invention is good with flocculation turbidity removal effect, is making full use of residual silicon tetrachloride liquor hydrolysis same simultaneously, the flocculating effect of flocculant is improved, while also achieving the utilization again of pollutant, has greatly saved cost, safety and environmental protection improves sewage treating efficiency.
Description
Technical field
The present invention relates to flocculant technical fields, and in particular to a kind of preparation method of composite flocculant.
Background technology
In recent years, economic rapid development, industrial development is swift and violent, and pollution of waterhead is on the rise；And water is the base of human survival
This demand.The safety guarantee work of drinking water causes national great attention already.On July 1st, 2007, what country newly revised《It is raw
Sanitary standard for drinking water living》(GB 5749-2006) is formally implemented, and finishes former standard (the GB 5749- for continuing 21 years as long as
1985).New standard set quota is significantly increased by original 35 to 106, and the limit value of part index number is also more stringent.This
Outside, on June 25th, 2008, country again issued 11 including pulping and paper-making, plating, fermentation etc. including newly it is more stringent
Discharge standard.This has important practical significance for ensureing the drinking-water health of the people, promoting people's living standard.Wherein wad a quilt with cotton
Solidifying is the first step of water process and the most key one of process, and the selection of flocculant directly determines flocculating effect
The key and key foundation of quality and flocculence water technology.Aluminium silicate polymer is a kind of New Inorganic High Polymer Coagulant.
The one kind of polymer aluminium silicate as New Inorganic High Polymer Coagulant is in polysilicon acid and traditional aluminium salt, molysite
The combination product of the polysilicon acid and metal salt that grow up on the basis of equal flocculants, it has the advantages of aluminium, ferric flocculant,
Weaken mutual weakness, there is the water purification performance more excellent than individual aluminum salt flocculant, polymeric silicicacid aluminium flocculating agent to prepare former
Material derives from a wealth of sources, produce can a large amount of, easy to operate, Environmental Safety, the pollution of environment is even more greatly reduced.And aluminium silicate polymer
It prepares usually with sodium silicate solution and a certain concentration hydrochloric acid or sulfuric acid, polysilicon acid solution is made.In above-mentioned obtained polysilicon acid solution
It is middle that a certain amount of Al is added3+Solution or aluminium salt, can be obtained polyaluminum silicate chloride coagulant.Patent No. 200910300930.8《Altogether
The new synthetic method of polysilicate flocculant》In the middle and later periods of the polyaluminium object flocculant synthesized with traditional method or to
Some polyaluminium thing liquid body flocculants are added high chlorosilane and are modified to obtain a kind of more preferably poly- silicon salt flocculant of turbidity removal effect, but
Its method does not make full use of wherein hydrolyzing chlorosilane to generate the property of a large amount of hydrochloric acid, therefore chlorosilane dosage relative quantity is less.
Invention content
It is of the existing technology the purpose of the invention is to overcome the problems, such as, a kind of preparation side of composite flocculant is provided
Method, this method is simple, and safety is suitble to large-scale industrial production.
To achieve the goals above, the present invention provides a kind of preparation method of composite flocculant, includes the following steps：
(1) alta-mud modification is handled：After bentonite is calcined, acid activation processing is carried out, modified alta-mud is obtained；It will change
Property bentonite, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and initiator are uniformly mixed in ethanol, then 80~
2~5 are heated to reflux at 100 DEG C, obtains intercalation modifying bentonite；
(2) aluminium-magnesium silicate, silane coupling agent are added into N- ethoxys in 120~130 DEG C of 15~30min of insulated and stirred
Acrylic amine continues cooled to room temperature after 2~5h of stirring, and the deionized water of 2~3 times of amounts is added, and is aged 5 at room temperature
~8h, obtains modified magnesium aluminium silicate；
(3) water stirring is added in modified magnesium aluminium silicate and suspension is made, then addition silicon tetrachloride waste liquid, stirring 30~
After 50min, 4~6h is reacted at 85~105 DEG C, obtains compound system A；
(4) into compound system A be added intercalation modifying bentonite, then under stirring conditions spray into ethylene glycol two shrink it is sweet
The ethanol solution of oily ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculation agent.
The present invention also provides a kind of composite flocculants, are made of the substance of following parts by weight：100~200 weight of bentonite
Measure part, 3~15 parts by weight of chitosan, 5~15 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, 1~5 parts by weight of initiator,
20~45 parts by weight of aluminium-magnesium silicate, 20~40 parts by weight of silicon tetrachloride waste liquid, 3~8 parts by weight of silane coupling agent, N- ethoxys third
2~10 parts by weight of olefin(e) acid amine, 30~60 parts by weight of ethylene glycol diglycidylether.
Under optimum condition, the composite flocculation agent is made of the substance of following parts by weight：120~180 weight of bentonite
Part, 5~10 parts by weight of chitosan, 8~12 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, 1~5 parts by weight of initiator, silicon
25~40 parts by weight of sour magnalium, 25~35 parts by weight of silicon tetrachloride waste liquid, 3~8 parts by weight of silane coupling agent, N- hydroxylethyls
3~8 parts by weight of acid amide, 40~50 parts by weight of ethylene glycol diglycidylether.It is further preferred that the composite flocculation agent, by
The substance of following parts by weight is made：150 parts by weight of bentonite, 8 parts by weight of chitosan, 2,3- epoxypropyltrimethylchloride chlorides 10
Parts by weight, 3 parts by weight of initiator, 30 parts by weight of aluminium-magnesium silicate, 30 parts by weight of silicon tetrachloride waste liquid, 5 parts by weight of silane coupling agent,
5 parts by weight of N- hydroxylethyls acid amide, 450 parts by weight of ethylene glycol diglycidylether.
The present invention carries out intercalation modifying, Neng Gou using 2,3- epoxypropyltrimethylchloride chlorides and initiator to bentonite
Polymerisation occurs between bentonite bed, significantly improves bentonitic flocculating effect, under optimum condition, the initiator is selected from azo
In two isobutyl dimethyl phthalates, azo-bis-isobutyrate hydrochloride, two isobutyl imidazoline hydrochloride of azo, azo isobutyl cyano formamide
At least one.
By carrying out the composite modified of surface to aluminium-magnesium silicate, it is formed on its surface polymer, generates two-layer compound flocculation
Agent improves flocculating effect of the flocculant to suspended matter in sewage；Then it is further reacted with silicon tetrachloride waste liquid again, utilizes four
The a large amount of hydrochloric acid and silicic acid that the hydrolysis of silicon chloride raffinate generates, in a small amount of polyaluminium silicic acid of two-layer compound flocculant Surface Creation
Aluminium obtains composite modified aluminium-magnesium silicate, further improves the flocculating effect of flocculant.Under optimum condition, the magnesium silicate
The weight ratio of aluminium and the silicon tetrachloride waste liquid is 1:1.Under optimum condition, the silane coupling agent is selected from aminopropyl-triethoxy
Silane, aminopropyl trimethoxysilane, 2- aminoethyl amino propyl trimethoxy silanes, divinyl triammonium base propyl trimethoxy silicon
Alkane, aminoethylaminopropyl methyl dimethoxysilane, aminoethylaminopropyl triethoxysilane, urea propyl-triethoxysilicane and
At least one of urea propyl trimethoxy silicane.
The bentonite of intercalation modifying is compound with composite modified aluminium-magnesium silicate and be granulated, obtained composite flocculation agent is to dirt
Suspended matter in water has excellent flocculating effect, and compared with general inorganic flocculant and organic polymer coargulator,
Preferable flocculating effect can be shown when low dosage；Also, used composite flocculation agent after rinsing can be by the outstanding of cohesion
Float removes, then secondary to come into operation.
Under optimum condition, the content of aluminium oxide is more than 30% in the aluminium-magnesium silicate.
In order to improve bentonitic flocculating effect, the present invention carries out calcination processing to bentonite, under optimum condition, in step
(1) in, the bentonitic calcination temperature is 300~450 DEG C, and calcination time is 2~5h.Then it is carried out at acid activation
Reason, improve bentonitic activity, what the acid solution can be well known to those skilled in the art, for example, hydrochloric acid, nitric acid,
One kind in sulfuric acid, specifically, as selected concentration in the hydrochloric acid solution of 1~2.5mol/L.
Under optimum condition, the weight ratio of the bentonite and the aluminium-magnesium silicate is (3~5):1.
Through the above technical solutions, the composite flocculant of the present invention has, flocculation turbidity removal effect is good, is making full use of four
The hydrolysis of silicon chloride raffinate improves the flocculating effect of flocculant, while also achieving the utilization again of pollutant, significantly with simultaneously
Saved cost, safety and environmental protection improves sewage treating efficiency.
The grain size of the composite flocculant of the present invention can select in a wider scope, and use scope is wide, application prospect
Greatly.
Specific implementation mode
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.Below will by embodiment to the present invention into
Row detailed description.
Embodiment 1
A kind of composite flocculant is made of the substance of following parts by weight：150 parts by weight of bentonite, 8 weight of chitosan
Part, 10 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, 3 parts by weight of azo-bis-iso-dimethyl, 30 weight of aluminium-magnesium silicate
Part (content of aluminium oxide is 35.6%), 30 parts by weight of silicon tetrachloride waste liquid (55.27wt%), aminopropyl triethoxysilane 5
Parts by weight, 5 parts by weight of N- hydroxylethyls acid amide, 450 parts by weight of ethylene glycol diglycidylether.
The preparation method of the composite flocculant, includes the following steps：
(1) alta-mud modification is handled：Bentonite is calcined into 3h at 350 DEG C, is then added in hydrochloric acid solution and is ultrasonically treated
Then 25min is 6.3 with ion water washing to pH, obtains modified alta-mud；
By modified alta-mud, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and azo-bis-iso-dimethyl in second
It is uniformly mixed in alcohol, is then heated to reflux 3h at 90 DEG C, obtains intercalation modifying bentonite；
(2) aluminium-magnesium silicate, aminopropyl triethoxysilane are added into N- hydroxyl second in 125 DEG C of 15~30min of insulated and stirred
Base acrylic amine continues cooled to room temperature after stirring 3h, the deionized waters of 3 times of amounts is added, and is aged 6h at room temperature, obtains
To modified magnesium aluminium silicate；
(3) water stirring is added in modified magnesium aluminium silicate and suspension is made, silicon tetrachloride waste liquid and silicon tetrachloride is then added
The water of 10 times of amounts of waste liquid reacts 5h at 100 DEG C, obtains compound system A after stirring 40min；
(4) into compound system A be added intercalation modifying bentonite, then under stirring conditions spray into ethylene glycol two shrink it is sweet
The ethanol solution of oily ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculant.
Embodiment 2
A kind of composite flocculant is made of the substance of following parts by weight：180 parts by weight of bentonite, 10 weight of chitosan
Part, 8 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, 5 parts by weight of azo isobutyl cyano formamide, 25 parts by weight of aluminium-magnesium silicate
(content of aluminium oxide is 35.6%), 35 parts by weight of silicon tetrachloride waste liquid (55.27wt%), 3 weight of aminopropyl triethoxysilane
Measure part, 3 parts by weight of N- hydroxylethyls acid amide, 50 parts by weight of ethylene glycol diglycidylether.
The preparation method of the composite flocculant, includes the following steps：
(1) alta-mud modification is handled：Bentonite is calcined into 2h at 400 DEG C, is then added in hydrochloric acid solution and is ultrasonically treated
Then 20min is 6.2 with ion water washing to pH, obtains modified alta-mud；
By modified alta-mud, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and azo isobutyl cyano formamide in second
It is uniformly mixed in alcohol, is then heated to reflux 4h at 85 DEG C, obtains intercalation modifying bentonite；
(2) aluminium-magnesium silicate, aminopropyl triethoxysilane are added into N- ethoxys third in 130 DEG C of insulated and stirred 15min
Olefin(e) acid amine continues cooled to room temperature after stirring 5h, the deionized waters of 2 times of amounts is added, and is aged 6h at room temperature, is changed
Property aluminium-magnesium silicate；
(3) water stirring is added in modified magnesium aluminium silicate and suspension is made, silicon tetrachloride waste liquid and silicon tetrachloride is then added
The water of 10 times of amounts of waste liquid reacts 6h at 90 DEG C, obtains compound system A after stirring 40min；
(4) into compound system A be added intercalation modifying bentonite, then under stirring conditions spray into ethylene glycol two shrink it is sweet
The ethanol solution of oily ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculant.
Embodiment 3
A kind of composite flocculant is made of the substance of following parts by weight：120 parts by weight of bentonite, 5 weight of chitosan
Part, 12 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, two isobutyl imidazoline hydrochloric acid sodium of nitrogen, 1 parts by weight, 40 weight of aluminium-magnesium silicate
Measure part (content of aluminium oxide is 35.6%), 25 parts by weight of useless (55.27wt%) liquid of silicon tetrachloride, aminoethylaminopropyl methyl two
8 parts by weight of methoxy silane, 8 parts by weight of N- hydroxylethyls acid amide, 40 parts by weight of ethylene glycol diglycidylether.
The preparation method of the composite flocculant, includes the following steps：
(1) alta-mud modification is handled：Bentonite is calcined into 3h at 350 DEG C, is then added in hydrochloric acid solution and is ultrasonically treated
Then 30min is 6.5 with ion water washing to pH, obtains modified alta-mud；
Modified alta-mud, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and two isobutyl imidazoline hydrochloric acid sodium of nitrogen are existed
It is uniformly mixed in ethyl alcohol, is then heated to reflux 4h at 100 DEG C, obtains intercalation modifying bentonite；
(2) aluminium-magnesium silicate, aminoethylaminopropyl methyl dimethoxysilane are added in 130 DEG C of insulated and stirred 15min
N- hydroxylethyl acid amides continue cooled to room temperature after stirring 3h, the deionized waters of 2 times of amounts are added, and old at room temperature
Change 5h, obtains modified magnesium aluminium silicate；
(3) water stirring is added in modified magnesium aluminium silicate and suspension is made, silicon tetrachloride waste liquid and silicon tetrachloride is then added
The water of 10 times of amounts of waste liquid reacts 4h at 95 DEG C, obtains compound system A after stirring 45min；
(4) into compound system A be added intercalation modifying bentonite, then under stirring conditions spray into ethylene glycol two shrink it is sweet
The ethanol solution of oily ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculant.
Embodiment 4
A kind of composite flocculant is made of the substance of following parts by weight：100 parts by weight of bentonite, 3 weight of chitosan
Part, 15 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, 1 parts by weight of azo-bis-iso-dimethyl, 45 weight of aluminium-magnesium silicate
Part (content of aluminium oxide is 35.6%), 20 parts by weight of silicon tetrachloride waste liquid (55.27wt%), 2- aminoethylaminopropyl trimethoxies
8 parts by weight of base silane, 2 parts by weight of N- hydroxylethyls acid amide, 60 parts by weight of ethylene glycol diglycidylether.
The preparation method of the composite flocculant, includes the following steps：
(1) alta-mud modification is handled：Bentonite is calcined into 2h at 450 DEG C, is then added in hydrochloric acid solution and is ultrasonically treated
Then 15min is 6.5 with ion water washing to pH, obtains modified alta-mud；
By modified alta-mud, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and azo-bis-iso-dimethyl in second
It is uniformly mixed in alcohol, is then heated to reflux 2h at 100 DEG C, obtains intercalation modifying bentonite；
(2) aluminium-magnesium silicate, 2- aminoethyl amino propyl trimethoxy silanes are added into N- in 130 DEG C of insulated and stirred 15min
Hydroxylethyl acid amide continues cooled to room temperature after stirring 5h, the deionized waters of 2 times of amounts is added, and is aged at room temperature
8h obtains modified magnesium aluminium silicate；
(3) water stirring is added in modified magnesium aluminium silicate and suspension is made, silicon tetrachloride waste liquid and silicon tetrachloride is then added
The water of 10 times of amounts of waste liquid reacts 4h at 105 DEG C, obtains compound system A after stirring 50min；
(4) into compound system A be added intercalation modifying bentonite, then under stirring conditions spray into ethylene glycol two shrink it is sweet
The ethanol solution of oily ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculant.
Embodiment 5
A kind of composite flocculant is made of the substance of following parts by weight：200 parts by weight of bentonite, 15 weight of chitosan
Part, 5 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, 5 parts by weight of azo isobutyl cyano formamide, 20 parts by weight of aluminium-magnesium silicate
(content of aluminium oxide is 35.6%), 40 parts by weight of silicon tetrachloride waste liquid (55.27wt%), 2- aminoethylaminopropyl trimethoxies
3 parts by weight of silane, 10 parts by weight of N- hydroxylethyls acid amide, 30 parts by weight of ethylene glycol diglycidylether.
The preparation method of the composite flocculant, includes the following steps：
(1) alta-mud modification is handled：Bentonite is calcined into 5h at 300 DEG C, is then added in hydrochloric acid solution and is ultrasonically treated
Then 30min is 6.5 with ion water washing to pH, obtains modified alta-mud；
By modified alta-mud, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and azo isobutyl cyano formamide in second
It is uniformly mixed in alcohol, is then heated to reflux 5h at 80 DEG C, obtains intercalation modifying bentonite；
(2) aluminium-magnesium silicate, 2- aminoethyl amino propyl trimethoxy silanes are added into N- in 120 DEG C of insulated and stirred 30min
Hydroxylethyl acid amide continues cooled to room temperature after stirring 2h, the deionized waters of 3 times of amounts is added, and is aged at room temperature
5h obtains modified magnesium aluminium silicate；
(3) water stirring is added in modified magnesium aluminium silicate and suspension is made, silicon tetrachloride waste liquid and silicon tetrachloride is then added
The water of 10 times of amounts of waste liquid reacts 6h at 85 DEG C, obtains compound system A after stirring 30min；
(4) into compound system A be added intercalation modifying bentonite, then under stirring conditions spray into ethylene glycol two shrink it is sweet
The ethanol solution of oily ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculant.
Comparative example 1
A kind of composite flocculant is made of the substance of following parts by weight：150 parts by weight of bentonite, 30 weight of aluminium-magnesium silicate
Measure part (content of aluminium oxide is 35.6%), 30 parts by weight of silicon tetrachloride waste liquid (55.27wt%), aminopropyl triethoxysilane
5 parts by weight, 5 parts by weight of N- hydroxylethyls acid amide, 450 parts by weight of ethylene glycol diglycidylether.
The preparation method of the composite flocculant, includes the following steps：
(1) alta-mud modification is handled：Bentonite is calcined into 3h at 350 DEG C, is then added in hydrochloric acid solution and is ultrasonically treated
Then 25min is 6.3 with ion water washing to pH, obtains modified alta-mud；
(2) aluminium-magnesium silicate, aminopropyl triethoxysilane are added into N- hydroxyl second in 125 DEG C of 15~30min of insulated and stirred
Base acrylic amine continues cooled to room temperature after stirring 3h, the deionized waters of 3 times of amounts is added, and is aged 6h at room temperature, obtains
To modified magnesium aluminium silicate；
(3) water stirring is added in modified magnesium aluminium silicate and suspension is made, silicon tetrachloride waste liquid and silicon tetrachloride is then added
The water of 10 times of amounts of waste liquid reacts 5h at 100 DEG C, obtains compound system A after stirring 40min；
(4) into compound system A be added intercalation modifying bentonite, then under stirring conditions spray into ethylene glycol two shrink it is sweet
The ethanol solution of oily ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculant.
Comparative example 2
A kind of composite flocculant is made of the substance of following parts by weight：150 parts by weight of bentonite, 8 weight of chitosan
Part, 10 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, 3 parts by weight of azo-bis-iso-dimethyl, 30 weight of aluminium-magnesium silicate
Part (content of aluminium oxide is 35.6%), 30 parts by weight of silicon tetrachloride waste liquid (55.27wt%), ethylene glycol diglycidylether
450 parts by weight.
The preparation method of the composite flocculant, includes the following steps：
(1) alta-mud modification is handled：Bentonite is calcined into 3h at 350 DEG C, is then added in hydrochloric acid solution and is ultrasonically treated
Then 25min is 6.3 with ion water washing to pH, obtains modified alta-mud；
By modified alta-mud, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and azo-bis-iso-dimethyl in second
It is uniformly mixed in alcohol, is then heated to reflux 3h at 90 DEG C, obtains intercalation modifying bentonite；
(2) water stirring is added in modified magnesium aluminium silicate and suspension is made, silicon tetrachloride waste liquid and silicon tetrachloride is then added
The water of 10 times of amounts of waste liquid reacts 5h at 100 DEG C, obtains compound system A after stirring 40min；
(3) into compound system A be added intercalation modifying bentonite, then under stirring conditions spray into ethylene glycol two shrink it is sweet
The ethanol solution of oily ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculant.
Comparative example 3
A kind of composite flocculant is made of the substance of following parts by weight：150 parts by weight of bentonite, 8 weight of chitosan
Part, 10 parts by weight of 2,3- epoxypropyltrimethylchloride chlorides, 3 parts by weight of azo-bis-iso-dimethyl, 30 weight of aluminium-magnesium silicate
Part (content of aluminium oxide is 35.6%), 5 parts by weight of aminopropyl triethoxysilane, 5 parts by weight of N- hydroxylethyls acid amide, second
450 parts by weight of Hexanediol diglycidyl ether.
The preparation method of the composite flocculant, includes the following steps：
(1) alta-mud modification is handled：Bentonite is calcined into 3h at 350 DEG C, is then added in hydrochloric acid solution and is ultrasonically treated
Then 25min is 6.3 with ion water washing to pH, obtains modified alta-mud；
By modified alta-mud, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and azo-bis-iso-dimethyl in second
It is uniformly mixed in alcohol, is then heated to reflux 3h at 90 DEG C, obtains intercalation modifying bentonite；
(2) aluminium-magnesium silicate, aminopropyl triethoxysilane are added into N- hydroxyl second in 125 DEG C of 15~30min of insulated and stirred
Base acrylic amine continues cooled to room temperature after stirring 3h, the deionized waters of 3 times of amounts is added, and is aged 6h at room temperature, obtains
To modified magnesium aluminium silicate；
(3) by modified magnesium aluminium silicate and intercalation modifying bentonite, then ethylene glycol two is sprayed under stirring conditions and is shunk
The ethanol solution of glycerin ether is granulated after being uniformly mixed through automatic pill-making machine, obtains the composite flocculant.
Experiment test：
The composite flocculant 5kg for taking above-described embodiment 1~5 and comparative example 1~3 to be prepared respectively, with the poly- of equivalent
Aluminium chloride (being purchased from Shandong Tian Jian water process Science and Technology Ltd. white aluminium polychloride product) is closed as a control group, to same batch etc.
Amount sewage is handled, and each embodiment handles 1t sewage, and sewage index is：Suspension content (C0) 358.5mg/L, hardness
(H) it is 296mg/L, 20 ± 5 DEG C of water temperature, record is launched after flocculant 1h and suspension content C in sewage after 3h1、C2, and calculate
Removal efficiency after 3h, experimental result are as shown in table 1.
The assay method of suspended matter is according to GB/T 11901-89 gravimetric deteminations.
Table 1：The flocculating property table of flocculant in the present invention
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In the skill of the present invention
In art conception range, technical scheme of the present invention can be carried out a variety of simple variants, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to
Protection scope of the present invention.
Claims (7)
1. a kind of preparation method of composite flocculant, which is characterized in that include the following steps：
(1) alta-mud modification is handled：After bentonite is calcined, acid activation processing is carried out, modified alta-mud is obtained；It will be modified swollen
Profit soil, 2,3- epoxypropyltrimethylchloride chlorides, chitosan and initiator are uniformly mixed in ethanol, then at 80~100 DEG C
Under be heated to reflux 2~5h, obtain intercalation modifying bentonite；
(2) aluminium-magnesium silicate, silane coupling agent are added into N- hydroxylethyls in 120~130 DEG C of 15~30min of insulated and stirred
Acid amide, continues cooled to room temperature after 2~5h of stirring, is added the deionized waters of 2~3 times of amounts, and at room temperature ageing 5~
8h obtains modified magnesium aluminium silicate；
(3) water stirring is added in modified magnesium aluminium silicate and suspension is made, silicon tetrachloride is then added, after stirring 30~50min,
4~6h is reacted at 85~105 DEG C, obtains compound system A；
(4) intercalation modifying bentonite is added into compound system A, then sprays into ethylene glycol diglycidylether under stirring conditions
Ethanol solution, be granulated through automatic pill-making machine after being uniformly mixed, obtain the composite flocculation agent.
2. the preparation method of composite flocculant according to claim 1, which is characterized in that described swollen in step (1)
The calcination temperature of profit soil is 300~450 DEG C, and calcination time is 2~5h.
3. the preparation method of composite flocculant according to claim 1, which is characterized in that the initiator is selected from azo
In two isobutyl dimethyl phthalates, azo-bis-isobutyrate hydrochloride, two isobutyl imidazoline hydrochloride of azo, azo isobutyl cyano formamide
At least one.
4. the preparation method of composite flocculant according to claim 1, which is characterized in that the silane coupling agent is selected from
Aminopropyl triethoxysilane, aminopropyl trimethoxysilane, 2- aminoethyl amino propyl trimethoxy silanes, divinyl triammonium base
Propyl trimethoxy silicane, aminoethylaminopropyl methyl dimethoxysilane, aminoethylaminopropyl triethoxysilane, urea propyl
At least one of triethoxysilane and urea propyl trimethoxy silicane.
5. the preparation method of composite flocculant according to claim 1, which is characterized in that aoxidized in the aluminium-magnesium silicate
The content of aluminium is more than 30%.
6. the preparation method of composite flocculant according to claim 1, which is characterized in that the aluminium-magnesium silicate with
The weight ratio of the silicon tetrachloride is 1:1.
7. the preparation method of composite flocculant according to claim 1, which is characterized in that the bentonite and the silicon
The weight ratio of sour magnalium is (3~5):1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111646535A (en) * | 2020-07-06 | 2020-09-11 | 宁波首创厨余垃圾处理有限公司 | Attapulgite surface modification method and application of modified attapulgite |
| CN113666529A (en) * | 2021-06-25 | 2021-11-19 | 湖南瀚洋环保科技有限公司 | Chromium pollutant treating agent and using method thereof |
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| CN104891618A (en) * | 2015-06-05 | 2015-09-09 | 杨强 | Novel compound water treatment flocculant as well as preparation method and application thereof |
| CN106430496A (en) * | 2016-12-12 | 2017-02-22 | 乐山师范学院 | Method of preparing poly aluminum chloride flocculant and poly aluminum silicate chloride flocculant simultaneously |
| CN106732425A (en) * | 2016-12-28 | 2017-05-31 | 西北师范大学 | The modified bentonite adsorption material of Quaternary Ammonium Salt of Chitosan and its preparation and the application in Adsorbing Lead Ion in Polluted Water |
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| CN104891618A (en) * | 2015-06-05 | 2015-09-09 | 杨强 | Novel compound water treatment flocculant as well as preparation method and application thereof |
| CN106430496A (en) * | 2016-12-12 | 2017-02-22 | 乐山师范学院 | Method of preparing poly aluminum chloride flocculant and poly aluminum silicate chloride flocculant simultaneously |
| CN106732425A (en) * | 2016-12-28 | 2017-05-31 | 西北师范大学 | The modified bentonite adsorption material of Quaternary Ammonium Salt of Chitosan and its preparation and the application in Adsorbing Lead Ion in Polluted Water |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111646535A (en) * | 2020-07-06 | 2020-09-11 | 宁波首创厨余垃圾处理有限公司 | Attapulgite surface modification method and application of modified attapulgite |
| CN113666529A (en) * | 2021-06-25 | 2021-11-19 | 湖南瀚洋环保科技有限公司 | Chromium pollutant treating agent and using method thereof |
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