CN109437377A - A kind of preparation method of sewage treatment flocculating agent - Google Patents
A kind of preparation method of sewage treatment flocculating agent Download PDFInfo
- Publication number
- CN109437377A CN109437377A CN201811485505.6A CN201811485505A CN109437377A CN 109437377 A CN109437377 A CN 109437377A CN 201811485505 A CN201811485505 A CN 201811485505A CN 109437377 A CN109437377 A CN 109437377A
- Authority
- CN
- China
- Prior art keywords
- salt
- preparation
- flocculating agent
- bromination
- sewage treatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- 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 present invention provides a kind of preparation methods of sewage treatment flocculating agent, are first uniformly mixed bromination diallyl pyrroles salt and bromination diallyl piperidinium salt, obtain mixture, then a certain amount of calcium silicates and diatomite are added into mixture, are uniformly mixed to obtain the final product.Sewage treatment flocculating agent functional group of the invention is more, and the wadding body of generation is big, and flocculated speed is fast, time required for treatment process is short, and treatment effect is preferable, and dosage is few, sludge yield is smaller, and the removal rate for reaching 90%, COD to the turbidity removal rate of sanitary sewage reaches 80%.
Description
Technical field
The invention belongs to sewage purification fields, and in particular to a kind of preparation method of sewage treatment flocculating agent.
Background technique
With the development of surge and the modern industrial or agricultural of population, water consumption is sharply increased in recent years, especially industrial hair
Exhibition, needs a large amount of industrial water, the industrial wastewater then generated is also growing day by day, to accelerate the pollution of water, therefore such as
What cheap effectively processing sewage has become a top priority.
Flocculent precipitation refers to is added a certain amount of flocculant in waste water, so that it is carried out physical-chemical reaction, to reach
It is a kind of not only economic but also easy water treatment method generally used both at home and abroad at present to the purpose of water body purification.Flocculation is heavy
The core and key of shallow lake method are the selections of flocculant, and the property of flocculant directly affects the quality of flocculating effect.With water pollution
Increase, simple inorganic salts flocculant has been unable to meet the needs of present water process, the appearance of high polymer coagulant and from
Single type moves towards compound, and water process efficiency is made to be greatly improved.
The research of organic polymer coargulator is mainly natural polymer at present, and studying more is starch, shell
Glycan and the outer high-molecular compound of extracellular microbial, however China still locates the development of organic polymer coargulator, production and application
In the development phase, still belong to weak link.Technological gap is larger, is mainly shown as: seriation level is low, and specific breed is few, quotient
The product of product only has polyacrylamide and polyacrylic acid two major classes；Low output, not formed economic scale are certain external industrial
The kind of change is still unqualified in China so far；It lags behind in production, total quality level is not high.Therefore flocculation efficiently, economic is found
Agent is always the technical problem of the area research.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of flocculants efficiently, economic, and sanitary sewage can be effectively reduced
Turbidity and COD.
The preparation method of sewage treatment flocculating agent of the invention, comprising the following steps:
(1) by bromination diallyl pyrroles salt and bromination diallyl piperidinium salt by weight (1-3): (1-2) is mixed
It closes uniformly, obtains mixture；
(2) by mixture with calcium silicates, diatomite according to weight ratio 10:(4-5): (3-7) is uniformly mixed to get dirt
Water treatment flocculant.
Preferably, the sewage treatment flocculating agent further includes 2- amino -3- picoline, wherein mixture and 2- amino -
The weight ratio of 3- picoline is 10:(0.08-0.15), preferably 10:0.1.
Preferably, the weight ratio of the bromination diallyl pyrroles salt and bromination diallyl piperidinium salt is 1:1.
Preferably, the weight ratio of mixture and calcium silicates, diatomite is 10:4.5:5.
Preferably, the calcium silicates is synthesis porous calcium silicate.
Wherein, bromination diallyl pyrroles's salt preparation the following steps are included:
(1) in molar ratio (2-4): (1-3) takes diallylamine, Isosorbide-5-Nitrae-dibromobutane, by volume (5-8): (1-3) takes
K2CO3Solution and aqueous slkali；
(2) by diallylamine and K2CO3Solution is added in reaction vessel, is heated to 60-70 DEG C, hands over into reaction vessel
For Isosorbide-5-Nitrae-dibromobutane and aqueous slkali is added dropwise, the reaction was continued after being added dropwise to complete 3-6h；
(3) after the reaction was completed, by solution left standstill liquid separation in reaction vessel, water phase and oily phase are obtained；
(4) water phase is concentrated, dehydrated alcohol is added later and is dissolved, filters；
(5) filtrate is subjected to secondary concentration, acetone is added and is crystallized, filters, filtered crystal is used into acetone again
Washing is dried in vacuo to get bromination diallyl pyrroles's salt.
The preparation of the bromination diallyl piperidinium salt the following steps are included:
(1) in molar ratio (2-4): (1-3) takes diallylamine, 1, and pentamethylene bromide, by volume (5-8): (1-3) takes
K2CO3Solution and aqueous slkali；
(2) by diallylamine and K2CO3Solution is added in reaction vessel, is heated to 60-70 DEG C, hands over into reaction vessel
For being added dropwise 1, pentamethylene bromide and aqueous slkali, the reaction was continued after being added dropwise to complete 3-6h；
(3) after the reaction was completed, by solution left standstill liquid separation in reaction vessel, water phase and oily phase are obtained；
(4) water phase is concentrated, dehydrated alcohol is added later and is dissolved, filters；
(5) filtrate is subjected to secondary concentration, acetone is added and is crystallized, filters, filtered crystal is used into acetone again
Washing is dried in vacuo to get bromination diallyl piperidinium salt.
Preferably, the diallylamine, Isosorbide-5-Nitrae-dibromobutane molar ratio are 3:2.
Preferably, the diallylamine, 1, the molar ratio of pentamethylene bromide are 3:2.
The reaction vessel of step (2) is reaction kettle, and by 1 when dropwise addition, pentamethylene bromide and aqueous slkali are respectively placed in constant pressure drop
In liquid funnel.
Wherein, the K2CO3The mass fraction of solution is 40%.
The aqueous slkali is NaOH solution, concentration 1mol/L.
Preferably, the K2CO3The volume ratio of solution and aqueous slkali is 7:2.
Preferably, the heating temperature of reaction kettle is 65 DEG C.
The dropwise addition alt time of Isosorbide-5-Nitrae-dibromobutane or 1 in step (2), pentamethylene bromide and aqueous slkali is 30-90s, excellent
It is selected as 60s.
The time that liquid separation is stood in step (3) is 15min.
Carrying out crystallization with acetone in step (5) is to carry out under cryogenic, and temperature is 10-20 DEG C, preferably 15 DEG C.
Vacuum drying condition is to be dried in vacuo 8h at 60 DEG C in step (5).
The present invention it has been investigated that, using bromination diallyl piperidinium salt, the inorganic flocculating agent diatomite of arranging in pairs or groups conventional
With synthesis porous calcium silicate, the flocculating effect of obtained composite flocculant is better than the effect of inorganic flocculating agent, lives in processing
Turbidity removal rate and COD removal rate are higher when sewage, can satisfy the processing requirement in terms of sanitary sewage.Further research hair
It is existing, bromination diallyl pyrroles's salt is added, can be further improved the turbidity removal rate and COD removal rate of sanitary sewage,
It can be extended to field of industrial waste water treatment, possible reason is bromination diallyl pyrroles salt and bromination diallyl
The positive charge density of piperidinium salt is high, functional group is more, has by the positive charge group contained by it to the negative electrical charge in sewage
Machine colloid electrical property neutralization and the excellent bridge formation of macromolecule agglomerate function, and colloidal solid is promoted to be gathered into floccule, outstanding from it
It is separated in supernatant liquid.
But since the relative molecular mass of bromination diallyl pyrroles salt and bromination diallyl piperidinium salt is lower,
Therefore suspended matter can only be made to form small and fine and close floc sedimentation when its flocculation, coagulation effect is poor.In order to improve its flocculating effect, this
Field technical staff is usually to share its organic polymer coargulator further with high relative molecular mass, opposite using height
Cation group in the organic polymer coargulator molecular structure of molecular mass is adsorbed in the outstanding of bear electricity by electrostatic interaction
Floating object particle etc. makes suspended particulate cohesion, flocculating setting, so as to improve flocculating effect.Therefore in general, addition will not be passed through
The substance of low molecular weight enhances its flocculating effect.
2- amino -3- the picoline of small-molecular-weight is added in the present invention in component, cooperates bromination diallyl pyrroles
Salt, bromination diallyl piperidinium salt and diatomite and synthesis porous calcium silicate, the effect of obtained flocculant is more preferable, right
The removal rate that the turbidity removal rate of sanitary sewage reaches 90%, COD reaches 80%.Inventor is the study found that this thing happens
Possible reason is that 2- amino -3- picoline can form certain small field in sewage, make when handling sewage
Suspended matter and water in sewage form preliminary separation, add bromination diallyl pyrroles salt, bromination diallyl piperidines
After salt and diatomite and synthesis porous calcium silicate, using the strong adsorptivity of synthesis porous calcium silicate, and pass through diatomite conduct
Flocculation aid, bromination diallyl pyrroles salt, bromination diallyl piperidinium salt Cationic functional groups flocculation when the wadding that generates
Body is bigger, and flocculation rate is fast, can quickly separate from suspension, the time required for treatment process is short, treatment effect
Good, dosage is few, and sludge yield is smaller.
Beneficial effects of the present invention:
1. the present invention uses two kinds of monomers of bromination diallyl pyrroles salt and bromination diallyl piperidinium salt, silicon of arranging in pairs or groups
Diatomaceous earth and synthesis porous calcium silicate, obtained sewage treatment flocculating agent reach 90%, COD's to the turbidity removal rate of sanitary sewage
Removal rate reaches 80%, and after adding the 2- amino -3- picoline of small molecule, treatment effect is more preferable.
2. preparing for sewage treatment flocculating agent of the invention is simple and convenient, safety and environmental protection not will cause secondary pollution.
3. calcium silicates of the invention is using synthesis porous silicic acid calcium material, absorption property is 10-15 times of active carbon, tool
Have that bulk density is small, matter is soft and light, high-specific surface area, low wearing valve, weak negative electrical charge intensity and higher oil suction water imbibition, and
Has the function of ion storing.
4. flocculant functional group of the invention is more, the wadding body of generation is big, and flocculated speed is fast, required for treatment process
Time is short, and treatment effect is preferable, and dosage is few, and sludge yield is smaller.
Specific embodiment
Embodiment 1
The K that 0.15mol diallylamine and 70mL mass fraction are 40% is added in a kettle2CO3Solution, then distinguish
The NaOH solution that Isosorbide-5-Nitrae-dibromobutane of 0.1mol and 20mL concentration are 1mol/L is added in two constant pressure funnels, is pressed
The time interval alternate dropwise addition 1,4- dibromobutane and NaOH solution of 60s.It is kept for 65 DEG C of reaction temperature, after adding material, continued
React 4h.Reaction solution is transferred in separatory funnel, after standing 15min, liquid separation.Isolated water phase is subjected to concentrated by rotary evaporation, to
After water in solution is spin-dried for, dehydrated alcohol dissolution, filtering is added, until inorganic salts are white, by filtered inorganic salt crystal
It is recycled, filtrate carries out concentrated by rotary evaporation again, and dehydrated alcohol is substantially spin-dried for.Then third is added into the solution after revolving
Ketone crystallizes under the conditions of 15 DEG C.After standing 8h, filtering, by filtered crystal acetone washing, until crystal be it is colourless, in 60
It is dried in vacuo 8h under the conditions of DEG C, obtains the monomer of bromination diallyl pyrroles's salt.
The K that 0.15mol diallylamine and 70mL mass fraction are 40% is added in a kettle2CO3Solution, then distinguish
By the 1 of 0.1mol, pentamethylene bromide and 20mL concentration are added in two constant pressure funnels for the NaOH solution of 1mol/L, are pressed
The time interval alternate dropwise addition pentamethylene bromide and NaOH solution of 60s.It is kept for 65 DEG C of reaction temperature, after adding material, continued
React 4h.Subsequent processing obtains bromination diallyl piperidines with the preparation method of the monomer of bromination diallyl pyrroles's salt
The monomer of salt.
10g bromination diallyl pyrroles salt and 10g bromination diallyl piperidinium salt is taken to be mixed to get mixture, Xiang Qi
Middle addition 4.5g synthesizes porous calcium silicate, 5g diatomite, is uniformly mixed to get sewage treatment flocculating agent.
Its turbidity removal rate and COD removal rate to sanitary sewage is measured, the results are shown in Table 1.
Embodiment 2
The K that 0.15mol diallylamine and 70mL mass fraction are 40% is added in a kettle2CO3Solution, then distinguish
The NaOH solution that Isosorbide-5-Nitrae-dibromobutane of 0.1mol and 20mL concentration are 1mol/L is added in two constant pressure funnels, is pressed
The time interval alternate dropwise addition 1,4- dibromobutane and NaOH solution of 30s.It is kept for 60 DEG C of reaction temperature, after adding material, continued
React 4h.Reaction solution is transferred in separatory funnel, after standing 15min, liquid separation.Isolated water phase is subjected to concentrated by rotary evaporation, to
After water in solution is spin-dried for, dehydrated alcohol dissolution, filtering is added, until inorganic salts are white, by filtered inorganic salt crystal
It is recycled, filtrate carries out concentrated by rotary evaporation again, and dehydrated alcohol is substantially spin-dried for.Then third is added into the solution after revolving
Ketone crystallizes under the conditions of 10 DEG C.After standing 6h, filtering, by filtered crystal acetone washing, until crystal be it is colourless, in 60
It is dried in vacuo 8h under the conditions of DEG C, obtains the monomer of bromination diallyl pyrroles's salt.
The K that 0.15mol diallylamine and 70mL mass fraction are 40% is added in a kettle2CO3Solution, then distinguish
By the 1 of 0.08mol, pentamethylene bromide and 14mL concentration are added in two constant pressure funnels for the NaOH solution of 1mol/L,
By the time interval alternate dropwise addition pentamethylene bromide and NaOH solution of 30s.Kept for 60 DEG C of reaction temperature, after adding material, after
Continuous reaction 4h.Subsequent processing obtains bromination diallyl piperidines with the preparation method of the monomer of bromination diallyl pyrroles's salt
The monomer of salt.
The ratio that bromination diallyl pyrroles salt and bromination diallyl piperidinium salt are 3:2 by weight is mixed
Conjunction obtains mixture, is added each component of following parts by weight thereto: 40% synthesis porous calcium silicate, 30% diatomite and
0.8% 2- amino -3- picoline is uniformly mixed to get sewage treatment flocculating agent.
Its turbidity removal rate and COD removal rate to sanitary sewage is measured, the results are shown in Table 1.
Embodiment 3
The K that 0.15mol diallylamine and 70mL mass fraction are 40% is added in a kettle2CO3Solution, then distinguish
The NaOH solution that Isosorbide-5-Nitrae-dibromobutane of 0.15mol and 30mL concentration are 1mol/L is added in two constant pressure funnels,
By the time interval alternate dropwise addition 1,4- dibromobutane and NaOH solution of 90s.Kept for 70 DEG C of reaction temperature, after adding material, after
Continuous reaction 4h.Reaction solution is transferred in separatory funnel, after standing 15min, liquid separation.Isolated water phase is subjected to concentrated by rotary evaporation,
After the water in solution is spin-dried for, dehydrated alcohol dissolution, filtering is added, until inorganic salts are white, filtered inorganic salts are brilliant
Body is recycled, and filtrate carries out concentrated by rotary evaporation again, and dehydrated alcohol is substantially spin-dried for.Then third is added into the solution after revolving
Ketone crystallizes under the conditions of 20 DEG C.After standing 10h, filtering, by filtered crystal acetone washing, until crystal be it is colourless, in 60
It is dried in vacuo 8h under the conditions of DEG C, obtains the monomer of bromination diallyl pyrroles's salt.
The K that 0.15mol diallylamine and 70mL mass fraction are 40% is added in a kettle2CO3Solution, then distinguish
By the 1 of 0.1mol, pentamethylene bromide and 20mL concentration are added in two constant pressure funnels for the NaOH solution of 1mol/L, are pressed
The time interval alternate dropwise addition pentamethylene bromide and NaOH solution of 90s.It is kept for 70 DEG C of reaction temperature, after adding material, continued
React 4h.Subsequent processing obtains bromination diallyl piperidines with the preparation method of the monomer of bromination diallyl pyrroles's salt
The monomer of salt.
The ratio that bromination diallyl pyrroles salt and bromination diallyl piperidinium salt are 2:1 by weight is mixed
Conjunction obtains mixture, is added each component of following parts by weight thereto: 50% synthesis porous calcium silicate, 70% diatomite and
1.5% 2- amino -3- picoline is uniformly mixed to get sewage treatment flocculating agent.
Its turbidity removal rate and COD removal rate to sanitary sewage is measured, the results are shown in Table 1.
Embodiment 4
The preparation of bromination diallyl pyrroles salt and bromination diallyl piperidinium salt is the same as embodiment 1.
10g bromination diallyl pyrroles salt and 10g bromination diallyl piperidinium salt is taken to be mixed to get mixture, Xiang Qi
Middle addition 4.5g synthesis porous calcium silicate, 5g diatomite and 0.1g 2- amino -3- picoline, are uniformly mixed to get sewage
Manage flocculant.
Its turbidity removal rate and COD removal rate to sanitary sewage is measured, the results are shown in Table 1.
Comparative example 1
The preparation of bromination diallyl piperidinium salt is the same as embodiment 1.
Take 4.5g synthesis porous calcium silicate, 5g diatomite be uniformly mixed, be added in sanitary sewage to be processed, then to its
Middle addition 20g bromination diallyl piperidinium salt measures its turbidity removal rate and COD removal rate to sanitary sewage, as a result sees
Table 1.
Comparative example 2
The preparation of bromination diallyl piperidinium salt and bromination diallyl pyrroles's salt is the same as embodiment 1.
It takes 4.5g synthesis porous calcium silicate, 5g diatomite to be uniformly mixed, is added in sanitary sewage to be processed, then to dirt
10g bromination diallyl piperidinium salt is added in water, adds 10g bromination diallyl pyrroles's salt later, measures it to life
The turbidity removal rate and COD removal rate of sewage, the results are shown in Table 1.
1 clean effect table of table
| Turbidity removal rate | COD removal rate | |
| Embodiment 1 | 94% | 86% |
| Embodiment 2 | 92% | 83% |
| Embodiment 3 | 91% | 80% |
| Embodiment 4 | 96% | 88% |
| Comparative example 1 | 72% | 67% |
| Comparative example 2 | 79% | 73% |
By comparing embodiment 1-3 it is found that embodiment 1 is most preferred embodiment, therefore its experiment condition is optimum condition.
By the comparison of embodiment 1 and comparative example 1 it is found that be added into sanitary sewage bromination diallyl piperidinium salt and
Bromination diallyl pyrroles two kinds of salt of salt, than a kind of bromination diallyl piperidinium salt is only added, to the place of sanitary sewage
It is more preferable to manage effect, this is because positive charge density is higher, functional group increases after bromination diallyl pyrroles's salt is added, leads to
Cross positive charge group contained by it in sewage negative electrical charge organic colloid electrical property neutralization and macromolecule it is excellent bridge formation it is solidifying
Poly- function, promotes colloidal solid to be gathered into floccule, separates from its suspension, therefore has better treatment effect.
By comparing embodiment 1 and comparative example 2 it is found that by means of the present invention first by bromination diallyl piperidinium salt
It is uniformly mixed with bromination diallyl pyrroles's salt, then after mixing with calcium silicates and diatomite, obtained flocculant is to life
The treatment effect of sewage living is more preferable, this is because first after evenly mixing by each component, interacting between each component, is formed steady
Fixed complex system after adding it in sanitary sewage, cooperates between each component, can play one's part to the full, thus
So that treatment effect is more preferable.
By comparing embodiment 1 and embodiment 4 it is found that the 2- amino -3- picoline of small molecule is added in embodiment 4
Afterwards, cooperate bromination diallyl pyrroles salt, bromination diallyl piperidinium salt and diatomite and synthesis porous calcium silicate,
The effect of obtained flocculant is more preferable, and possible reason is that 2- amino -3- picoline, can be in sewage when handling sewage
It is middle to form certain small field, so that suspended matter and water in sewage is formed preliminary separation, adds bromination diallyl pyrroles
After salt, bromination diallyl piperidinium salt and diatomite and synthesis porous calcium silicate, the strong of synthesis porous calcium silicate is utilized
Adsorptivity, and flocculation aid is used as by diatomite, bromination diallyl pyrroles salt, bromination diallyl piperidinium salt it is positive from
The wadding body that sub- functional group generates when flocculating is bigger, and flocculation rate is fast, can quickly separate from suspension, therefore handles effect
Fruit is more preferable.
Claims (9)
1. a kind of preparation method of sewage treatment flocculating agent, which comprises the following steps:
(1) by bromination diallyl pyrroles salt and bromination diallyl piperidinium salt by weight (1-3): (1-2) mixes equal
It is even, obtain mixture；
(2) by mixture with calcium silicates, diatomite according to weight ratio 10:(4-5): (3-7) is uniformly mixed to get at sewage
Manage flocculant.
2. the preparation method of sewage treatment flocculating agent as described in claim 1, which is characterized in that further include 2- amino -3- first
Yl pyridines, wherein the weight ratio of mixture and 2- amino -3- picoline is 10:(0.08-0.15).
3. the preparation method of sewage treatment flocculating agent as claimed in claim 1 or 2, which is characterized in that two allyl of bromination
The weight ratio of base pyrroles salt and bromination diallyl piperidinium salt is 1:1.
4. the preparation method of sewage treatment flocculating agent as claimed in claim 1 or 2, which is characterized in that mixture and calcium silicates,
The weight ratio of diatomite is 10:4.5:5.
5. the preparation method of sewage treatment flocculating agent as claimed in claim 2, which is characterized in that mixture and 2- amino -3-
The weight ratio of picoline is 10:0.1.
6. the preparation method of sewage treatment flocculating agent as claimed in claim 1 or 2, which is characterized in that two allyl of bromination
The preparation of base pyrroles's salt the following steps are included:
(1) in molar ratio (2-4): (1-3) takes diallylamine, Isosorbide-5-Nitrae-dibromobutane, by volume (5-8): (1-3) takes K2CO3
Solution and aqueous slkali；
(2) by diallylamine and K2CO3Solution is added in reaction vessel, is heated to 60-70 DEG C, alternately drips into reaction vessel
Add Isosorbide-5-Nitrae-dibromobutane and aqueous slkali, the reaction was continued 3-6h after being added dropwise to complete；
(3) after the reaction was completed, by solution left standstill liquid separation in reaction vessel, water phase and oily phase are obtained；
(4) water phase is concentrated, dehydrated alcohol is added later and is dissolved, filters；
(5) filtrate is subjected to secondary concentration, acetone is added and is crystallized, filters, filtered crystal is used into acetone washing again,
Vacuum drying is to get bromination diallyl pyrroles's salt.
7. the preparation method of sewage treatment flocculating agent as claimed in claim 1 or 2, which is characterized in that two allyl of bromination
The preparation of phenylpiperidines salt the following steps are included:
(1) in molar ratio (2-4): (1-3) takes diallylamine, 1, and pentamethylene bromide, by volume (5-8): (1-3) takes K2CO3
Solution and aqueous slkali；
(2) by diallylamine and K2CO3Solution is added in reaction vessel, is heated to 60-70 DEG C, alternately drips into reaction vessel
Add 1, pentamethylene bromide and aqueous slkali, the reaction was continued after being added dropwise to complete 3-6h；
(3) after the reaction was completed, by solution left standstill liquid separation in reaction vessel, water phase and oily phase are obtained；
(4) water phase is concentrated, dehydrated alcohol is added later and is dissolved, filters；
(5) filtrate is subjected to secondary concentration, acetone is added and is crystallized, filters, filtered crystal is used into acetone washing again,
Vacuum drying is to get bromination diallyl piperidinium salt.
8. the preparation method of sewage treatment flocculating agent as claimed in claim 2, which is characterized in that Isosorbide-5-Nitrae-dibromo in step (2)
Butane and the dropwise addition alt time of NaOH solution are 30-90s.
9. the preparation method of sewage treatment flocculating agent as claimed in claim 3, which is characterized in that 1,5- dibromo in step (2)
Pentane and the dropwise addition alt time of NaOH solution are 30-90s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811485505.6A CN109437377B (en) | 2018-12-05 | 2018-12-05 | Preparation method of sewage treatment flocculant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811485505.6A CN109437377B (en) | 2018-12-05 | 2018-12-05 | Preparation method of sewage treatment flocculant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109437377A true CN109437377A (en) | 2019-03-08 |
| CN109437377B CN109437377B (en) | 2021-05-11 |
Family
ID=65557797
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811485505.6A Active CN109437377B (en) | 2018-12-05 | 2018-12-05 | Preparation method of sewage treatment flocculant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109437377B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716597A (en) * | 2022-05-18 | 2022-07-08 | 河北科技大学 | Solid ionic organic porous polymer and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758821A (en) * | 2017-11-28 | 2018-03-06 | 申国庆 | A kind of coagulant for sanitary sewage disposal and preparation method thereof |
| CN107840395A (en) * | 2017-12-12 | 2018-03-27 | 成都育芽科技有限公司 | A kind of magnetic polyacrylamide is modified sewage-treating agent and preparation method thereof |
| CN108083614A (en) * | 2018-02-05 | 2018-05-29 | 中国科学院长春应用化学研究所 | A kind of water-dispersion type composite diatomite flocculation dewatering agent and its application |
| CN108435148A (en) * | 2018-06-21 | 2018-08-24 | 黄益良 | A kind of cyclo-dextrin-modified polyacrylamide sewage water inorganic agent and preparation method thereof |
| CN108503005A (en) * | 2018-04-08 | 2018-09-07 | 南宁市夏阳化工科技有限责任公司 | A kind of sanitary sewage flocculant and preparation method thereof |
-
2018
- 2018-12-05 CN CN201811485505.6A patent/CN109437377B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758821A (en) * | 2017-11-28 | 2018-03-06 | 申国庆 | A kind of coagulant for sanitary sewage disposal and preparation method thereof |
| CN107840395A (en) * | 2017-12-12 | 2018-03-27 | 成都育芽科技有限公司 | A kind of magnetic polyacrylamide is modified sewage-treating agent and preparation method thereof |
| CN108083614A (en) * | 2018-02-05 | 2018-05-29 | 中国科学院长春应用化学研究所 | A kind of water-dispersion type composite diatomite flocculation dewatering agent and its application |
| CN108503005A (en) * | 2018-04-08 | 2018-09-07 | 南宁市夏阳化工科技有限责任公司 | A kind of sanitary sewage flocculant and preparation method thereof |
| CN108435148A (en) * | 2018-06-21 | 2018-08-24 | 黄益良 | A kind of cyclo-dextrin-modified polyacrylamide sewage water inorganic agent and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716597A (en) * | 2022-05-18 | 2022-07-08 | 河北科技大学 | Solid ionic organic porous polymer and preparation method and application thereof |
| CN114716597B (en) * | 2022-05-18 | 2023-04-11 | 河北科技大学 | Solid ionic organic porous polymer and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109437377B (en) | 2021-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105540943A (en) | Silicon-containing wastewater treatment method, silicon-containing wastewater utilization system, molecular sieve preparation method and molecular sieve preparation system | |
| CN109734145A (en) | A kind for the treatment of of dyeing wastewater composite flocculation agent | |
| CN103253751B (en) | Inorganic-organic multi-element composite flocculant, and preparation method and application thereof | |
| CN106745591A (en) | A kind of preparation method of heavy metal ion adsorbed type composite flocculation agent and products thereof | |
| CN105565459B (en) | A kind of poly-ferric chloride-paper mill sludge base aminated polymer composite flocculation agent and preparation method thereof | |
| CN104925929A (en) | Composite flocculant for treating printing and dyeing wastewater | |
| CN109437377A (en) | A kind of preparation method of sewage treatment flocculating agent | |
| CN100500256C (en) | Preparation method of flocculation water purifier for drinking water, industrial water and dyeing-finishing sewage treatment | |
| CN104974454B (en) | A kind of flocculant and preparation method thereof | |
| CN109231387A (en) | A kind of compound material for water treatment of stalk/aluminium polychloride and preparation method thereof | |
| CN107899548A (en) | A kind of preparation method of Efficient antibacterial absorption water purification agent | |
| CN107324466A (en) | Method is prepared in situ in a kind of river course water treatment coagulant | |
| CN106477695B (en) | Composite flocculant, preparation method thereof and oilfield sewage treatment method | |
| CN108423782A (en) | A kind of preparation method of plant fiber water process sedimentation agent | |
| CN105967484A (en) | Sludge deep dehydration method for processing flue gas desulfurization wastewater sludge | |
| RU2482074C1 (en) | Method of treating waste water from arsenic | |
| CN105906006B (en) | A kind of preparation method of living drainage inorganic agent | |
| CN100376489C (en) | Flocculant for seawater and preparation method | |
| RU2288181C1 (en) | Method of preparing water-soluble reagent to clean natural and waste waters and to separate phases | |
| CN109867342A (en) | A kind of processing method for sewage of digging up mine | |
| CN108219064A (en) | A kind of method that aqueous dispersion polymerization prepares cationic polyacrylamide | |
| CN104356268A (en) | Preparation method for magnesium ion-containing modified polyacrylamide | |
| CN112978974B (en) | Papermaking sewage treatment agent and preparation method and application thereof | |
| CN110975799B (en) | Preparation method of diatomite sludge filter material for efficient adsorption and dephosphorization | |
| CN107892373A (en) | A kind of physical chemistry composite flocculation agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |