CN107629164B - A kind of preparation method of cation type water-soluble polymer polymer - Google Patents
A kind of preparation method of cation type water-soluble polymer polymer Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of cation type water-soluble polymer polymer, include the following steps: (1) synthesizing cationic type water soluble acrylic resin: preparing includes acrylic acid, butyl acrylate, methacrylic acid-beta-hydroxy ethyl ester, the mixed solution of methyl methacrylate and initiator is spare, solvent is fitted into four-necked bottle, heating, the mixed solution of 10-30% is first added into solvent again, remaining mixed solution is added dropwise again, initiator and solvent are added again, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride is finally added dropwise, cation type water-soluble acrylic resin is prepared；(2) synthesizing cationic type water soluble polymer: by volume it is that 80-100:10-30 is mixed by cation type water-soluble acrylic resin and hexamethoxymethyl melamine, cation type water-soluble polymer polymer is prepared.Cation type water-soluble polymer polymer prepared by the present invention has preferable flocculating effect.
Description
Technical field
The invention belongs to the technical field of sewage of environmental improvement, and in particular to a kind of cation type water-soluble polymer
The preparation method of polymer.
Background technique
As the enhancing of people's environmental consciousness and the continuous of law perfect, cation type water-soluble polymer is had become at water
Manage the Main way of medicament development.Wherein Key wordscationic polyacrylate resin is because its molecular weight is big, positive charge, adsorptivity, decoloration
The advantages that property, nonstaining property, is widely used in the fields such as flocculant, decolorising agent, chemical industry, environmental protection.General commercially available acroleic acid polymerization
The solvent of object is toluene, dimethylbenzene etc., and since these solvents are containing toxic, when solvent to be removed can cause certain dirt to environment
Dye.
The research and exploration to deepen continuously simultaneously with people to acrylate, and constantly pushing away in application field
Extensively, water soluble acrylate resin's copolymer just gradually replaces the similar resin of solvent type to become the heat subject studied both at home and abroad.
, it can be achieved that adsorptivity, cohesiveness, bridge formation ability, dissolution after the functional groups such as introducing-OH ,-COOH and-CONH- in strand
The performances such as property, decolourising property are more preferably.
CN104817251A discloses a kind of composite high-molecular sludge dehydrating agent and preparation method thereof, be a kind of combination without
Machine-organic polymer flocculation dewatering agent can wrap disclosed in it in scheme and contain acrylic acid as anionic monomer, methyl-prop
E pioic acid methyl ester as non-ionic monomer, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride as cationic monomer and inorganic salts into
Row is mixed to get composite high-molecular sludge dehydrating agent, and inorganic salts include ferric trichloride, ferric sulfate, bodied ferric sulfate, polyaluminium
One or more of iron, polymeric aluminum sulfate iron, alchlor, aluminum sulfate, polyaluminium sulfate and aluminium polychloride.This is multiple
Close high polymer sludge dehydration agent using inorganic, organic dehydrating agent cooperation can effectively save cost, but inorganic salts flocculation dewatering agent
Relative molecular mass and granularity and flocculation bridge formation ability are still more far short of what is expected than organic polymer coargulator, and exist to further water
Solve the instability problem of reaction.Current cation type water-soluble acrylic resin, which exists, is difficult to realize low cost and overpass
The combination of ability, high flocculability.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation side of cation type water-soluble polymer polymer
Method.
A kind of preparation method of cation type water-soluble polymer polymer of the invention, includes the following steps:
(1) synthesizing cationic type water soluble acrylic resin: preparing includes acrylic acid, butyl acrylate, methacrylic acid-
The mixed solution of beta-hydroxy ethyl ester, methyl methacrylate and initiator is spare, and solvent is fitted into four-necked bottle, and heat up 80-100
DEG C, then the mixed solution of 10-30% is first added into solvent, after keeping the temperature 10-50min, then remaining mixed solution is added dropwise, keeps the temperature
1-3 hours and then addition initiator and solvent, then insulation reaction 1-3 hour, finally dropwise addition methylacryoyloxyethyl front three
Ammonium chloride, and insulation reaction 1-3 hours, cation type water-soluble acrylic resin is prepared；
(2) synthesizing cationic type water soluble polymer: by cation type water-soluble acrylic resin and hexakis-methoxy
Methyl melamine is 80-100:10-30 mixing by volume, and cation type water-soluble polymer polymer is prepared.
Preferably, further include the preparation step of hexamethoxymethyl melamine: formalin is added in flask, adjust
PH value adds melamine, adjusts pH value again to 7.5-9, be warming up to 70-80 DEG C, insulation reaction obtains six to 7.5-9
Then methanol is added in melamine methylol into flask, adjust pH value to the hexamethylol trimerization between 2-3, being added
Cyanamide, heating continue to adjust pH value holding 2-3, terminate within finally insulation reaction 1 hour at 45-55 DEG C, hexakis-methoxy is prepared
Methyl melamine.
Preferably, described to adjust the sodium hydroxide solution or quality percentage that the solution that pH value is selected is mass percent 10%
The HCl solution of number 10%.
Preferably, the molar ratio of the formaldehyde and melamine are as follows: 10:1.
Preferably, the dosage of the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride accounts for acrylic acid, butyl acrylate, methyl
The 10-20% of senecioate-hydroxyl ethyl ester, methyl methacrylate and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride gross mass.
Preferably, the weight of the acrylic acid, butyl acrylate, methacrylic acid-beta-hydroxy ethyl ester and methyl methacrylate
Measure ratio are as follows: 1-10:5-20:1-10:1-10.
Preferably, the time that remaining mixed solution is added dropwise in the step (1) is 2.5-4 hours.
Preferably, in the step (2), cation type water-soluble acrylic resin and hexamethoxymethyl melamine are mixed
It further include auxiliary agent being added and with the water-reducible step of distillation after conjunction；The auxiliary agent include one of ammonium hydroxide and alcamines or
Two kinds.
Preferably, the volume ratio of the cation type water-soluble acrylic resin and hexamethoxymethyl melamine is 100:
10-30。
Preferably, the initiator amount accounts for acrylic acid, butyl acrylate, methacrylic acid-beta-hydroxy ethyl ester, metering system
The 1%-1.5% of sour methyl esters and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride gross mass.
Cation type water-soluble polymer polymer of the invention has very fast and preferable flocculating effect.
Specific embodiment
Technical solution of the present invention is described in further detail combined with specific embodiments below, so that the technology of this field
Personnel can better understand the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
The present embodiment provides a kind of preparation methods of cation type water-soluble polymer polymer, include the following steps:
(1) synthesizing cationic type water soluble acrylic resin: preparing includes acrylic acid, butyl acrylate, methacrylic acid-
The mixed solution of beta-hydroxy ethyl ester, methyl methacrylate and initiator is spare, and solvent is fitted into four-necked bottle, and heat up 80-100
DEG C, then the mixed solution of 10-30% is first added into solvent, after keeping the temperature 10-50min, then remaining mixed solution is added dropwise, keeps the temperature
1-3 hours and then addition initiator and solvent, then insulation reaction 1-3 hour, finally dropwise addition methylacryoyloxyethyl front three
Ammonium chloride, and insulation reaction 1-3 hours, cation type water-soluble acrylic resin is prepared；
(2) synthesizing cationic type water soluble polymer: by cation type water-soluble acrylic resin and hexakis-methoxy
Methyl melamine is 80-100:10-30 mixing by volume, and cation type water-soluble polymer polymer is prepared.
In a preferred embodiment, heating described in step (1) is to be warming up to 90 DEG C, and reaction temperature is 90 DEG C, is conducive to
Increase reaction rate to which the resin of high conversion must be broken, if reaction temperature is lower than 90 DEG C, reaction is slow, the molecular resin of preparation
Amount is high, and viscosity is larger；Weak reaction temperature is higher than 90 DEG C, and viscosity is smaller, and the degree of polymerization reduces.
In a preferred embodiment, further include the preparation step of hexamethoxymethyl melamine: formalin is added to burning
In bottle, adjust pH value to 7.5-9, (during reaction hydroxymethylation early period there is in polycondensation reaction there are polycondensation reaction,
When pH value is less than 7.5, polycondensation easily occurs between the methylol of generation, therefore can only obtain its copolymer；When pH value is greater than 9
When, it is not susceptible to polycondensation, but catalyst concn is high, reaction speed is too fast, and reaction is difficult to carry out completely, and the hexakis-methoxy first generated
Base melamine is easy agglomeration, therefore the pH value of reaction early period should be controlled in 7.5-9), in further preferred embodiments, pH value is answered
The control adds melamine in 8-9, adjusts pH value again to 7.5-9, is warming up to 70-80 DEG C, insulation reaction obtains six
Melamine methylol, is then added methanol into flask, adjusts pH value between 2-3, (during reaction later period etherification reaction
For general control p H value between 2-3, etherificate speed is moderate.When p H value between 1 and 2 when, catalyst concn is higher, reacts
In fierceness, it is too fast to be etherified speed；When p H value is between 4-5, etherificate speed is excessively slow) obtained hexamethylol melamine is added
Amine, heating continue to adjust pH value holding 2-3, terminate within finally insulation reaction 1 hour at 45-55 DEG C, hexakis-methoxy first is prepared
Base melamine.It is described to adjust the hydrogen-oxygen that the solution that pH value is selected is mass percent 10% in further preferred embodiments
Change the HCl solution of sodium solution or mass percent 10%.In further preferred embodiments, the formaldehyde and melamine rub
That ratio are as follows: 10:1, lower content of formaldehyde can preferably guarantee the synthesis of hexamethoxymethyl melamine.
In a preferred embodiment, the dosage of the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride accounts for acrylic acid, acrylic acid
Butyl ester, methacrylic acid-beta-hydroxy ethyl ester, methyl methacrylate and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride gross mass
10-20%.
In a preferred embodiment, the acrylic acid, butyl acrylate, methacrylic acid-beta-hydroxy ethyl ester and methacrylic acid
The weight ratio of methyl esters are as follows: 1-10:5-20:1-10:1-10.
In a preferred embodiment, the time that remaining mixed solution is added dropwise in the step (1) is 2.5-4 hours.
In a preferred embodiment, in the step (2), by cation type water-soluble acrylic resin and hexakis-methoxy methyl three
It further include auxiliary agent being added and with the water-reducible step of distillation after poly cyanamid mixing；The auxiliary agent includes in ammonium hydroxide and alcamines
One or two.
In a preferred embodiment, the volume of the cation type water-soluble acrylic resin and hexamethoxymethyl melamine
Than for 100:10-30.
In a preferred embodiment, the initiator amount account for acrylic acid, butyl acrylate, methacrylic acid-beta-hydroxy ethyl ester,
The 1%-1.5% of methyl methacrylate and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride gross mass, initiator are reasonably used
Amount can make the conversion ratio entirely reacted all reach 90% or more, and the viscosity downward trend of the resin prepared is gentle.
In a preferred embodiment, initiator is benzoyl peroxide；Solvent is n-butanol.
The cation type water-soluble polymer polymer that the present embodiment obtains can be used as flocculant, decolorising agent etc., at waste water
In reason field, the present embodiment is preferably applied in the processing of wastewater from chemical industry, coking wastewater and dyeing waste water.
In order to have further understanding and understanding to technical solution of the present invention, several preferred embodiments pair are now enumerated
It is described in further details.
Embodiment 1
Synthesizing cationic type water soluble acrylic resin: by methyl methacrylate 5.5mL, methacrylic acid-β-hydroxyl second
Ester 3.5mL, acrylic acid 2mL, butyl acrylate 16mL and initiator benzoyl peroxide (BPO) are mixed to get mixed solution.In
In four-necked bottle equipped with blender, thermometer, the low liquid funnel of constant pressure and condenser pipe, 20ml butanol solution is added, opens stirring,
Water bath with thermostatic control is warming up to 90 DEG C, and 20% mixed solution is first added dropwise, and after keeping the temperature 30min, then the mixing of residue 80% is at the uniform velocity added dropwise
Solution is added dropwise to complete for 2.5-4 hours, is kept the temperature 2 hours and then is added a certain amount of benzoyl peroxide (BPO) and the positive fourth of 5ml
Alcohol, the dosage of BPO account for the 1.25% of monomer gross mass.It is last insulation reaction 2 hours, rear that methylacryoyloxyethyl front three is added dropwise
Ammonium chloride, dosage account for the 18% of monomer gross mass, and insulation reaction 2 hours, and reaction terminates.
Synthetic cross-linking agent-hexamethoxymethyl melamine: (water-bath) heater, blender and temperature are loaded on three-necked flask
Degree meter, excessive formalin is added in flask, adjusts pH value to 8-9 with the NaOH solution that mass percent is 10%, then
The molar ratio of addition 63g melamine, formaldehyde and melamine is 10:1, stirs 30min, adjusts p H value, heating again
70-80 DEG C, to there is the precipitation of white crystalline solid substance, stops stirring, cooling after continuing heating standing reaction 1 hour, separates waste water
And free formaldehyde, obtain hexamethylolmelamine.Then, excessive methanol is added into flask, stirs, with 10% HCl tune
PH value is saved to hexamethylolmelamine between 2-3, is added, 45 DEG C is warming up under stirring condition, to sufficiently dissolve, adjusts pH
Value, terminates for insulation reaction 1 hour at 45-55 DEG C.
Cation type water-soluble polymer polymer: by cation type water-soluble acrylic resin and hexakis-methoxy methyl trimerization
Cyanamide is uniformly mixed by volume for 100:20, and required viscosity is diluted to distilled water.It is water-soluble that cationic is prepared
Property high molecular polymer.
Embodiment 2
Synthesizing cationic type water soluble acrylic resin: by methyl methacrylate 5.5mL, methacrylic acid-β-hydroxyl second
Ester 4.5mL, acrylic acid 5mL, butyl acrylate 12mL and initiator benzoyl peroxide (BPO) are mixed to get mixed solution.In
In four-necked bottle equipped with blender, thermometer, the low liquid funnel of constant pressure and condenser pipe, 45ml butanol solution is added, opens stirring,
Water bath with thermostatic control is warming up to 90 DEG C, and 10% mixed solution is first added dropwise, and after keeping the temperature 30min, then the mixing of residue 90% is at the uniform velocity added dropwise
Solution is added dropwise to complete for 3 hours, is kept the temperature 2 hours and then is added a certain amount of benzoyl peroxide (BPO) and 14ml n-butanol,
The dosage of BPO accounts for the 1.25% of monomer gross mass.It is last insulation reaction 2 hours, rear that methylacryoyloxyethyl trimethyl is added dropwise
Ammonium chloride, dosage account for the 15% of monomer gross mass, and insulation reaction 2 hours, and reaction terminates.
Synthetic cross-linking agent-hexamethoxymethyl melamine: (water-bath) heater, blender and temperature are loaded on three-necked flask
Degree meter, excessive formalin is added in flask, adjusts pH value to 8-9 with the NaOH solution that mass percent is 10%, then
The molar ratio of addition 63g melamine, formaldehyde and melamine is 10:1, stirs 30min, adjusts p H value, heating again
70-80 DEG C, to there is the precipitation of white crystalline solid substance, stops stirring, cooling after continuing heating standing reaction 1 hour, separates waste water
And free formaldehyde, obtain hexamethylolmelamine.Then, excessive methanol is added into flask, stirs, with 10% HCl tune
PH value is saved to hexamethylolmelamine between 2-3, is added, 45 DEG C is warming up under stirring condition, to sufficiently dissolve, adjusts pH
Value, terminates for insulation reaction 1 hour at 45-55 DEG C.
Cation type water-soluble polymer polymer: by cation type water-soluble acrylic resin and hexakis-methoxy methyl trimerization
Cyanamide is uniformly mixed by volume for 100:18, and required viscosity is diluted to distilled water.
Embodiment 3
Synthesizing cationic type water soluble acrylic resin: by methyl methacrylate 6mL, methacrylic acid-beta-hydroxy ethyl ester
5.5mL, acrylic acid 2mL, butyl acrylate 8mL and initiator benzoyl peroxide (BPO) are mixed to get mixed solution.It is filling
In the four-necked bottle for having the low liquid funnel of blender, thermometer, constant pressure and condenser pipe, 40ml butanol solution is added, opens stirring, it is permanent
Tepidarium is warming up to 90 DEG C, and 25% mixed solution is first added dropwise, and after keeping the temperature 30min, then the mixing of at the uniform velocity dropwise addition residue 75% is molten
Liquid is added dropwise to complete for 2.5 hours, is kept the temperature 2 hours and then is added a certain amount of benzoyl peroxide (BPO) and 20ml n-butanol,
The dosage of BPO accounts for the 1.25% of monomer gross mass.It is last insulation reaction 2 hours, rear that methylacryoyloxyethyl trimethyl is added dropwise
Ammonium chloride, dosage account for the 10% of monomer gross mass, and insulation reaction 2 hours, and reaction terminates.
Synthetic cross-linking agent-hexamethoxymethyl melamine: (water-bath) heater, blender and temperature are loaded on three-necked flask
Degree meter, excessive formalin is added in flask, adjusts pH value to 8-9 with the NaOH solution that mass percent is 10%, then
The molar ratio of addition 63g melamine, formaldehyde and melamine is 10:1, stirs 30min, adjusts p H value, heating again
70-80 DEG C, to there is the precipitation of white crystalline solid substance, stops stirring, cooling after continuing heating standing reaction 1 hour, separates waste water
And free formaldehyde, obtain hexamethylolmelamine.Then, excessive methanol is added into flask, stirs, with 10% HCl tune
PH value is saved to hexamethylolmelamine between 2-3, is added, 45 DEG C is warming up under stirring condition, to sufficiently dissolve, adjusts pH
Value, terminates for insulation reaction 1 hour at 45-55 DEG C.
Cation type water-soluble polymer polymer: by cation type water-soluble acrylic resin and hexakis-methoxy methyl trimerization
Cyanamide is uniformly mixed by volume for 100:28, and required viscosity is diluted to distilled water.It is water-soluble that cationic is prepared
Property high molecular polymer.
Embodiment 4
Synthesizing cationic type water soluble acrylic resin: by methyl methacrylate 6mL, methacrylic acid-beta-hydroxy ethyl ester
5.5mL, acrylic acid 7mL, butyl acrylate 14mL and initiator benzoyl peroxide (BPO) are mixed to get mixed solution.It is filling
In the four-necked bottle for having the low liquid funnel of blender, thermometer, constant pressure and condenser pipe, 35ml butanol solution is added, opens stirring, it is permanent
Tepidarium is warming up to 90 DEG C, and 15% mixed solution is first added dropwise, and after keeping the temperature 30min, then the mixing of at the uniform velocity dropwise addition residue 85% is molten
Liquid is added dropwise to complete for 2.5 hours, is kept the temperature 2 hours and then is added a certain amount of benzoyl peroxide (BPO) and 10ml n-butanol,
The dosage of BPO accounts for the 1.25% of monomer gross mass.It is last insulation reaction 2 hours, rear that methylacryoyloxyethyl trimethyl is added dropwise
Ammonium chloride, dosage account for the 12% of monomer gross mass, and insulation reaction 2 hours, and reaction terminates.
Synthetic cross-linking agent-hexamethoxymethyl melamine: (water-bath) heater, blender and temperature are loaded on three-necked flask
Degree meter, excessive formalin is added in flask, adjusts pH value to 8-9 with the NaOH solution that mass percent is 10%, then
The molar ratio of addition 63g melamine, formaldehyde and melamine is 10:1, stirs 30min, adjusts p H value, heating again
70-80 DEG C, to there is the precipitation of white crystalline solid substance, stops stirring, cooling after continuing heating standing reaction 1 hour, separates waste water
And free formaldehyde, obtain hexamethylolmelamine.Then, excessive methanol is added into flask, stirs, with 10% HCl tune
PH value is saved to hexamethylolmelamine between 2-3, is added, 45 DEG C is warming up under stirring condition, to sufficiently dissolve, adjusts pH
Value, terminates for insulation reaction 1 hour at 45-55 DEG C.
Cation type water-soluble polymer polymer: by cation type water-soluble acrylic resin and hexakis-methoxy methyl trimerization
Cyanamide is uniformly mixed by volume for 100:25, and required viscosity is diluted to distilled water.It is water-soluble that cationic is prepared
Property high molecular polymer.
Comparative example 1
Compared with Example 2, in comparative example 1, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride dosage accounts for monomer gross mass
20%, remaining compositing formula ratio and preparation method condition are same as Example 2.
Comparative example 2
Compared with Example 2, in comparative example 2, cation type water-soluble acrylic resin and hexamethoxymethyl melamine
It is by volume 100:35, remaining compositing formula ratio and preparation method condition are same as Example 2.
Effect example
1. chemical wastewater treatment: taking the waste water in certain chemical plant: 1000ppm embodiment 1-4 and comparative example 1-2 preparation is added
Cation type water-soluble polymer polymer is as Coagulation and Adsorption agent, and COD (mg/L) and suspended matter before and after test processes
(mg/L).Concrete outcome is shown in Table 1.
Table 1
2. being used for treatment of dyeing wastewater: taking 6 parts of 500mL dye house effluents (pH=7.4~7.9 of dyeing waste water, turbidity
1112~1340mg/l of 120~140NTU, COD) it is respectively placed in the beaker of 800ml, then use hydrochloric acid and sodium hydroxide solution
The pH of dyeing waste water is adjusted, then adds embodiment 1-4 and comparative example 1-2 into each beaker in such a way that dosage is 80mg/L
The cation type water-soluble polymer polymer of preparation tests cation type water-soluble high score as coagulant, and with national standard method
The turbidity and COD of waste water solution, calculate its turbidity removal rate and COD removal rate, and take 6 groups before and after sub- polymer flocculation
Average value record.Test result is as shown in table 2:
Table 2
3. being used for Treatment of Coking Effluent: taking the bio-chemical effluent of certain coke-oven plant, 1000ppm embodiment is added under stirring
The cation type water-soluble polymer polymer of 1-4 and comparative example 1-2 preparation is kept stirring as coking wastewater coagulation release agent
Uniformly, after standing sedimentation 1min, take supernatant measurement COD and coloration, test result as shown in table 3:
Table 3
It can be seen that the Ionic water-soluble high molecular polymer conduct that embodiment 1-4 is prepared from the data of table 1-3
Flocculant has better effects in the processing of wastewater from chemical industry, dyeing waste water and coking wastewater relative to comparative example 1-2.
In comparative example 1, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride dosage accounts for the 20% of monomer gross mass, obtained sun
Ionic water-soluble high molecular polymer illustrates this in the effect of wastewater from chemical industry, dyeing waste water and Treatment of Coking Effluent and bad
Invention MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride dosage rationally realizes preferable effect.
In comparative example 2, cation type water-soluble acrylic resin and hexamethoxymethyl melamine are 100 by volume:
35, obtained Ionic water-soluble high molecular polymer wastewater from chemical industry, dyeing waste water and Treatment of Coking Effluent effect not
It is good, illustrate that the proportion of cation type water-soluble acrylic resin and hexamethoxymethyl melamine will affect cation type water-soluble
The flocculating effect of high molecular polymer.The hydroxyl and carboxylic in active group and acrylic resin in hexamethoxymethyl melamine
Cross-linking reaction has occurred for itself in remaining active group after base crosslinking, and product viscosity is caused to increase, and density increases, property stability
Decline, flocculating effect are bad.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all utilizations
Equivalent structure or equivalent flow shift made by description of the invention is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of the cation type water-soluble polymer polymer of use in waste water treatment, which is characterized in that including such as
Lower step:
(1) synthesizing cationic type water soluble acrylic resin: preparing includes acrylic acid, butyl acrylate, methacrylic acid-β-hydroxyl
The mixed solution of ethyl ester, methyl methacrylate and initiator is spare, and solvent is fitted into four-necked bottle, heats up 80-100 DEG C, then
The mixed solution of 10-30% is first added into solvent, after keeping the temperature 10-50min, then remaining mixed solution is added dropwise, heat preservation 1-3 is small
When and then addition initiator and solvent, then insulation reaction 1-3 hour, last dropwise addition methylacryoyloxyethyl trimethyl chlorine
Change ammonium, and insulation reaction 1-3 hours, cation type water-soluble acrylic resin is prepared；
(2) synthesizing cationic type water soluble polymer: by cation type water-soluble acrylic resin and hexakis-methoxy methyl
Melamine is 100:10-30 mixing by volume, and cation type water-soluble polymer polymer is prepared；
The time that remaining mixed solution is added dropwise in the step (1) is 2.5-4 hours；
The dosage of the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride accounts for acrylic acid, butyl acrylate, methacrylic acid-β-hydroxyl
The 10-18% of ethyl ester, methyl methacrylate and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride gross mass.
2. the preparation method of cation type water-soluble polymer polymer as described in claim 1, which is characterized in that further include
The preparation step of hexamethoxymethyl melamine: formalin is added in flask, is adjusted pH value to 7.5-9, is added three
Poly cyanamid adjusts pH value to 7.5-9 again, is warming up to 70-80 DEG C, and insulation reaction obtains hexamethylolmelamine, then to
Methanol is added in flask, adjusts pH value to the hexamethylolmelamine between 2-3, being added, heating continues to adjust pH value
2-3 is kept, terminates within finally insulation reaction 1 hour at 45-55 DEG C, hexamethoxymethyl melamine is prepared.
3. the preparation method of cation type water-soluble polymer polymer as claimed in claim 2, which is characterized in that the tune
Saving the solution that pH value is selected is the sodium hydroxide solution of mass percent 10% or the HCl solution of mass percent 10%.
4. the preparation method of cation type water-soluble polymer polymer as claimed in claim 2, which is characterized in that the first
The molar ratio of aldehyde and melamine are as follows: 10:1.
5. the preparation method of cation type water-soluble polymer polymer as described in claim 1, which is characterized in that described third
The weight ratio of olefin(e) acid, butyl acrylate, methacrylic acid-beta-hydroxy ethyl ester and methyl methacrylate are as follows: 1-10:5-20:1-10:
1-10。
6. the preparation method of cation type water-soluble polymer polymer as described in claim 1, which is characterized in that the step
It suddenly further include that auxiliary agent is added after cation type water-soluble acrylic resin and hexamethoxymethyl melamine are mixed in (2)
With with distilling water-reducible step；The auxiliary agent includes one or both of ammonium hydroxide and alcamines.
7. the preparation method of cation type water-soluble polymer polymer as described in claim 1, which is characterized in that described to draw
Hair agent dosage accounts for acrylic acid, butyl acrylate, methacrylic acid-beta-hydroxy ethyl ester, methyl methacrylate and methacryloxypropyl
The 1%-1.5% of ethyl-trimethyl salmiac gross mass.
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| CN104073117A (en) * | 2014-06-23 | 2014-10-01 | 无锡市崇安区科技创业服务中心 | Water-soluble acrylic resin coating and preparation method thereof |
| CN105366789A (en) * | 2015-11-10 | 2016-03-02 | 陕西科技大学 | Multifunctional amphoteric polymer flocculant and preparation method thereof |
| CN105504163A (en) * | 2016-01-20 | 2016-04-20 | 广东溢达纺织有限公司 | Cationic flocculant and preparation method thereof |
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