CN104356268A - Preparation method for magnesium ion-containing modified polyacrylamide - Google Patents
Preparation method for magnesium ion-containing modified polyacrylamide Download PDFInfo
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- CN104356268A CN104356268A CN201410678526.5A CN201410678526A CN104356268A CN 104356268 A CN104356268 A CN 104356268A CN 201410678526 A CN201410678526 A CN 201410678526A CN 104356268 A CN104356268 A CN 104356268A
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- polyacrylamide
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Abstract
The invention relates to a preparation method for magnesium ion-containing modified polyacrylamide. The preparation method comprises the following steps of: adding magnesium hydroxide solution in a four-necked flask, and then adding acrylamide and deionized water to completely dissolve the acrylamide monomer; continuously charging nitrogen and dropwise adding ammonia water; heating the system in a water bath, and adding ammonium persulphate, sodium hydrogen sulphite, urea and EDTA (ethylene diamine tetraacetic acid); taking out after 4.5-5.0 hours and pouring in the flask, rapidly transferring into a vacuum drying oven and curing a colloid; and cooling to a room temperature; cleaning with the mixed solution of isopropanol and deionized water, and then washing with deionized water; drying in a drying oven with a constant temperature of 80 DEG C for 48 hours, and crushing to obtain the magnesium ion-containing modified polyacrylamide finished product. The method is mature and convenient, and easy to control; the prepared magnesium ion-containing modified polyacrylamide is environment-friendly and excellent in performance. The use amount of the magnesium ion-containing modified polyacrylamide is reduced by more than 10% than that of polyacrylamide commonly used by sewage treatment plants.
Description
Technical field
The present invention relates to a kind of modified polyacrylamide, particularly relate to a kind of as sewage treatment plant residual Sludge Dewatering Flocculant, excellent performance and eco-friendly containing magnesium ion modified polyacrylamide preparation method.
Background technology
At present, sewage work of China about 80% have employed thickening integrated technique, in order to reach higher dehydrating effect object, before sludge dewatering, carries out medicament conditioning, thus improves dewatering performance of sludge.In conventional sludge conditioner (flocculation agent), polyacrylamide (Polyacrylamide, PAM) application is the most general.Polyacrylamide is a kind of organic polymer coargulator, and it increases mud flco by effects such as adsorption bridgings, improves sludge settling and dehydrating effect.The polyacrylamide that current sewage work uses mainly comes in import, the high price of import polyacrylamide, becomes each sewage work's running cost integral part.
Modified polyacrylamide refers to and is improved by conventional polypropylene acid amides synthesis and production process, introduce different materials, produce the water-soluble modified polyacrylamide that performance is improved, structure changes to some extent, make it to become better, the eco-friendly modified polyacrylamide of performance.
Aqueous solution polymerization be by monomer and initiator soluble in water, the polyreaction of carrying out under solution state is a kind of important synthetic method in Polymer Synthesizing process.The viscosity ratio mass polymerization of polymerization system is low, mixing and heat radiation are than being easier to, production operation and temperature are all easy to control, evaporation of water also can be utilized to get rid of heat of polymerization, be the method both at home and abroad being generally used for preparing polyacrylamide, this method is more ripe and have with low cost, easy to operate, simple from laboratory to course of industrialization, the advantages such as safety and environmental protection.
The present invention utilizes water solution polymerization process to prepare the modified polyacrylamide containing magnesium ion, the environmentally friendly Mg of employing
2+, thus guarantee obtained modified polyacrylamide environmental safety, and Mg
2+introducing also accelerate the natural degradation of polyacrylamide, slow down the toxicological effects brought to soil and biology when the mud even overcome containing polyacrylamide returns environment.
Summary of the invention
The object of the present invention is to provide a kind of processability excellent in, eco-friendly magnesium ion modified polyacrylamide preparation method.Utilize water solution polymerization process, in the polymerization process of polyacrylamide, introduce Mg
2+, prepare have stronger flocculation ability containing magnesium ion modified polyacrylamide.
The object of the invention is to be achieved by the following scheme:
1, fill a prescription:
Namely magnesium hydroxide liquid 5 ~ 10mL is joined
Acrylamide (AM) 90g
Sodium hydroxide solution 1M
Hydrochloric acid 1M
Ammonium persulphate 70 ~ 80mg
Sodium bisulfite 8 ~ 12 mg
Urea 10 ~ 15mg
EDTA 6～10 mg
2, preparation method
(1) to learn from else's experience washing, dried four-hole boiling flask, first add the magnesium hydroxide solution of namely joining, then be fixed on 250 r/min on constant temperature electric mixer after adding acrylamide and 200mL deionized water and at the uniform velocity stir, acrylamide monomer is dissolved completely.
(2) continuing to pass in above-mentioned system in the process of nitrogen 28 ~ 35min, drip ammoniacal liquor 0.3 ~ 0.5mL, and control temperature is being 35 ~ 40 DEG C of scopes.
(3) system be placed in water-bath heat, temperature-stable in 63 ~ 65 DEG C time, add ammonium persulphate, sodium bisulfite, urea and EDTA, and with the pH of sodium hydroxide solution or hydrochloric acid regulation system in 7.5 ~ 8.2 scopes.
(4) keep the reaction of system continuously stirring, rotating speed is 200 ~ 250 r/min, is taken out by the mixed solution of reaction system and pour beaker into after 4.5 ~ 5.0 hours, and proceeds to rapidly in 80 ~ 82 DEG C of vacuum drying ovens and turn out colloid, then takes out and is cooled to room temperature.
(5) adopt volume ratio to be that Virahol and the deionized water mixing solutions of 1:1 carries out 4 ~ 6 times to above-mentioned colloid of turning out and wash, then with deionized water 3 ~ 5 flushings, remove washing process generation white precipitate, obtain a kind of new modified Laemmli sample.
(6) sample after washing in 80 DEG C of thermostatic drying chambers dry 48 hours, takes out after putting into moisture eliminator cooling, pulverizes with pulverizer, the final finished product obtained containing magnesium ion modified polyacrylamide.
Namely magnesium hydroxide liquid of joining of the present invention is formulated by dropwise adding sodium hydroxide solution in soluble magnesium salts solution, wherein solubility magnesium salts refers to magnesium sulfate, magnesium chloride or magnesium nitrate, and in soluble magnesium salts solution, the mass concentration of magnesium salts is 2 ~ 10 g/L.
Of the present invention continuing passes into nitrogen, and its air flow is 1 L/min.
Described ammoniacal liquor, refers to the volume mixture liquid of ammoniacal liquor and water 1:1.
The invention has the advantages that:
Adopt water solution polymerization process, method maturation is convenient, easily controls; Obtained contains magnesium ion modified polyacrylamide environmental friendliness, superior performance.In the application of disposing of sewage treatment plant's excess sludge, for same dosage, same dehydration equipment condition, the polyacrylamide of the moisture percentage in sewage sludge use more conventional than sewage work after containing magnesium ion modified polyacrylamide conditioning dehydration is adopted to reduce more than 10%.
Embodiment
embodiment 1
(1) to learn from else's experience washing, dried four-hole boiling flask, namely what first to add 5mL be 2g/L with magnesium chloride mass concentration joins magnesium hydroxide liquid, add 90g acrylamide (AM) monomer and 200ml deionized water again, after be fixed on constant temperature electric mixer, at the uniform velocity stir with 250 r/min rotating speeds, acrylamide monomer is dissolved completely.
(2) continue to pass into nitrogen 30min in system, and drip 0.3 mL ammoniacal liquor in the process.
(3) above-mentioned reaction system is put into 65 DEG C of thermostat water baths to heat, add 70mg ammonium persulphate, 8mg sodium bisulfite, 10mg urea and 6mgEDTA simultaneously, regulate reaction soln pH to be 7.5 with hydrochloric acid or sodium hydroxide solution.
(4) continue to stir, rotating speed is 250 r/min, successive reaction 4.5 hours, takes out and pours beaker into, and be placed in rapidly after colloid turned out by 80 DEG C of vacuum drying ovens and be cooled to room temperature.
(5) adopt the 1:1 mixing solutions of Virahol and deionized water to carry out 4 times to colloid wash, and with deionized water rinsing 3 times, remove washing process generation white precipitate, finally obtain modified polyacrylamide sample.
(6) sample after washing is placed in dry 48 hours of the thermostatic drying chamber of 80 DEG C, takes out and puts into after moisture eliminator is cooled to room temperature, pulverize, namely obtain containing Mg with pulverizer
2+modified polyacrylamide.
After measured, prepared containing Mg in magnesium ion modified polyacrylamide
2+content is 32.7ppm.
embodiment 2
(1) to learn from else's experience washing, dried four-hole boiling flask, namely what first to add 5mL be 5g/L with magnesium sulfate mass concentration joins magnesium hydroxide liquid, add 90g acrylamide (AM) monomer and 200ml deionized water again, after be fixed on constant temperature electric mixer, at the uniform velocity stir with 250 r/min rotating speeds, acrylamide monomer is dissolved completely.
(2) continue to pass into nitrogen 32min in system, and drip 0.4 mL ammoniacal liquor in the process.
(3) above-mentioned reaction system is put into 66 DEG C of thermostat water baths to heat, add 72mg ammonium persulphate, 10mg sodium bisulfite, 12mg urea and 8mgEDTA simultaneously, regulate reaction soln pH to be 7.6 with hydrochloric acid or sodium hydroxide solution.
(4) continue to stir, rotating speed is 250 r/min, successive reaction 4.75 hours, takes out and pours beaker into, and be placed in rapidly after colloid turned out by 80 DEG C of vacuum drying ovens and be cooled to room temperature.
(5) adopt the 1:1 mixing solutions of Virahol and deionized water to carry out 5 times to colloid wash, and with deionized water rinsing 3 times, remove washing process generation white precipitate, finally obtain modified polyacrylamide sample.
(6) the modified polyacrylamide sample after washing is placed in dry 48 hours of the thermostatic drying chamber of 80 DEG C, takes out and puts into after moisture eliminator is cooled to room temperature, pulverize, namely obtain containing Mg with pulverizer
2+modified polyacrylamide.
After measured, prepared containing Mg in magnesium ion modified polyacrylamide
2+content is 65.4ppm.
embodiment 3
(1) to learn from else's experience washing, dried four-hole boiling flask, namely what first to add 6mL be 6g/L with magnesium nitrate mass concentration joins magnesium hydroxide liquid, add 90g acrylamide (AM) monomer and 200ml deionized water again, after be fixed on constant temperature electric mixer, at the uniform velocity stir with 250 r/min rotating speeds, acrylamide monomer is dissolved completely.
(2) continue to pass into nitrogen 35min in system, and drip 0.5 mL ammoniacal liquor in the process.
(3) above-mentioned reaction system is put into 68 DEG C of thermostat water baths to heat, add 72mg ammonium persulphate, 10mg sodium bisulfite, 12mg urea and 10mgEDTA simultaneously, regulate reaction soln pH to be 7.8 with hydrochloric acid or sodium hydroxide solution.
(4) continue to stir, rotating speed is 200 r/min, successive reaction 5 hours, takes out and pours beaker into, and be placed in rapidly after colloid turned out by 80 DEG C of vacuum drying ovens and be cooled to room temperature.
(5) adopt the 1:1 mixing solutions of Virahol and deionized water to carry out 6 times to colloid wash, and with deionized water rinsing 4 times, remove washing process generation white precipitate, finally obtain modified polyacrylamide sample.
(6) the modified polyacrylamide sample after washing is placed in dry 48 hours of the thermostatic drying chamber of 80 DEG C, takes out and puts into after moisture eliminator is cooled to room temperature, pulverize, namely obtain containing Mg with pulverizer
2+modified polyacrylamide.
After measured, prepared containing Mg in magnesium ion modified polyacrylamide
2+content is 102.8ppm.
embodiment 4
(1) to learn from else's experience washing, dried four-hole boiling flask, namely what first to add 5mL be 10g/L with magnesium sulfate mass concentration joins magnesium hydroxide liquid, add 90g acrylamide (AM) monomer and 200ml deionized water again, after be fixed on constant temperature electric mixer, at the uniform velocity stir with 250 r/min rotating speeds, acrylamide monomer is dissolved completely.
(2) continue to pass into nitrogen 32min in system, and drip 0.5mL ammoniacal liquor in the process.
(3) above-mentioned reaction system is put into 68 DEG C of thermostat water baths to heat, add 75mg ammonium persulphate, 12mg sodium bisulfite, 12mg urea and 10mgEDTA simultaneously, regulate reaction soln pH to be 8.0 with hydrochloric acid or sodium hydroxide solution.
(4) continue to stir, rotating speed is 200 r/min, successive reaction 5 hours, takes out and pours beaker into, and be placed in rapidly after colloid turned out by 80 DEG C of vacuum drying ovens and be cooled to room temperature.
(5) adopt the 1:1 mixing solutions of Virahol and deionized water to carry out 5 times to colloid wash, and with deionized water rinsing 3 times, remove washing process generation white precipitate, finally obtain modified polyacrylamide sample.
(6) the modified polyacrylamide sample after washing is placed in dry 48 hours of the thermostatic drying chamber of 80 DEG C, takes out and puts into after moisture eliminator is cooled to room temperature, pulverize, namely obtain containing Mg with pulverizer
2+modified polyacrylamide.
After measured, prepared containing Mg in magnesium ion modified polyacrylamide
2+content is 132.4ppm.
embodiment 5
(1) to learn from else's experience washing, dried four-hole boiling flask, namely what first to add 10mL be 4g/L with magnesium chloride mass concentration joins magnesium hydroxide liquid, add 90g acrylamide (AM) monomer and 200ml deionized water again, after be fixed on constant temperature electric mixer, at the uniform velocity stir with 250 r/min rotating speeds, acrylamide monomer is dissolved completely.
(2) continue to pass into nitrogen 35min in system, and drip 0.5 mL ammoniacal liquor in the process.
(3) above-mentioned reaction system is put into 68 DEG C of thermostat water baths to heat, add 75mg ammonium persulphate, 12mg sodium bisulfite, 15mg urea and 10mgEDTA simultaneously, regulate reaction soln pH to be 8.5 with hydrochloric acid or sodium hydroxide solution.
(4) continue to stir, rotating speed is 200 r/min, successive reaction 5 hours, takes out and pours beaker into, and be placed in rapidly after colloid turned out by 80 DEG C of vacuum drying ovens and be cooled to room temperature.
(5) adopt the 1:1 mixing solutions of Virahol and deionized water to carry out 6 times to colloid wash, and with deionized water rinsing 4 times, remove washing process generation white precipitate, finally obtain modified polyacrylamide sample.
(6) the modified polyacrylamide sample after washing is placed in dry 48 hours of the thermostatic drying chamber of 80 DEG C, takes out and puts into after moisture eliminator is cooled to room temperature, pulverize, can obtain containing Mg with pulverizer
2+modified polyacrylamide.
After measured, prepared containing Mg in magnesium ion modified polyacrylamide
2+content is 117.1ppm.
embodiment 6
Adopt respectively prepared by the invention process case 3, case study on implementation 4 and case study on implementation 5 to process initial haze containing magnesium ion modified polyacrylamide association aggregation aluminum chloride (PAC) be 1823 NTU stone slab waste water, measure the turbidity of its supernatant liquor after flocculation sediment.Only with PAC(polyacrylamide) flocculation sediment after supernatant fluid turbidity be 60.2NTU, and use the turbidity containing magnesium ion modified polyacrylamide of PAC and above-mentioned 3 kinds of associating to be respectively 21.5NTU, 15.4NTU and 18.8 NTU, the highest clearance of turbidity is 99.16%, and effect ratio is used alone PAC and improves 74.4%.
embodiment 7
Adopt respectively prepared by the invention process case 3, case study on implementation 4 and case study on implementation 5 containing magnesium ion modified polyacrylamide and West, Fuzhou City sewage work use the commercially available cationic-type polyacrylamide of molecular weight 600-800 ten thousand to West sewage treatment plant residual mud (sludge specific resistance 2.14 × 10
13cm/g) flocculation conditioning is carried out, and sludge specific resistance after measuring conditioning.After commercially available cationic-type polyacrylamide conditioning, sludge specific resistance is 2.52 × 10
10cm/g, and use above-mentioned 3 kinds to be respectively 1.21 × 10 containing sludge specific resistance after the conditioning of magnesium ion modified polyacrylamide
10cm/g, 0.66 × 10
10cm/g and 1.04 × 10
10cm/g, wherein best effect improves 73.8% than commercially available cationic-type polyacrylamide.
embodiment 8
On the basis of case study on implementation 7, adopt plate-and-frame filter press to carry out press dewatering to the mud after 4 kinds of polyacrylamide conditionings, and measure the water ratio of the rear mud cake of dehydration.After adopting the dehydration of commercially available cationic-type polyacrylamide, moisture content of the cake is 84.2%, and use above-mentioned 3 kinds to be respectively 78. 5%, 73.8% and 76.3% containing moisture content of the cake after the dehydration of magnesium ion modified polyacrylamide, wherein best effect decreases 10.4% only than moisture content of the cake after the dehydration of the commercially available cationic-type polyacrylamide of employing.
Claims (5)
1., containing a preparation method for Mg ion modification polyacrylamide, it is characterized in that:
1) fill a prescription:
Namely magnesium hydroxide liquid 5 ~ 10mL is joined
Acrylamide 90g
Sodium hydroxide solution 1M
Hydrochloric acid 1M
Ammonium persulphate 70 ~ 80mg
Sodium bisulfite 8 ~ 12 mg
Urea 10 ~ 15mg
EDTA 6～10 mg；
2) preparation method
(1) to learn from else's experience washing, dried four-hole boiling flask, first add the magnesium hydroxide solution of namely joining, then be fixed on 250 r/min on constant temperature electric mixer after adding acrylamide and 200mL deionized water and at the uniform velocity stir, acrylamide monomer is dissolved completely;
(2) continuing to pass in above-mentioned system in the process of nitrogen 28 ~ 35min, drip ammoniacal liquor 0.3 ~ 0.5mL, and control temperature is being 35 ~ 40 DEG C of scopes;
(3) system be placed in water-bath heat, temperature-stable in 63 ~ 65 DEG C time, add ammonium persulphate, sodium bisulfite, urea and EDTA, and with the pH of sodium hydroxide solution or hydrochloric acid regulation system in 7.5 ~ 8.2 scopes;
(4) keep the reaction of system continuously stirring, rotating speed is 200 ~ 250 r/min, is taken out by the mixed solution of reaction system and pour beaker into after 4.5 ~ 5.0 hours, and proceeds to rapidly in 80 ~ 82 DEG C of vacuum drying ovens and turn out colloid, then takes out and is cooled to room temperature;
(5) adopt volume ratio to be that Virahol and the deionized water mixing solutions of 1:1 carries out 4 ~ 6 times to above-mentioned colloid of turning out and wash, then with deionized water 3 ~ 5 flushings, remove washing process generation white precipitate, obtain a kind of new modified Laemmli sample;
(6) sample after washing in 80 DEG C of thermostatic drying chambers dry 48 hours, takes out after putting into moisture eliminator cooling, pulverizes with pulverizer, the final finished product obtained containing magnesium ion modified polyacrylamide.
2. a kind of preparation method containing Mg ion modification polyacrylamide according to claim 1, is characterized in that described magnesium hydroxide liquid of namely joining is formulated by dropwise adding sodium hydroxide solution in soluble magnesium salts solution.
3. a kind of preparation method containing Mg ion modification polyacrylamide according to claim 2, it is characterized in that solubility magnesium salts refers to magnesium sulfate, magnesium chloride or magnesium nitrate, in soluble magnesium salts solution, the mass concentration of magnesium salts is 2 ~ 10 g/L.
4. a kind of preparation method containing Mg ion modification polyacrylamide according to claim 1, it is characterized in that described continuing passes into nitrogen, its air flow is 1 L/min.
5. the preparation method of a kind of modified polyacrylamide according to claim 1, is characterized in that described ammoniacal liquor, refers to the volume mixture liquid of ammoniacal liquor and water 1:1.
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| CN110122269A (en) * | 2019-06-18 | 2019-08-16 | 大连地拓环境科技有限公司 | A kind of high gradient slope is sowed grass seeds by duster with granule agent and its application method |
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