CN101618937B - Hydrophobic cation polymeric flocculant preparation method - Google Patents
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Abstract
The invention discloses hydrophobic cation polymeric flocculant and a preparation method and application thereof. The preparation method comprises the following steps: adding acrylamide, methyl oxiranyl trimethyl ammonium chloride and octadecyl vinyl ether into a reaction vessel with the mol ratio of (89.5-5.5) to (10-40) to (0.5-3.5); adding a urea cation surface active; adding deionized water and stirring to dissolve the mixture in the reaction vessel;, raising the temperature of the mixed solution to 30-35 DEG C; adding octadecyl vinyl ether into the reaction vessel again and stirring evenly, adding an evocating agent into the reaction vessel; keeping the temperature at 30-35 DEG C to carry out polyreaction; obtaining a translucent or milky colloidal product after the reaction is carried out for 3-6 hours; pouring the translucent or milky colloidal product into acetone to be precipitated; taking out the sediment; and extracting the sentiment for 24 hours by ethanol to obtain the hydrophobic cation polymeric flocculant. The invention has the advantages of simple preparation process and remarkable flocculating and dewatering effect for substrate sludge.
Description
Technical field
The invention discloses a kind of hydrophobic cation polymeric flocculant, the invention also discloses a kind of preparation method and application thereof of hydrophobic cation polymeric flocculant.
Background technology
Flocculent precipitation is one of main method that is used at present sludge dewatering, and it makes the mud particle take off steady sedimentation rapidly by effects such as bridge formation, absorption, associations, reaches the effect of quick mud-water separation.Because river lakebed mud particle is tiny, relative density is little, is difficult for sinking, compacting, and water content is high and be difficult for dehydration, therefore must add high-performance sludge dewatering flocculation agent in the bed mud treating processes.Organic polymer coargulator is a kind of polymkeric substance that has good throwing out, with respect to inorganic polymer flocculant, it is little to have consumption, flocculation ability is strong, advantages such as flocculation rate is fast, especially in that to improve aspect flco physical strength and the dewatering efficiency thereof effect more outstanding, so the production of organic polymer coargulator and application development are very fast.Organic polymer coargulator mainly is divided into anionic, cationic and amphoteric, wherein cationic high-molecular flocculant has characteristics such as high charge density, sterilization because of it, electronegative mud granule is had flocculating effect preferably and becomes the first-selected flocculation agent of sludge dewatering.
Synthetic methylacryoyloxyethyl trimethyl ammonium chloride (DMC), acrylyl oxy-ethyl-trimethyl salmiac (DAC), diallyldimethylammonium chloride (DMDAAC) etc. and acrylamide (AM) copolymerization of mainly containing of present cationic high-molecular flocculant, but commercially available positively charged ion organic floculant can not improve the bottom-mud dewatering rate by force effectively because of its hydrophobicity, cause the desilting bed mud to be difficult to rapid mummification, therefore need to improve the hydrophobicity of flocculation agent, thereby improve the bottom-mud dewatering rate.People such as Shen Yiding have studied acrylamide (AM), diallyldimethylammonium chloride (DMDAAC), the copolymerization of octadecyl acrylate (OA), and be used for flocculation to paper waste, but this polymkeric substance is very limited to the throwing out of bed mud, and methylacryoyloxyethyl trimethyl ammonium chloride (DMC) has high reaction activity and high, and easily make the multipolymer of higher molecular weight, have certain hydrophobicity concurrently, so the present invention adopts methylacryoyloxyethyl trimethyl ammonium chloride (DMC) as cationic monomer, experimental results show that the multipolymer that is generated has good flocculating effect to bed mud.People such as Chen Hong have studied the copolymerization of acrylamide (AM), diallyldimethylammonium chloride (DMDAAC), butyl acrylate (BA), and use as flocculation agent, because the hydrophobicity of octadecyl vinyl ether is stronger than octadecyl acrylate and butyl acrylate, and can not produce excessive polymerism in the polymerization process, product is also more soluble in water, so the introducing of octadecyl vinyl ether can effectively improve the bottom-mud dewatering rate.
Summary of the invention
One of purpose of the present invention is to overcome the deficiencies in the prior art, and a kind of dewatering rate hydrophobic cation polymeric flocculant preferably is provided.
Another object of the present invention provides a kind of preparation method of hydrophobic cation polymeric flocculant.
Of the present invention also have a purpose to provide the application of a kind of hydrophobic cation polymeric flocculant in containing dirt water flocculation dehydration.
According to technical scheme provided by the invention, described hydrophobic cation polymeric flocculant has following structure:
The solid content of described hydrophobic cation polymeric flocculant is 20%～30%, and limiting viscosity is 380～700cm
3G
-1, cationic degree is 10%～40%.
Above-mentioned hydrophobic cation polymeric flocculant preparation method comprises following steps:
A, take by weighing mol ratio for (89.5～56.5): (10～40): the acrylamide of (0.5～3.5), methylacryoyloxyethyl trimethyl ammonium chloride and octadecyl vinyl ether are standby, and described three kinds of material total amounts are counted the total monomer amount;
B, acrylamide and methylacryoyloxyethyl trimethyl ammonium chloride that step a is taken by weighing add in the reaction vessel, add the cats product that accounts for the urea of total monomer amount 0.5%～2wt% and account for total monomer amount 6%～7wt% again, add deionized water and stirring at last, make the mixture dissolving in the reaction vessel, the add-on of deionized water and total monomer amount weight ratio are (70～80): (20～30);
C, the mixing solutions of step b is warming up to 30～35 ℃, in reaction vessel, adds again and account for the octadecyl vinyl ether of total monomer amount 0.5%～3.5mol% and stir;
D, add the initiator of the 0.2%～0.5wt% account for the total monomer amount in the reaction vessel of step c, insulation is carried out polyreaction to 30～35 ℃, obtains translucent or milky gluey product behind 3～6h;
E, product are poured in the acetone, make its precipitation, behind the taking-up throw out throw out are used ethanol extracting 24h again, promptly obtain hydrophobic cation polymeric flocculant.
Described cats product is a cetyl trimethylammonium bromide.Described initiator is that ammonium persulphate, sodium bisulfite mass ratio are 2: 1 mixture.
The application of described hydrophobic polymeric flocculant in containing dirt water flocculation dehydration.
Hydrophobic cation polymeric flocculant of the present invention has been compared with the prior art following advantage:
The hydrophobic cation polymeric flocculant of the present invention's preparation is to introduce the long-chain hydrophobic grouping in the molecular structure of traditional cationic polyacrylamide, in the time of advantage such as have traditional cationic polyacrylamide molecular weight height, the adsorption bridging ability is strong, flocculating effect good, use range is wide, it is strong to have hydrophobicity concurrently, characteristics such as dehydration rate height.
The present invention adopts simple preparation technology, characteristics such as have economy, be suitable for.The polymkeric substance of preparation in feedwater, wastewater treatment, oil production, desilt and dredge, all there is purposes more widely in fields such as mining, daily-use chemical industry, and are particularly remarkable for the flocculation dewatering effect of bed mud.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1:
With acrylamide, the methylacryoyloxyethyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, urea, deionized water adds in the four-hole boiling flask, stir and heat up and the adding octadecyl vinyl ether, add initiator (ammonium persulphate after the violent stirring, the mass ratio of sodium bisulfite is 2: 1 a mixture), insulation reaction was prepared hydrophobic cation polymeric flocculant in 4 hours, participate in the acrylamide of reaction, methylacryoyloxyethyl trimethyl ammonium chloride and octadecyl vinyl ether total amount are designated as the total monomer amount, wherein acrylamide content accounts for the 89.5mol% of total monomer amount, methylacryoyloxyethyl trimethyl ammonium chloride content accounts for the 10mol% of total monomer amount, cetyl trimethylammonium bromide content accounts for the 6wt% of total monomer amount, urea content accounts for the 2wt% of total monomer amount, the weight ratio of total monomer amount and deionized water is 20: 80, octadecyl vinyl ether content accounts for the 0.5mol% of total monomer amount, initiator content accounts for the 0.2wt% of total monomer amount, and product is represented with NUM1.
Concrete preparation method is as follows:
(1), 15.90g acrylamide, 5.19g methylacryoyloxyethyl trimethyl ammonium chloride and 0.37g octadecyl vinyl ether is standby, described three kinds of material total amounts are counted the total monomer amount;
(2), acrylamide that step (1) is taken by weighing and methylacryoyloxyethyl trimethyl ammonium chloride add in the four-hole boiling flask, the cetyl trimethylammonium bromide that adds 0.43g urea and 1.29g again adds in the four-hole boiling flask, add 86g deionized water and stirring at last, make the mixture dissolving in the reaction vessel;
(3), place water-bath to make that mixed reaction solution is warming up to 35 ℃ in the four-hole boiling flask four-hole boiling flask of step (2), add the 0.37g octadecyl vinyl ether, violent stirring 20 minutes;
(4), in the four-hole boiling flask of step (3), add initiator 0.042g (mixture of ammonium persulphate 0.028g, sodium bisulfite 0.014g), insulation is carried out polyreaction to 35 ℃, reacts to stop after 4 hours, obtains translucent or milky gluey product;
(5), step (4) obtains translucent or milky gluey product, uses acetone precipitation, throw out used ethanol extracting 24h again after taking out throw out, is white solid after the ethanol extracting, solid content is 20%, limiting viscosity is 700cm
3G
-1, cationic degree is 10%, dissolution time is 30 minutes, promptly obtains hydrophobic cation polymeric flocculant.
Embodiment 2:
With acrylamide, the methylacryoyloxyethyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, urea, deionized water adds in the four-hole boiling flask, stir and heat up and the adding octadecyl acrylate, add initiator (ammonium persulphate after the violent stirring, the mass ratio of sodium bisulfite is 2: 1 a mixture), insulation reaction was prepared hydrophobic cation polymeric flocculant in 4 hours, participate in the acrylamide of reaction, methylacryoyloxyethyl trimethyl ammonium chloride and octadecyl vinyl ether total amount are designated as the total monomer amount, wherein acrylamide content accounts for the 86.5mol% of total monomer amount, methylacryoyloxyethyl trimethyl ammonium chloride content accounts for the 10mol% of total monomer amount, cetyl trimethylammonium bromide content accounts for the 6wt% of total monomer amount, urea content accounts for the 2wt% of total monomer amount, the weight ratio of total monomer amount and deionized water is 20: 80, octadecyl vinyl ether content accounts for the 3.5mol% of total monomer amount, initiator content accounts for the 0.2wt% of total monomer amount, and product is represented with NUM2.
Concrete preparation method is as follows:
(1), 15.37g acrylamide, 5.19g methylacryoyloxyethyl trimethyl ammonium chloride and 0.37g octadecyl vinyl ether is standby, described three kinds of material total amounts are counted the total monomer amount;
(2), acrylamide that step (1) is taken by weighing and methylacryoyloxyethyl trimethyl ammonium chloride add in the four-hole boiling flask, the cetyl trimethylammonium bromide that adds 0.46g urea and 1.39g again adds in the four-hole boiling flask, add 93g deionized water and stirring at last, make the mixture dissolving in the reaction vessel;
(3), place water-bath to make that mixed reaction solution is warming up to 31 ℃ in the four-hole boiling flask four-hole boiling flask of step (2), add the 2.59g octadecyl vinyl ether, violent stirring 20 minutes;
(4), in the four-hole boiling flask of step (3), add initiator 0.045g (mixture of ammonium persulphate 0.030g, sodium bisulfite 0.015g), insulation is carried out polyreaction to 31 ℃, reacts to stop after 4 hours, obtains translucent or milky gluey product;
(5), step (4) obtains translucent or milky gluey product, uses acetone precipitation, throw out used ethanol extracting 24h again after taking out throw out, is white solid after the ethanol extracting, solid content is 20%, limiting viscosity is 558cm
3G
-1, cationic degree is 10%, dissolution time is 70 minutes, promptly obtains hydrophobic cation polymeric flocculant.
Embodiment 3:
With acrylamide, the methylacryoyloxyethyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, urea, deionized water adds in the four-hole boiling flask, stir and heat up and the adding octadecyl acrylate, add initiator (ammonium persulphate after the violent stirring, the mass ratio of sodium bisulfite is 2: 1 a mixture), insulation reaction was prepared hydrophobic cation polymeric flocculant in 4 hours, participate in the acrylamide of reaction, methylacryoyloxyethyl trimethyl ammonium chloride and octadecyl vinyl ether total amount are designated as the total monomer amount, wherein acrylamide content accounts for the 56.5mol% of total monomer amount, methylacryoyloxyethyl trimethyl ammonium chloride content accounts for the 40mol% of total monomer amount, cetyl trimethylammonium bromide content accounts for the 6wt% of total monomer amount, urea content accounts for the 2wt% of total monomer amount, the weight ratio of total monomer amount and deionized water is 20: 80, octadecyl vinyl ether content accounts for the 3.5mol% of total monomer amount, initiator content accounts for the 0.2wt% of total monomer amount, and product is represented with NUM3.
Concrete preparation method is as follows:
(1), 10.04g acrylamide, 20.77g methylacryoyloxyethyl trimethyl ammonium chloride and 0.37g octadecyl vinyl ether is standby, described three kinds of material total amounts are counted the total monomer amount;
(2), acrylamide that step (1) is taken by weighing and methylacryoyloxyethyl trimethyl ammonium chloride add in the four-hole boiling flask, the cetyl trimethylammonium bromide that adds 0.67g urea and 2.00g again adds in the four-hole boiling flask, add 134g deionized water and stirring at last, make the mixture dissolving in the reaction vessel;
(3), place water-bath to make that mixed reaction solution is warming up to 30 ℃ in the four-hole boiling flask four-hole boiling flask of step (2), add the 2.59g octadecyl vinyl ether, violent stirring 20 minutes;
(4), in the four-hole boiling flask of step (3), add initiator 0.066g (mixture of ammonium persulphate 0.044g, sodium bisulfite 0.022g), insulation is carried out polyreaction to 30 ℃, reacts to stop after 4 hours, obtains translucent or milky gluey product;
(5), step (4) obtains translucent or milky gluey product, uses acetone precipitation, throw out used ethanol extracting 24h again after taking out throw out, is white solid after the ethanol extracting, solid content is 20%, limiting viscosity is 380cm
3G
-1, cationic degree is 40%, dissolution time is 50 minutes, promptly obtains hydrophobic cation polymeric flocculant.
Embodiment 4:
With acrylamide, the methylacryoyloxyethyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, urea, deionized water adds in the four-hole boiling flask, stir and heat up and the adding octadecyl vinyl ether, add initiator (ammonium persulphate after the violent stirring, the mass ratio of sodium bisulfite is 2: 1 a mixture), insulation reaction was prepared hydrophobic cation polymeric flocculant in 4 hours, participate in the acrylamide of reaction, methylacryoyloxyethyl trimethyl ammonium chloride and octadecyl vinyl ether total amount are designated as the total monomer amount, wherein acrylamide content accounts for the 86.5mol% of total monomer amount, methylacryoyloxyethyl trimethyl ammonium chloride content accounts for the 10mol% of total monomer amount, cetyl trimethylammonium bromide content accounts for the 6wt% of total monomer amount, urea content accounts for the 2wt% of total monomer amount, the weight ratio of total monomer amount and deionized water is 30: 70, octadecyl vinyl ether content accounts for the 3.5mol% of total monomer amount, initiator content accounts for the 0.2wt% of total monomer amount, and product is represented with NUM4.
Concrete preparation method is as follows:
(1), 15.37g acrylamide, 5.19g methylacryoyloxyethyl trimethyl ammonium chloride and 0.37g octadecyl vinyl ether is standby, described three kinds of material total amounts are counted the total monomer amount;
(2), acrylamide that step (1) is taken by weighing and methylacryoyloxyethyl trimethyl ammonium chloride add in the four-hole boiling flask, the cetyl trimethylammonium bromide that adds 0.46g urea and 1.39g again adds in the four-hole boiling flask, add 54g deionized water and stirring at last, make the mixture dissolving in the reaction vessel;
(3), place water-bath to make that mixed reaction solution is warming up to 30 ℃ in the four-hole boiling flask four-hole boiling flask of step (2), add the 2.59g octadecyl vinyl ether, violent stirring 20 minutes;
(4), in the four-hole boiling flask of step (3), add initiator 0.045g (mixture of ammonium persulphate 0.030g, sodium bisulfite 0.015g), insulation is carried out polyreaction to 30 ℃, reacts to stop after 4 hours, obtains translucent or milky gluey product;
(5), step (4) obtains translucent or milky gluey product, uses acetone precipitation, throw out used ethanol extracting 24h again after taking out throw out, is white solid after the ethanol extracting, solid content is 30%, limiting viscosity is 410cm
3G
-1, cationic degree is 10%, dissolution time is 40 minutes, promptly obtains hydrophobic cation polymeric flocculant.
Embodiment 5:
With acrylamide, the methylacryoyloxyethyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, urea, deionized water adds in the four-hole boiling flask, stir and heat up and the adding octadecyl vinyl ether, add initiator (ammonium persulphate after the violent stirring, the mass ratio of sodium bisulfite is 2: 1 a mixture), insulation reaction was prepared hydrophobic cation polymeric flocculant in 4 hours, participate in the acrylamide of reaction, methylacryoyloxyethyl trimethyl ammonium chloride and octadecyl vinyl ether total amount are designated as the total monomer amount, wherein acrylamide content accounts for the 86.5mol% of total monomer amount, methylacryoyloxyethyl trimethyl ammonium chloride content accounts for the 10mol% of total monomer amount, cetyl trimethylammonium bromide content accounts for the 6wt% of total monomer amount, urea content accounts for the 2wt% of total monomer amount, the weight ratio of total monomer amount and deionized water is 20: 80, octadecyl vinyl ether content accounts for the 3.5mol% of total monomer amount, initiator content accounts for the 0.5wt% of total monomer amount, and product is represented with NUM5.
Concrete preparation method is as follows:
(1), 15.37g acrylamide, 5.19g methylacryoyloxyethyl trimethyl ammonium chloride and 0.37g octadecyl vinyl ether is standby, described three kinds of material total amounts are counted the total monomer amount;
(2), acrylamide that step (1) is taken by weighing and methylacryoyloxyethyl trimethyl ammonium chloride add in the four-hole boiling flask, the cetyl trimethylammonium bromide that adds 0.46g urea and 1.39g again adds in the four-hole boiling flask, add 93g deionized water and stirring at last, make the mixture dissolving in the reaction vessel;
(3), place water-bath to make that mixed reaction solution is warming up to 30 ℃ in the four-hole boiling flask four-hole boiling flask of step (2), add the 2.59g octadecyl vinyl ether, violent stirring 20 minutes;
(4), in the four-hole boiling flask of step (3), add initiator 0.117g (mixture of ammonium persulphate 0.078g, sodium bisulfite 0.039g), insulation is carried out polyreaction to 30 ℃, reacts to stop after 4 hours, obtains translucent or milky gluey product;
(5), step (4) obtains translucent or milky gluey product, uses acetone precipitation, throw out used ethanol extracting 24h again after taking out throw out, is white solid after the ethanol extracting, solid content is 20%, limiting viscosity is 543cm
3G
-1, cationic degree is 10%, dissolution time is 100 minutes, promptly obtains hydrophobic cation polymeric flocculant.
The hydrophobic cation polymeric flocculant of the present invention's preparation can be used as the flocculation dewatering that a kind of novel sludge dehydrating agent is widely used in river, lakebed mud, sets forth concrete effect with application example below.
Application example:
The flocculation dewatering that above-mentioned synthetic hydrophobic cation polymeric flocculant is used for moon gulf, Taihu Lake bed mud is handled, and compare with commercially available cationic-type polyacrylamide (CPAM), polydimethyl two rare propyl ammonium chlorides (PDMDAAC), result sees Table 1.
Table 1 hydrophobic type cationic polyacrylamide of the present invention and reference substance
Flocculation dewatering treatment effect to moon gulf, Taihu Lake bed mud compares
From above result as can be known dewatering cationic type terpolymer the dehydrating effect of bed mud is better than commercially available CPAM, PDMDAAC.
Claims (3)
1. hydrophobic cation polymeric flocculant preparation method, it is characterized in that: described method comprises following steps:
A, take by weighing mol ratio for (89.5～56.5): (10～40): the acrylamide of (0.5～3.5), methylacryoyloxyethyl trimethyl ammonium chloride and octadecyl vinyl ether are standby, and described three kinds of material total amounts are counted the total monomer amount;
B, acrylamide and methylacryoyloxyethyl trimethyl ammonium chloride that step a is taken by weighing add in the reaction vessel, add the cats product that accounts for the urea of total monomer amount 0.5%～2wt% and account for total monomer amount 6%～7wt% again, add deionized water and stirring at last, make the mixture dissolving in the reaction vessel, the add-on of deionized water and total monomer amount weight ratio are (70～80): (20～30);
C, the mixing solutions of step b is warming up to 30～35 ℃, in reaction vessel, adds again and account for the octadecyl vinyl ether of total monomer amount 0.5%～3.5mol% and stir;
D, add the initiator of the 0.2%～0.5wt% account for the total monomer amount in the reaction vessel of step c, insulation is carried out polyreaction to 30～35 ℃, obtains translucent or milky gluey product behind 3～6h;
E, product are poured in the acetone, make its precipitation, behind the taking-up throw out throw out are used ethanol extracting 24h again, promptly obtain hydrophobic cation polymeric flocculant;
Hydrophobic cation polymeric flocculant has following structure:
2. method according to claim 1 is characterized in that, described cats product is a cetyl trimethylammonium bromide.
3. method according to claim 1 is characterized in that, described initiator is that ammonium persulphate, sodium bisulfite mass ratio are 2: 1 mixture.
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