CN111363091A - Cationic polyacrylamide and preparation method thereof - Google Patents
Cationic polyacrylamide and preparation method thereof Download PDFInfo
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- CN111363091A CN111363091A CN202010364370.9A CN202010364370A CN111363091A CN 111363091 A CN111363091 A CN 111363091A CN 202010364370 A CN202010364370 A CN 202010364370A CN 111363091 A CN111363091 A CN 111363091A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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Abstract
The invention discloses cationic polyacrylamide and a preparation method thereof, relating to the technical field of polyacrylamide, wherein the cationic polyacrylamide comprises the following raw materials: acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt; the cationic polyacrylamide provided by the invention adopts a network penetration micro-crosslinking polymerization method, the hydrolysis degree is close to 0, the ionization degree is high, and the acid and alkali resistance is obviously enhanced; the cationic polyacrylamide provided by the invention has less ionic charge carrying and more blank surfaces, so that a bridge frame is easier to form, and flocculation is better formed; the polyacrylamide product of the invention can generate good flocculation and sedimentation effects on pollutants in different sewage, reduces selectivity, has wider application field range, and greatly enhances the salt resistance and strong acid resistance.
Description
Technical Field
The invention relates to the technical field of polyacrylamide, and particularly relates to cationic polyacrylamide and a preparation method thereof.
Background
The cationic polyacrylamide is a linear high molecular compound, and can form hydrogen bonds by affinity and adsorption with a plurality of substances due to a plurality of active groups. The flocculating negatively charged colloid has the functions of turbidity removal, decoloration, adsorption, adhesion and the like, is suitable for treating wastewater with higher organic colloid content in industries such as dyeing, papermaking, food, building, metallurgy, mineral separation, pulverized coal, oil fields, aquatic product processing, fermentation and the like, and is particularly suitable for dewatering treatment of municipal sewage, municipal sludge, papermaking sludge and other industrial sludge.
The cationic polyacrylamide products sold on the market at present have strong selectivity to the substances in the treated sewage and weak flocculation capacity to strong acid and high-salt sewage, and a large amount of cationic polyacrylamide flocculant is usually added to generate only a small amount of flocculation precipitates, so that the universality is not high.
Disclosure of Invention
The present invention is directed to a cationic polyacrylamide which solves the problems of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 350-450 parts of acrylamide, 250-350 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 250-350 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
As a further scheme of the invention: the composite material comprises the following raw materials in parts by weight: 380-420 parts of acrylamide, 280-320 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 280-320 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
As a further scheme of the invention: the composite material comprises the following raw materials in parts by weight: 400 parts of acrylamide, 300 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 300 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
Another object of the present invention is to provide a method for preparing the above cationic polyacrylamide, comprising the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.5-99.9%, adding an initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into the polymerization kettle, adding an initiator, introducing the nitrogen for 15-25 minutes, adding the initiator, continuously introducing the nitrogen for 30-50 minutes, adding the initiator, continuously introducing the nitrogen for 3-7 minutes, adding the initiator, continuously introducing the nitrogen until the reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise;
step three, granulation: introducing compressed air into the polymerization kettle, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed through a conveying fan for drying, crushing and sieving to obtain the cationic polyacrylamide.
As a further scheme of the invention: the initiators added in the first step are 100-120 parts of sodium hydroxide and 28-35 parts of carboxymethyl cellulose, the initiators added in the second step are 26-34 parts of carboxymethyl cellulose and 270-330 parts of aluminum oxide, the initiators added in the third step are 45-55 parts of carboxymethyl cellulose and 100-120 parts of sodium hydroxide, and the initiators added in the fourth step are 280-320 parts of aluminum oxide and 950-1050 parts of sodium chloride.
As a further scheme of the invention: the initiator added in the first step is 110 parts of sodium hydroxide and 32 parts of carboxymethyl cellulose, the initiator added in the second step is 30 parts of carboxymethyl cellulose and 300 parts of aluminum oxide, the initiator added in the third step is 50 parts of carboxymethyl cellulose and 110 parts of sodium hydroxide, and the initiator added in the fourth step is 300 parts of aluminum oxide and 1000 parts of sodium chloride.
As a further scheme of the invention: and in the second step, introducing nitrogen into the polymerization kettle, adding the initiator, introducing the nitrogen for 20 minutes, adding the initiator, continuously introducing the nitrogen for 40 minutes, adding the initiator, continuously introducing the nitrogen for 5 minutes, adding the initiator, continuously introducing the nitrogen until the reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise.
As a further scheme of the invention: and in the second step, the temperature in the polymerization kettle rises to 86-90 ℃ and then granulation is started.
As a further scheme of the invention: and in the third step, the pressure in the polymerization kettle is not more than 0.02MP after compressed air is pressed in.
As a further scheme of the invention: the temperature of the fluidized bed in the fourth step is constant at 110-130 ℃.
In the invention, the water solution of the cationic polyacrylamide is a polymer electrolyte with positive charges, can effectively agglomerate suspended organic colloid and organic matters, and can strengthen the process of solid-liquid separation, thereby being mainly used for flocculation precipitation of turbid liquid and suspended matters in water or dehydration of organic sludge.
Compared with the prior art, the invention has the beneficial effects that:
1. in the preparation method of the cationic polyacrylamide, the raw materials are polymerized by adopting the polymerization kettle, so that the phenomenon that the rubber blocks are easy to adhere to the kettle wall is overcome, the polymerization kettle has large volume, the number of the rubber blocks produced at one time is large, and the yield is high;
2. in the granulation process of the cationic polyacrylamide preparation method provided by the invention, a synthesis method of cationic polyacrylamide with a micro-crosslinking structure is adopted, so that the product is the cationic polyacrylamide with a network penetrating through micro-crosslinking, and the number average molecular weight can be increased by 3-5 times on the original basis, thereby increasing the salt resistance of the cationic polyacrylamide provided by the invention;
3. for strong acid and strong base, the more the polyacrylamide ionization degree is, the stronger the corresponding acid-base property is, and the weaker the hydrolysis degree is, for some easily soluble polyacrylamides, the more the ionization degree is, the more the corresponding ionized ions are, and the weaker the hydrolysis degree is, generally, the ionization degree is large, the weaker the hydrolysis degree is, conversely, the ionization degree is small, and the hydrolysis degree is, the larger the degree is, the cation polyacrylamide provided by the invention adopts a network penetration micro-crosslinking polymerization method, the hydrolysis degree is close to 0, the ionization degree is large, and the acid-base resistance is obviously enhanced;
4. the action mechanism of polyacrylamide is generally considered to be adsorption-electric neutralization-bridging, but electric neutralization is not the main mechanism. In the flocculation process, when the concentration of macromolecules is lower, macromolecule long chains adsorbed on the surfaces of particles can be adsorbed on the surfaces of other particles at the same time, two or more particles are connected together in a bridging mode to cause flocculation, namely a bridging mechanism for generating a macromolecule flocculation effect, the necessary condition of bridging is that blank surfaces exist on the particles, if the concentration of macromolecules in a solution is very high, the surfaces of the particles are completely covered by the adsorbed macromolecules, the particles can not flocculate through bridging, and the macromolecules play a role in protection at the moment, so that the addition amount of the macromolecule flocculant has an optimal range, the flocculation effect is poor if the addition amount of the macromolecule flocculant exceeds the optimal range, fewer ionic charges are carried, the blank surfaces are more, a bridge is easier to form, and the flocculation is better formed;
5. the polyacrylamide product of the invention can generate good flocculation and sedimentation effects on pollutants in different sewage, reduces selectivity, has wider application field range, and greatly enhances the salt resistance and strong acid resistance.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 350 parts of acrylamide, 250 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 250 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.5%, adding 100 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 100 parts of sodium hydroxide and 28 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 15 minutes, adding 26 parts of carboxymethyl cellulose and 270 parts of aluminum oxide initiator, continuing to introduce the nitrogen for 30 minutes, adding 45 parts of carboxymethyl cellulose and 100 parts of sodium hydroxide initiator, continuing to introduce the nitrogen for 3 minutes, adding 280 parts of aluminum oxide and 950 parts of sodium chloride initiator, continuing to introduce the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 86 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 110 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 2:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 450 parts of acrylamide, 350 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 350 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.9%, adding 120 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 120 parts of sodium hydroxide and 35 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 25 minutes, adding 34 parts of carboxymethyl cellulose and 330 parts of aluminum oxide initiator, continuously introducing the nitrogen for 50 minutes, adding 55 parts of carboxymethyl cellulose and 120 parts of sodium hydroxide initiator, continuously introducing the nitrogen for 7 minutes, adding 320 parts of aluminum oxide and 1050 parts of sodium chloride initiator, continuously introducing the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 90 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 130 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 3:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 380 parts of acrylamide, 280 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 280 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.6%, adding 105 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 105 parts of sodium hydroxide and 29 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 16 minutes, adding 27 parts of carboxymethyl cellulose and 280 parts of aluminum oxide initiator, continuously introducing the nitrogen for 35 minutes, adding 48 parts of carboxymethyl cellulose and 105 parts of sodium hydroxide initiator, continuously introducing the nitrogen for 4 minutes, adding 290 parts of aluminum oxide and 980 parts of sodium chloride initiator, continuously introducing the nitrogen until the reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 88 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 115 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 4:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 420 parts of acrylamide, 320 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 320 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.7%, adding 108 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 108 parts of sodium hydroxide and 30 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 19 minutes, adding 29 parts of carboxymethyl cellulose and 290 parts of aluminum oxide initiator, continuing to introduce the nitrogen for 38 minutes, adding 49 parts of carboxymethyl cellulose and 108 parts of sodium hydroxide initiator, continuing to introduce the nitrogen for 5 minutes, adding 285 parts of aluminum oxide and 990 parts of sodium chloride initiator, continuing to introduce the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 87 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 108 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 5:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 400 parts of acrylamide, 300 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 300 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.8%, adding 110 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 110 parts of sodium hydroxide and 32 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 20 minutes, adding 30 parts of carboxymethyl cellulose and 300 parts of aluminum oxide initiator, continuously introducing the nitrogen for 40 minutes, adding 50 parts of carboxymethyl cellulose and 110 parts of sodium hydroxide initiator, continuously introducing the nitrogen for 5 minutes, adding 300 parts of aluminum oxide and 1000 parts of sodium chloride initiator, continuously introducing the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 88 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 120 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 6:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 360 parts of acrylamide, 340 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 280 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.7%, adding 115 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 112 parts of sodium hydroxide and 33 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 21 minutes, adding 30 parts of carboxymethyl cellulose and 305 parts of aluminum oxide initiator, continuing to introduce the nitrogen for 42 minutes, adding 52 parts of carboxymethyl cellulose and 112 parts of sodium hydroxide initiator, continuing to introduce the nitrogen for 5 minutes, adding 305 parts of aluminum oxide and 1010 parts of sodium chloride initiator, continuing to introduce the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 89 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 122 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 7:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 440 parts of acrylamide, 260 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 310 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.8%, adding 115 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 115 parts of sodium hydroxide and 33 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 22 minutes, adding 32 parts of carboxymethyl cellulose and 320 parts of aluminum oxide initiator, continuing to introduce the nitrogen for 45 minutes, adding 50 parts of carboxymethyl cellulose and 115 parts of sodium hydroxide initiator, continuing to introduce the nitrogen for 6 minutes, adding 310 parts of aluminum oxide and 1020 parts of sodium chloride initiator, continuing to introduce the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 89 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 125 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 8:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 380 parts of acrylamide, 290 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 320 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.7%, adding 118 parts of a sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 120 parts of sodium hydroxide and 33 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 23 minutes, adding 32 parts of carboxymethyl cellulose and 310 parts of aluminum oxide initiator, continuing to introduce the nitrogen for 48 minutes, adding 53 parts of carboxymethyl cellulose and 118 parts of sodium hydroxide initiator, continuing to introduce the nitrogen for 6 minutes, adding 1000 parts of sodium chloride initiator of 310 parts of aluminum oxide, continuing to introduce the nitrogen until the reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 89 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 125 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 9:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 410 parts of acrylamide, 270 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 330 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.8%, adding 110 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 110 parts of sodium hydroxide and 32 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 20 minutes, adding 30 parts of carboxymethyl cellulose and 300 parts of aluminum oxide initiator, continuously introducing the nitrogen for 40 minutes, adding 50 parts of carboxymethyl cellulose and 110 parts of sodium hydroxide initiator, continuously introducing the nitrogen for 5 minutes, adding 300 parts of aluminum oxide and 1000 parts of sodium chloride initiator, continuously introducing the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 88 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 120 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 10:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 440 parts of acrylamide, 280 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 330 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.8%, adding 110 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 110 parts of sodium hydroxide and 32 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 20 minutes, adding 30 parts of carboxymethyl cellulose and 300 parts of aluminum oxide initiator, continuously introducing the nitrogen for 40 minutes, adding 50 parts of carboxymethyl cellulose and 110 parts of sodium hydroxide initiator, continuously introducing the nitrogen for 5 minutes, adding 300 parts of aluminum oxide and 1000 parts of sodium chloride initiator, continuously introducing the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 88 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 120 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
Example 11:
the cationic polyacrylamide comprises the following raw materials in parts by weight: 430 parts of acrylamide, 320 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 330 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
The preparation method comprises the following steps:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.8%, adding 110 parts of sodium hydroxide initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into a polymerization kettle, adding 110 parts of sodium hydroxide and 32 parts of carboxymethyl cellulose initiator, introducing the nitrogen for 20 minutes, adding 30 parts of carboxymethyl cellulose and 300 parts of aluminum oxide initiator, continuously introducing the nitrogen for 40 minutes, adding 50 parts of carboxymethyl cellulose and 110 parts of sodium hydroxide initiator, continuously introducing the nitrogen for 5 minutes, adding 300 parts of aluminum oxide and 1000 parts of sodium chloride initiator, continuously introducing the nitrogen until reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise to 88 ℃;
step three, granulation: introducing compressed air into the polymerization kettle, wherein the pressure in the polymerization kettle is not more than 0.02MP, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed for drying by a material conveying fan, wherein the temperature of the fluidized bed is constant at 120 ℃, and crushing and sieving after drying to obtain the cationic polyacrylamide.
In order to better illustrate the performance of the cationic polyacrylamide provided by the invention, after the new product is subjected to an actual production application case, the following tests are carried out:
and (3) detecting the flocculation effect performance: the results of the cationic polyacrylamide powders prepared in examples 1 to 11 when put into wastewater from a sewage treatment plant in Henan, show that: flocs generated in the wastewater have larger volume and faster settling speed, and the transmittance of the treated sewage at the wavelength of 500nm is more than 99 percent through the analysis of a spectrophotometer.
And (3) detecting acid resistance: the results of treating the cationic polyacrylamide powders prepared in examples 1 to 11 by adding them to the waste pickle liquor containing 11% hydrochloric acid show: the pH value of the pickling waste liquid is less than or equal to 1, and after the product is added and stirred for 60-90 seconds, chlorate suspended matters such as lead, iron and the like in the waste liquid form floc to be rapidly settled, the viscosity of the waste liquid is slight, and the pH value of the waste liquid is unchanged; and in addition, the cationic polyacrylamide powder produced by other companies purchased in the market is added in the same amount, and the mixture is stirred for the same time, so that no reaction is generated, no viscosity exists in waste liquid, and the pH value is unchanged. It can be seen that the cationic polyacrylamide powder provided by the present invention has enhanced acid resistance.
And (3) detecting the salt resistance: the results of treating the cationic polyacrylamide powder prepared in examples 1 to 11 by adding it to the pickle liquor wastewater with 5% of sodium chloride concentration show that: the pickle sewage, the sodium chloride concentration of which is 5 percent, the turbidity of which is 650 percent and the suspended matter of which is 400 percent, is matched with the polyaluminium chloride for use, and after the pickle sewage is added and stirred, the pickle sewage, the sodium chloride concentration of which is 3 percent, the turbidity of which is 180 percent and the suspended matter of which is 55 percent; and adding the cationic polyacrylamide powder produced by other companies on the market in the same amount, and stirring to obtain the pickle sewage with the sodium chloride concentration of 5 percent, the turbidity of 400 and the suspended matter of 325. It can be seen that the cationic polyacrylamide powder provided by the present invention has enhanced salt resistance.
And (3) detecting the dissolution speed: adding deionized water into the cationic polyacrylamide powder prepared in the examples 1-11 to dissolve the cationic polyacrylamide powder to prepare a solution with the mass concentration of 0.08%, wherein the dissolving time of the cationic polyacrylamide powder is kept within the time range of 5-15 minutes; in addition, deionized water is added into cationic polyacrylamide powder produced by certain environmental protection technology company Limited in Henan, which is purchased from the market to be dissolved to prepare a solution with the mass concentration of 0.08 percent as a comparative example, and the dissolution time of the cationic polyacrylamide powder produced by the company is between 50 and 70 minutes, so that the cationic polyacrylamide powder provided by the invention has better solubility and high dissolution speed.
Furthermore, it should be understood that various changes and modifications of the present invention can be made by those skilled in the art after reading the above teachings of the present invention, and these equivalents also fall within the scope of the present invention as defined by the appended claims.
Claims (10)
1. The cationic polyacrylamide is characterized by comprising the following raw materials in parts by weight:
350-450 parts of acrylamide, 250-350 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 250-350 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
2. The cationic polyacrylamide of claim 1, wherein the cationic polyacrylamide comprises the following raw materials in parts by weight: 380-420 parts of acrylamide, 280-320 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 280-320 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
3. The cationic polyacrylamide of claim 2, wherein the cationic polyacrylamide comprises the following raw materials in parts by weight: 400 parts of acrylamide, 300 parts of methacrylic acid dimethylamino ethyl methyl chloride salt and 300 parts of acrylic acid dimethylamino ethyl methyl chloride salt.
4. A method for preparing the cationic polyacrylamide according to any one of claims 1 to 3, comprising the steps of:
step one, batching: weighing acrylamide, methacrylic acid dimethylamino ethyl methyl chloride salt and acrylic acid dimethylamino ethyl methyl chloride salt according to parts by weight into a batching kettle, adding purified water to enable the concentration of a solution in the batching kettle to be 99.5-99.9%, adding an initiator, and feeding the solution into a polymerization kettle;
step two, polymerization: introducing nitrogen into the polymerization kettle, adding an initiator, introducing the nitrogen for 15-25 minutes, adding the initiator, continuously introducing the nitrogen for 30-50 minutes, adding the initiator, continuously introducing the nitrogen for 3-7 minutes, adding the initiator, continuously introducing the nitrogen until the reaction liquid in the polymerization kettle becomes viscous, and closing all valves after the temperature begins to rise;
step three, granulation: introducing compressed air into the polymerization kettle, pressing the polymerized rubber blocks out of the polymerization kettle, adding the pressed rubber blocks into the dispersion liquid, and starting a granulator for granulation;
step four, drying: and conveying the small-particle rubber blocks produced by the granulator into a fluidized bed through a conveying fan for drying, crushing and sieving to obtain the cationic polyacrylamide.
5. The method as claimed in claim 4, wherein the initiator added in the first step is 100-120 parts of sodium hydroxide and 28-35 parts of carboxymethyl cellulose, the initiator added in the second step is 26-34 parts of carboxymethyl cellulose and 270-330 parts of aluminum oxide, the initiator added in the third step is 45-55 parts of carboxymethyl cellulose and 100-120 parts of sodium hydroxide, and the initiator added in the fourth step is 280-320 parts of aluminum oxide and 950-1050 parts of sodium chloride.
6. The method for preparing cationic polyacrylamide according to claim 5, wherein the initiator added in the first step is 110 parts of sodium hydroxide and 32 parts of carboxymethyl cellulose, the initiator added in the second step is 30 parts of carboxymethyl cellulose and 300 parts of aluminum oxide, the initiator added in the third step is 50 parts of carboxymethyl cellulose and 110 parts of sodium hydroxide, and the initiator added in the fourth step is 300 parts of aluminum oxide and 1000 parts of sodium chloride.
7. The method for preparing cationic polyacrylamide according to claim 4, wherein in the second step, nitrogen is introduced into the polymerization kettle, the initiator is added after the nitrogen is introduced for 20 minutes, the initiator is added after the nitrogen is further introduced for 40 minutes, the initiator is added after the nitrogen is further introduced for 5 minutes, the nitrogen is further introduced until the reaction solution in the polymerization kettle becomes viscous, and all valves are closed after the temperature begins to rise.
8. The method for preparing cationic polyacrylamide according to claim 4, wherein in the second step, granulation is started after the temperature in the polymerization vessel is increased to 86 to 90 °.
9. The method for preparing cationic polyacrylamide according to claim 4, wherein the pressure in the polymerization vessel after the compressed air is introduced in the third step is not more than 0.02 MP.
10. The method for preparing cationic polyacrylamide as claimed in claim 4, wherein the temperature of the fluidized bed in the fourth step is constant at 110-130 °.
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Cited By (2)
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| CN113479983A (en) * | 2021-08-20 | 2021-10-08 | 湖南江冶机电科技股份有限公司 | Use method of polyacrylamide as flocculating agent for lead plaster sedimentation in waste lead-acid storage battery |
| CN113880973A (en) * | 2021-08-20 | 2022-01-04 | 湖南江冶机电科技股份有限公司 | Preparation method of polyacrylamide for lead plaster sedimentation in lead-acid storage battery |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5733462A (en) * | 1996-10-03 | 1998-03-31 | Cytec Technology Corp. | Cationic water-soluble polymer precipitation in salt solutions |
| CN101648740A (en) * | 2009-06-29 | 2010-02-17 | 上海东升新材料有限公司 | Cationic flocculant and preparation method thereof |
| CN104355385A (en) * | 2014-10-27 | 2015-02-18 | 无锡伊佩克科技有限公司 | Industrial wastewater purification flocculant and preparation method thereof |
-
2020
- 2020-04-30 CN CN202010364370.9A patent/CN111363091A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5733462A (en) * | 1996-10-03 | 1998-03-31 | Cytec Technology Corp. | Cationic water-soluble polymer precipitation in salt solutions |
| CN101648740A (en) * | 2009-06-29 | 2010-02-17 | 上海东升新材料有限公司 | Cationic flocculant and preparation method thereof |
| CN104355385A (en) * | 2014-10-27 | 2015-02-18 | 无锡伊佩克科技有限公司 | Industrial wastewater purification flocculant and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113479983A (en) * | 2021-08-20 | 2021-10-08 | 湖南江冶机电科技股份有限公司 | Use method of polyacrylamide as flocculating agent for lead plaster sedimentation in waste lead-acid storage battery |
| CN113880973A (en) * | 2021-08-20 | 2022-01-04 | 湖南江冶机电科技股份有限公司 | Preparation method of polyacrylamide for lead plaster sedimentation in lead-acid storage battery |
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