CN114773543B - Modified polyacrylamide papermaking retention and drainage aid and preparation method thereof - Google Patents
Modified polyacrylamide papermaking retention and drainage aid and preparation method thereof Download PDFInfo
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- CN114773543B CN114773543B CN202210682935.7A CN202210682935A CN114773543B CN 114773543 B CN114773543 B CN 114773543B CN 202210682935 A CN202210682935 A CN 202210682935A CN 114773543 B CN114773543 B CN 114773543B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/06—Paper forming aids
- D21H21/10—Retention agents or drainage improvers
Abstract
The invention provides a modified polyacrylamide papermaking retention and drainage aid and a preparation method thereof, relating to the field of high polymer polymerization and comprising the following steps: carrying out polycondensation reaction on melamine and aldehyde compounds to obtain a melamine polycondensate; carrying out copolymerization reaction on the melamine polycondensate and p-methylstyrene to obtain a modified melamine polycondensate; carrying out sulfonation reaction on the modified melamine polycondensate and a sulfonating agent to obtain a sulfonated modified melamine polycondensate; and adding the sulfonated modified melamine polycondensate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride, a structure regulator, a surfactant, a chain transfer agent, deionized water and an initiator into a reactor to perform copolymerization reaction to obtain the modified polyacrylamide papermaking retention and drainage aid. The modified polyacrylamide papermaking retention and filtration aid prepared by the method has excellent solubility, good temperature resistance and salt tolerance, remarkably improves papermaking retention rate, reduces white water turbidity, and reduces the load of white water treatment.
Description
Technical Field
The invention relates to the technical field of high polymer polymerization, in particular to a modified polyacrylamide papermaking retention and drainage aid and a preparation method thereof.
Background
Polyacrylamide (PAM) is a water-soluble high-molecular polymer, can introduce various ionic groups to obtain specific properties, is widely applied to various fields such as chemical industry, metallurgy, geology, coal, petroleum, papermaking and water treatment, and has the name of "all-industry auxiliary agent". The polyacrylamide contains charges opposite to those of the fibers and the fillers in the molecular weight, is used as a retention and drainage aid for papermaking, enhances the adsorption force among the fibers in the paper pulp by utilizing the charges carried by the polyacrylamide, thereby enhancing the retention rate of the fibers, and achieves the effects of reducing the loss of the fibers and the fillers, reducing the concentration and ash content of the pulp on a net and prolonging the service life of the formed net by changing the flocculation state of papermaking pulp.
In the pulping process, pulp fibers are sheared and damaged by pulping equipment to generate a plurality of fine fibers, but most of the fine fibers are lost along with white water in the papermaking process, the existing papermaking retention and drainage aid can improve retention of the fine fibers to a certain degree, but the retention effect is still poor. Meanwhile, with the increase of the closed circulation degree of the white water, the content of inorganic salts in the white water is increased, which is not beneficial to the dissolution of the retention and drainage aids for papermaking and the adsorption of the retention and drainage aids to fine fibers.
Chinese patent CN101157016A discloses a preparation method of bentonite binary microparticle papermaking retention and drainage aid, which is prepared from montmorillonite, sodium hexametaphosphate, sodium carbonate, silica sol and aluminum hydroxide, improves retention of fine fiber substances, reduces cost and reduces discharge of waste. However, the content of inorganic salt in the product is very high, and the content of the inorganic salt is only higher along with the increase of the closed circulation degree of the white water, so that the product is not beneficial to the dissolution of the retention and drainage aid for papermaking and the improvement of the retention of fine fibers.
Disclosure of Invention
The embodiment of the invention provides a modified polyacrylamide papermaking retention and drainage aid and a preparation method thereof, which can provide a salt-resistant and temperature-resistant papermaking retention and drainage aid with excellent solubility, remarkably improve papermaking retention rate, especially retention of fine fibers, reduce white water turbidity, lighten the load of white water treatment and improve production efficiency.
In a first aspect, the present invention provides a preparation method of a modified polyacrylamide papermaking retention and drainage aid, comprising the following steps:
(1) carrying out polycondensation reaction on melamine and aldehyde compounds to obtain a melamine polycondensate;
(2) carrying out copolymerization reaction on the melamine polycondensate and p-methylstyrene to obtain a modified melamine polycondensate;
(3) carrying out sulfonation reaction on the modified melamine polycondensate and a sulfonating agent to obtain a sulfonated modified melamine polycondensate;
(4) and adding the sulfonated modified melamine polycondensate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride, a structure regulator, a surfactant, a chain transfer agent, deionized water and an initiator into a reactor to carry out copolymerization reaction, thereby obtaining the modified polyacrylamide papermaking retention and drainage aid.
Preferably, in the step (1), the aldehyde compound is at least one of formaldehyde and paraformaldehyde;
the mass ratio of the melamine to the aldehyde compound is 1 (3-3.5).
Preferably, in the step (1), the polycondensation reaction is performed at 60-90 ℃ for 1-3 h.
Preferably, the step (1) comprises:
putting the melamine into deionized water, uniformly stirring, and then adding the aldehyde compound to perform polycondensation reaction;
wherein the temperature for uniformly stirring is 40-60 ℃; the mass ratio of the melamine to the deionized water is 1 (1-2).
Preferably, in the step (2), the copolymerization reaction is carried out at 70-100 ℃ for 0.5-2 h.
Preferably, in the step (2), the mass ratio of the p-methylstyrene to the melamine polycondensate is 1 (10-1000).
Preferably, in the step (3), the sulfonating agent is at least one of sodium sulfite and sodium bisulfite;
the mass ratio of the modified melamine polycondensate to the sulfonating agent is 1 (1-1.5).
Preferably, in the step (3), the sulfonation reaction is performed at 80-100 ℃ for 1-3 hours.
Preferably, in the step (4), the surfactant is at least one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate;
the structure regulator is N, N-methylene bisacrylamide.
Preferably, the initiator is a persulfate; the persulfate is potassium persulfate, sodium persulfate, ammonium persulfate, calcium persulfate, potassium hydrogen persulfate, sodium hydrogen persulfate, ammonium hydrogen persulfate or calcium hydrogen persulfate;
the chain transfer agent is formate and thioglycollic acid; the formate is at least one of ammonium formate, sodium formate and potassium formate.
Preferably, the step (4) includes:
adding the sulfonated modified melamine polycondensate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride, the structure regulator, the surfactant and deionized water into a reactor, uniformly mixing to obtain a mixed solution, introducing nitrogen into the mixed solution, and then adding the initiator and the chain transfer agent to perform copolymerization reaction to obtain the modified polyacrylamide papermaking retention and drainage aid.
Preferably, in the step (4), after the mixed solution is obtained, the following steps are further included:
adjusting the pH value of the mixed solution to 7-7.5;
and adjusting the temperature of the mixed solution to 0-5 ℃.
Preferably, in the step (4), the nitrogen is introduced for 30-40 min;
the reaction time of the copolymerization reaction is 1.5-2.5 h.
Preferably, the modified polyacrylamide papermaking retention and drainage aid is prepared from the following raw materials in parts by weight: 5-50 parts of sulfonated modified melamine polycondensate, 150-200 parts of acrylamide, 80-100 parts of methacryloyloxyethyl trimethyl ammonium chloride, 20-50 parts of structure regulator, 1-15 parts of surfactant, 300-800 parts of deionized water, 0.01-1 part of chain transfer agent and 0.001-1 part of initiator.
In a second aspect, the invention provides a modified polyacrylamide papermaking retention and drainage aid prepared by the preparation method of any one of the first aspect.
Preferably, the dissolving time of the modified polyacrylamide papermaking retention and drainage aid in water is less than 30 min; the retention rate of paper making is more than 90 percent; the white water turbidity is less than 20NYU, and the white water viscosity retention rate is more than 90%.
Compared with the prior art, the invention at least has the following beneficial effects:
according to the invention, firstly, a modified melamine polycondensate with carbon-carbon double bonds is obtained through copolymerization of the melamine polycondensate and p-methylstyrene, then a sulfonated modified melamine polycondensate with sulfonic acid groups is obtained based on sulfonation reaction, and finally the modified polyacrylamide papermaking retention and drainage aid is prepared by copolymerization of the sulfonated modified melamine polycondensate, acrylamide and methacryloyloxyethyl trimethyl ammonium chloride. Compared with the common papermaking retention and drainage aid, the modified polyacrylamide papermaking retention and drainage aid has strong papermaking retention and white water turbidity performance and high dissolution speed. Due to the addition of the sulfonated modified melamine polycondensate, the association effect among polyacrylamide molecules is enhanced, and a net structure is formed, so that the adsorption on fine fibers and fillers is enhanced; meanwhile, the sulfonated modified melamine polycondensate provides a large number of sulfonic acid groups for polyacrylamide molecular chains, so that the dissolving speed of polyacrylamide in water is effectively improved, and the influence of inorganic salt ions on a polyacrylamide aqueous solution is reduced, thereby enhancing the salt resistance and temperature resistance of polyacrylamide molecules in white water. Meanwhile, the polyacrylamide is enabled to form a micro-crosslinked net structure by adding the structure regulator, so that the net catching effect on the fine fibers and the filler is further enhanced, and the turbidity of the white water is greatly reduced. Therefore, the modified polyacrylamide papermaking retention and drainage aid remarkably improves the retention rate of papermaking, reduces the turbidity of white water, lightens the load of white water treatment, and improves the production efficiency of the papermaking retention and drainage aid in the papermaking industry.
The modified polyacrylamide papermaking retention and drainage aid prepared in the invention has the following properties: the dissolution time in water is less than 30min, and the excellent solubility is achieved; the retention rate of paper making is more than 90 percent and is as high as 96.5 percent; the turbidity of the white water is less than 20NYU, the viscosity retention rate of the white water at 50-80 ℃ after 3 times of circulation is more than 90%, great convenience is brought to the papermaking industry, the preparation method is simple, the preparation raw materials are simple and easy to obtain, the cost is low, and the method is suitable for continuous large-scale production of enterprises.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete, the technical solutions of the present invention will be described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the protection scope of the present invention.
The invention provides a preparation method of modified polyacrylamide papermaking retention and drainage aid, which comprises the following steps:
(1) carrying out polycondensation reaction on melamine and aldehyde compounds to obtain a melamine polycondensate;
(2) carrying out copolymerization reaction on the melamine polycondensate and p-methylstyrene to obtain a modified melamine polycondensate;
(3) carrying out sulfonation reaction on the modified melamine polycondensate and a sulfonating agent to obtain a sulfonated modified melamine polycondensate;
(4) and adding the sulfonated modified melamine polycondensate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride, a structure regulator, a surfactant, a chain transfer agent, deionized water and an initiator into a reactor to perform copolymerization reaction to obtain the modified polyacrylamide papermaking retention and drainage aid.
According to some preferred embodiments, in step (1), the aldehyde compound is at least one of formaldehyde and paraformaldehyde;
the mass ratio of melamine to the aldehyde compound is 1 (3 to 3.5) (for example, 1:3, 1:3.1, 1:3.2, 1:3.3, 1:3.4, or 1: 3.5).
At least one of them is a mixture of any one or any several of them mixed in any ratio.
According to some preferred embodiments, in the step (1), the polycondensation reaction is a polycondensation reaction at 60 to 90 ℃ (for example, may be 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃ or 90 ℃) for 1 to 3 hours (for example, may be 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours).
According to some preferred embodiments, step (1) comprises:
putting melamine into deionized water, stirring and mixing uniformly, and then adding an aldehyde compound to carry out polycondensation reaction;
wherein the temperature for stirring and mixing is 40-60 deg.C (for example, 40 deg.C, 45 deg.C, 50 deg.C, 55 deg.C or 60 deg.C); the mass ratio of the melamine to the deionized water is 1 (1-2) (for example, 1:1, 1:1.2, 1:1.5, 1:1.8 or 1: 2).
It should be noted that, because melamine is slightly soluble in water at normal temperature, in order to accelerate the dissolution process and shorten the preparation time of the modified polyacrylamide papermaking retention and drainage aid, the temperature is raised to 40-60 ℃ during stirring and mixing.
In the invention, the viscosity-average molecular weight of the melamine polycondensate is 800-1000, and the polymerization degree is controlled by controlling the amount of the polycondensation agent. Experiments prove that the melamine polycondensate is difficult to polymerize when the consumption of the polycondensation agent (namely the aldehyde compound) is too small; if the amount of the polycondensation agent is too large, the melamine polycondensate is liable to undergo implosion.
According to some preferred embodiments, in the step (2), the copolymerization reaction is carried out at 70 to 100 ℃ (for example, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃ or 100 ℃) for 0.5 to 2 hours (for example, 0.5 hour, 1 hour, 1.5 hour, 1.8 hour or 2 hours).
According to some preferred embodiments, in the step (2), the mass ratio of the p-methylstyrene to the melamine polycondensate is 1 (10 to 1000) (for example, may be 1:10, 1:15, 1:20, 1:40, 1:50, 1:80, 1:100, 1:200, 1:500, 1:600, 1:800 or 1: 1000).
In the invention, the modified melamine polycondensate with carbon-carbon double bonds is obtained through the copolymerization reaction of the melamine polycondensate and the p-methylstyrene, so that the modified melamine polycondensate can be polymerized with acrylamide double bonds, and a network structure can be formed subsequently.
In a preferred embodiment, in step (2), p-methylstyrene is added dropwise to the reactor containing the melamine polycondensate, so that the p-methylstyrene can be successfully grafted onto the melamine polycondensate by adding dropwise thereto with sufficient mixing. It should be noted that, in step (2), an isomer of p-methylstyrene, for example, m-methylstyrene or o-methylstyrene, may also be used.
According to some preferred embodiments, in step (3), the sulfonating agent is at least one of sodium sulfite and sodium bisulfite;
the mass ratio of the modified melamine polycondensate to the sulfonating agent is 1 (1 to 1.5) (for example, 1:1, 1:1.1, 1:1.2, 1:1.3, 1:1.4, or 1: 1.5).
According to some preferred embodiments, in the step (3), the sulfonation reaction is performed at 80 to 100 ℃ (for example, 80 ℃, 82 ℃, 85 ℃, 90 ℃, 92 ℃, 95 ℃ or 100 ℃) for 1 to 3 hours (for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours).
In the invention, the sulfonated modified melamine polycondensate also effectively enhances the association effect among polyacrylamide molecules and forms a net structure, thereby enhancing the adsorption on fine fibers and fillers, improving the retention on the fine fibers and improving the retention rate of papermaking. Meanwhile, the sulfonated modified melamine polycondensate carries a large number of sulfonic acid groups through sulfonation reaction, the monomer containing the sulfonic acid groups is easier to dissolve, and the salt resistance of the modified polyacrylamide papermaking retention and drainage aid is improved by utilizing the characteristics of insensitivity of the sulfonic acid groups to cations and high charge density.
According to some preferred embodiments, in the step (4), the surfactant is at least one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate;
the structure regulator is N, N-methylene bisacrylamide.
In the invention, the addition of the surfactant further improves the solubility of the prepared modified polyacrylamide papermaking retention and drainage aid in water. The addition of the structure regulator enables the polyacrylamide to form a micro-crosslinked net structure, further enhances the net capturing effect on the fine fibers and the filler, and greatly reduces the turbidity of the white water.
According to some preferred embodiments, the initiator is a persulfate; the persulfate is potassium persulfate, sodium persulfate, ammonium persulfate, calcium persulfate, potassium hydrogen persulfate, sodium hydrogen persulfate, ammonium hydrogen persulfate or calcium hydrogen persulfate;
the chain transfer agent is formate and thioglycollic acid; the formate is at least one of ammonium formate, sodium formate and potassium formate.
According to some preferred embodiments, step (4) comprises:
adding sulfonated modified melamine polycondensate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride, a structure regulator, a surfactant and deionized water into a reactor, uniformly mixing to obtain a mixed solution, introducing nitrogen into the mixed solution, and then adding an initiator and a chain transfer agent to perform copolymerization reaction to obtain the modified polyacrylamide papermaking retention and filtration aid.
According to some preferred embodiments, after the mixed solution is obtained in step (4), the following steps are further included:
adjusting the pH value of the mixed solution to 7-7.5;
and adjusting the temperature of the mixed solution to 0-5 ℃.
Experiments prove that the pH of the mixed solution is adjusted to 7-7.5 (for example, the pH can be 7, 7.1, 7.2, 7.3, 7.4 or 7.5), and specifically, the pH can be adjusted by using a sodium hydroxide aqueous solution, but not limited to. Therefore, the method can avoid the influence of the acid-base property of the reaction medium on the decomposition rate of the initiator, ensure the polymerization degree of the modified polyacrylamide papermaking retention and filtration aid, and the environment of the reaction medium is neutral, so that the preparation process is more environment-friendly.
In the invention, the viscosity-average molecular weight of the prepared modified polyacrylamide papermaking retention and drainage aid is further regulated by a continuous transfer agent to be 600-800 w. Experiments prove that if the viscosity average molecular weight of the prepared retention and drainage aid for papermaking is less than 600w, the formed network structure is incomplete, and the retention rate of the retention and drainage aid for papermaking is influenced; if the viscosity average molecular weight of the prepared retention and drainage aid for papermaking is more than 800w, the solubility is poor, and the production efficiency in the papermaking industry is influenced.
Experiments prove that because the copolymerization reaction in the step (4) is an exothermic reaction, when the copolymerization reaction is initiated at a higher temperature, the higher temperature increases the collision chance of free radicals, so that the reaction rate is accelerated, the heat release is too fast, the control is not easy, and the dangers of overflow, even scalding and the like can occur; however, when the copolymerization reaction is initiated at a relatively low temperature, the possibility of radical collision is reduced, the chain growth is slowed, and the molecular weight of polyacrylamide is affected, so that the temperature of the mixed solution is adjusted to 0 to 5 ℃ (for example, 0 ℃, 1 ℃, 2 ℃, 3 ℃, 4 ℃ or 5 ℃). Thus, the copolymerization reaction can be completed in the step (3) by means of the heat release of the self reaction after the initiation, and the temperature of the system is about 80 ℃ at the end of the reaction.
In the invention, water is used as a reaction medium for copolymerization reaction, so that the cost is low, the influence of an organic solvent on environmental pollution can be eliminated, the preparation process is simple, and heating is not required. And the environment of the reaction medium is neutral, the preparation process is environment-friendly, pollution-free, low in energy consumption, and the product is non-toxic and non-corrosive, does not produce secondary pollution, and accords with the development direction of green and environment-friendly chemical additives.
According to some preferred embodiments, in step (4), the nitrogen is introduced for 30-40min (for example, 30min, 32min, 35min, 38min or 40 min);
the reaction time of the copolymerization reaction is 1.5 to 2.5 hours (for example, 1.5 hours, 2 hours or 2.5 hours).
In the present invention, since oxygen is used as a polymerization inhibitor and affects the copolymerization reaction of polyacrylamide, nitrogen is introduced to remove oxygen to ensure the normal progress of the polymerization reaction.
According to some preferred embodiments, the parts by weight of the raw materials used for preparing the modified polyacrylamide papermaking retention and drainage aid are as follows: 5 to 50 parts (for example, may be 5 parts, 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts or 50 parts), 150 to 200 parts of acrylamide (for example, may be 150 parts, 155 parts, 160 parts, 165 parts, 170 parts, 175 parts, 180 parts, 185 parts, 190 parts, 195 parts or 200 parts), 80 to 100 parts of methacryloyloxyethyltrimethylammonium chloride (for example, may be 80 parts, 82 parts, 85 parts, 88 parts, 90 parts, 92 parts, 95 parts, 98 parts or 100 parts), 20 to 50 parts of a structure modifier (for example, may be 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts or 50 parts), 1 to 15 parts of a surfactant (for example, may be 1 part, 2 parts, 5 parts, 6 parts, 8 parts, 10 parts, 12 parts or 15 parts), 300 to 800 parts of deionized water (for example, may be 300 parts, 310 parts, 350 parts or 50 parts), or 100 parts of a surfactant, 400 parts, 450 parts, 500 parts, 550 parts, 600 parts, 650 parts, 700 parts, 750 parts, or 800 parts), a chain transfer agent 0.01 to 1 part (which may be, for example, 0.01 part, 0.02 part, 0.05 part, 0.08 part, 0.1 part, 0.2 part, 0.5 part, 0.6 part, 0.8 part, or 1 part), an initiator 0.001 to 1 part (which may be, for example, 0.001 part, 0.002 part, 0.005 part, 0.008 part, 0.01 part, 0.02 part, 0.05 part, 0.08 part, 0.1 part, 0.2 part, 0.5 part, 0.6 part, 0.8 part, or 1 part).
In the present invention, the influence of polyacrylamide on the retention in papermaking and the white water turbidity is adjusted by adjusting the amounts of the initiator, the chain transfer agent and the sulfonated modified melamine polycondensate. The modified polyacrylamide papermaking retention and drainage aid obtained by the preparation method is colloidal polyacrylamide, and the colloidal polyacrylamide is dried, ground and packaged, so that the modified polyacrylamide papermaking retention and drainage aid is more convenient to store and transport, and the transportation cost can be further reduced.
The invention also provides a modified polyacrylamide papermaking retention and drainage aid prepared by the preparation method.
According to some preferred embodiments, the modified polyacrylamide papermaking retention and drainage aid has the following properties:
the dissolving time in water is less than 30 min; the retention rate of paper making is more than 90 percent; the turbidity of the white water is less than 20NYU, and the viscosity retention rate of the white water is more than 90 percent.
In order to more clearly illustrate the technical scheme and advantages of the present invention, a modified polyacrylamide papermaking retention and drainage aid and a preparation method thereof are described in detail by using several examples.
In the following examples, the mass of the sulfonated modified melamine polycondensate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride, structure modifier, surfactant, deionized water, chain transfer agent, and initiator are all expressed in parts by weight;
wherein the adopted formaldehyde is a formaldehyde water solution with the mass fraction of 37-40%.
Example 1
(1) Adding 1 part of melamine and 1 part of deionized water into a three-neck flask provided with a stirrer, a reflux condenser and a thermometer, heating to 50 ℃ for dissolution, slowly adding 3 parts of formaldehyde, and carrying out polycondensation reaction at 70 ℃ for 2 hours to obtain a melamine polycondensate;
(2) slowly adding 1 part of p-methylstyrene into 50 parts of melamine polycondensate, and carrying out copolymerization reaction for 1h at the temperature of 80 ℃ to obtain a modified melamine polycondensate;
(3) slowly adding 1 part of sulfonating agent (sodium bisulfite water solution with solid content of 50%) into 0.5 part of modified melamine polycondensate, and performing sulfonation reaction at 100 ℃ for 1h to obtain sulfonated modified melamine polycondensate;
(4) adding 10 parts of sulfonated modified melamine polycondensate, 180 parts of acrylamide, 80 parts of methacryloyloxyethyl trimethyl ammonium chloride, 30 parts of structure regulator (N, N-methylene bisacrylamide), 5 parts of surfactant (sodium dodecyl benzene sulfonate) and 695 parts of deionized water into a reactor, uniformly mixing to obtain a mixed solution, adjusting the pH value of the mixed solution to 7.0, and adjusting the temperature of the mixed solution to 0 ℃; and then introducing nitrogen into the mixed solution for 30min, adding 0.005 part of initiator (potassium persulfate) and 0.03 part of chain transfer agent (potassium formate) into the mixed solution under the protection of nitrogen to perform copolymerization reaction for 2h (wherein the reactor is sealed after the solution is blown to be viscous), and obtaining the modified polyacrylamide papermaking retention and drainage aid in a colloidal state after the reaction is finished.
Example 2
(1) Adding 1 part of melamine and 1 part of deionized water into a three-neck flask provided with a stirrer, a reflux condenser and a thermometer, heating to 50 ℃ for dissolution, slowly adding 3.5 parts of formaldehyde, and carrying out polycondensation reaction at 80 ℃ for 3 hours to obtain a melamine polycondensate;
(2) slowly adding 1 part of p-methylstyrene into 100 parts of melamine polycondensate, and carrying out copolymerization reaction for 1h at 100 ℃ to obtain a modified melamine polycondensate;
(3) slowly adding 1 part of sulfonating agent (sodium bisulfite water solution with solid content of 50%) into 0.5 part of modified melamine polycondensate, and performing sulfonation reaction at 80 ℃ for 1h to obtain sulfonated modified melamine polycondensate;
(4) adding 20 parts of sulfonated modified melamine polycondensate, 150 parts of acrylamide, 100 parts of methacryloyloxyethyl trimethyl ammonium chloride, 20 parts of structure regulator (N, N-methylene bisacrylamide), 5 parts of surfactant (sodium dodecyl benzene sulfonate) and 705 parts of deionized water into a reactor, uniformly mixing to obtain a mixed solution, adjusting the pH value of the mixed solution to 7.0, and adjusting the temperature of the mixed solution to 2 ℃; and then introducing nitrogen into the mixed solution for 30min, adding 0.003 part of initiator (potassium persulfate) and 0.05 part of chain transfer agent (potassium formate) into the mixed solution under the protection of the nitrogen to perform copolymerization reaction for 2h (wherein the reactor is sealed after the solution is blown to be viscous), and obtaining the modified polyacrylamide papermaking retention and filtration aid in a colloidal state after the reaction is finished.
Example 3
(1) Adding 1 part of melamine and 1 part of deionized water into a three-neck flask provided with a stirrer, a reflux condenser and a thermometer, heating to 40 ℃ for dissolution, slowly adding 3.5 parts of formaldehyde, and carrying out polycondensation reaction at 90 ℃ for 1h to obtain a melamine polycondensate;
(2) slowly adding 1 part of p-methylstyrene into 200 parts of melamine polycondensate, and carrying out copolymerization reaction for 1.5h at 100 ℃ to obtain a modified melamine polycondensate;
(3) slowly adding 1 part of sulfonating agent (sodium bisulfite water solution with solid content of 50%) into 0.5 part of modified melamine polycondensate, and carrying out sulfonation reaction at 80 ℃ for 2 hours to obtain sulfonated modified melamine polycondensate;
(4) adding 50 parts of sulfonated modified melamine polycondensate, 150 parts of acrylamide, 100 parts of methacryloyloxyethyl trimethyl ammonium chloride, 20 parts of structure regulator (N, N-methylene bisacrylamide), 15 parts of surfactant (sodium dodecyl benzene sulfonate) and 665 parts of deionized water into a reactor, uniformly mixing to obtain a mixed solution, adjusting the pH value of the mixed solution to 7.5, and adjusting the temperature of the mixed solution to 0 ℃; and then introducing nitrogen into the mixed solution for 30min, adding 0.01 part of initiator (potassium persulfate) and 0.5 part of chain transfer agent (potassium formate) under the protection of nitrogen, carrying out copolymerization reaction for 1.5h (wherein the reactor is sealed after the solution is blown to be viscous), and obtaining the modified polyacrylamide papermaking retention and drainage aid in a colloidal state after the reaction is finished.
Example 4
(1) Adding 1 part of melamine and 1 part of deionized water into a three-neck flask provided with a stirrer, a reflux condenser and a thermometer, heating to 60 ℃ for dissolution, slowly adding 3.3 parts of formaldehyde, and carrying out polycondensation reaction at 80 ℃ for 2 hours to obtain a melamine polycondensate;
(2) slowly adding 1 part of p-methylstyrene into 100 parts of melamine polycondensate, and carrying out copolymerization reaction for 1.5h at 100 ℃ to obtain a modified melamine polycondensate;
(3) slowly adding 1 part of sulfonating agent (sodium bisulfite water solution with solid content of 50%) into 0.75 part of modified melamine polycondensate, and performing sulfonation reaction for 2 hours at 100 ℃ to obtain sulfonated modified melamine polycondensate;
(4) adding 30 parts of sulfonated modified melamine polycondensate, 200 parts of acrylamide, 100 parts of methacryloyloxyethyl trimethyl ammonium chloride, 30 parts of structure regulator (N, N-methylene bisacrylamide), 10 parts of surfactant (sodium dodecyl benzene sulfonate) and 630 parts of deionized water into a reactor, uniformly mixing to obtain a mixed solution, adjusting the pH value of the mixed solution to 7.0, and adjusting the temperature of the mixed solution to 5 ℃; and then introducing nitrogen into the mixed solution for 30min, adding 0.02 part of initiator (potassium persulfate) and 0.05 part of chain transfer agent (potassium formate) into the mixed solution under the protection of the nitrogen to perform copolymerization reaction for 2h (wherein the reactor is sealed after the solution is blown to be viscous), and obtaining the modified polyacrylamide papermaking retention and drainage aid in a colloidal state after the reaction is finished.
Example 5
(1) Adding 1 part of melamine and 1 part of deionized water into a three-neck flask provided with a stirrer, a reflux condenser and a thermometer, heating to 50 ℃ to dissolve, slowly adding 3 parts of paraformaldehyde, and carrying out polycondensation reaction at 80 ℃ for 3 hours to obtain a melamine polycondensate;
(2) slowly adding 1 part of p-methylstyrene into 500 parts of melamine polycondensate, and carrying out copolymerization reaction for 2h at 100 ℃ to obtain a modified melamine polycondensate;
(3) slowly adding 1 part of sulfonating agent (sodium bisulfite water solution with solid content of 50%) into 0.75 part of modified melamine polycondensate, and performing sulfonation reaction at 100 ℃ for 1h to obtain sulfonated modified melamine polycondensate;
(4) adding 50 parts of sulfonated modified melamine polycondensate, 180 parts of acrylamide, 100 parts of methacryloyloxyethyl trimethyl ammonium chloride, 30 parts of structure regulator (N, N-methylene bisacrylamide), 10 parts of surfactant (sodium dodecyl benzene sulfonate) and 630 parts of deionized water into a reactor, uniformly mixing to obtain a mixed solution, adjusting the pH value of the mixed solution to 7.0, and adjusting the temperature of the mixed solution to 5 ℃; and then introducing nitrogen into the mixed solution for 30min, adding 0.002 part of initiator (potassium persulfate) and 0.05 part of chain transfer agent (potassium formate) into the mixed solution under the protection of nitrogen, carrying out copolymerization reaction for 2h (wherein the reactor is sealed after the solution is blown to be viscous), and obtaining the modified polyacrylamide papermaking retention and filtration aid in a colloidal state after the reaction is finished.
Example 6
(1) Adding 1 part of melamine and 1 part of deionized water into a three-neck flask provided with a stirrer, a reflux condenser and a thermometer, heating to 60 ℃ for dissolution, slowly adding 3.5 parts of formaldehyde, and carrying out polycondensation reaction at 80 ℃ for 2 hours to obtain a melamine polycondensate;
(2) slowly adding 1 part of p-methylstyrene into 100 parts of melamine polycondensate, and carrying out copolymerization reaction for 0.5h at 100 ℃ to obtain a modified melamine polycondensate;
(3) slowly adding 1 part of sulfonating agent (sodium bisulfite water solution with solid content of 50%) into 0.75 part of modified melamine polycondensate, and performing sulfonation reaction for 3 hours at 100 ℃ to obtain sulfonated modified melamine polycondensate;
(4) adding 20 parts of sulfonated modified melamine polycondensate, 200 parts of acrylamide, 80 parts of methacryloyloxyethyl trimethyl ammonium chloride, 20 parts of structure regulator (N, N-methylene bisacrylamide), 10 parts of surfactant (sodium dodecyl benzene sulfonate) and 670 parts of deionized water into a reactor, uniformly mixing to obtain a mixed solution, adjusting the pH value of the mixed solution to 7.0, and adjusting the temperature of the mixed solution to 0 ℃; and then introducing nitrogen into the mixed solution for 30min, adding 0.02 part of initiator (potassium persulfate) and 0.005 part of chain transfer agent (potassium formate) into the mixed solution under the protection of the nitrogen to perform copolymerization reaction for 2.5h (wherein the reactor is sealed after the solution is blown to be viscous), and obtaining the modified polyacrylamide papermaking retention and drainage aid in a colloidal state after the reaction is finished.
Example 7
Example 7 is essentially the same as example 1, except that: in the step (2), 1 part of p-methylstyrene is slowly added to 10 parts of the melamine polycondensate, and copolymerization is carried out at 70 ℃ for 2 hours to obtain the modified melamine polycondensate.
Example 8
Example 8 is essentially the same as example 1, except that: in step (2), 1 part of p-methylstyrene is slowly added to 1000 parts of the melamine polycondensate.
Example 9
Example 9 is essentially the same as example 1 except that: in the step (4), 5 parts of sulfonated modified melamine polycondensate, 180 parts of acrylamide, 80 parts of methacryloyloxyethyl trimethyl ammonium chloride, 30 parts of structure regulator (N, N-methylene bisacrylamide), 5 parts of surfactant (sodium dodecyl sulfate) and 700 parts of deionized water are added into a reactor and uniformly mixed to obtain a mixed solution, the pH value of the mixed solution is adjusted to 7.0, and the temperature of the mixed solution is adjusted to 0 ℃; and then introducing nitrogen into the mixed solution for 30min, adding 0.005 part of initiator (sodium persulfate) and 0.03 part of chain transfer agent (thioglycolic acid) into the mixed solution under the protection of the nitrogen to perform copolymerization reaction for 2h (wherein the reactor is sealed after the solution is blown to be viscous), and obtaining the modified polyacrylamide papermaking retention and drainage aid in a colloidal state after the reaction is finished.
Comparative example 1
The general polyacrylamide which is purchased from Taian Xin spring chemical engineering and used as a papermaking retention and drainage aid has a cationic type and a molecular weight of 800-1000 w.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that: step (3) was not included, i.e., step (4) used 10 parts of the modified melamine polycondensate.
Comparative example 3
Comparative example 3 is substantially the same as example 1 except that: instead of adding 30 parts of deionized water, no 30 parts of structure regulator were added, i.e., a total of 725 parts of deionized water.
Comparative example 4
Comparative example 4 is substantially the same as example 1 except that: 3 parts of sulfonated modified melamine polycondensate and 702 parts of deionized water are added, and the use amount of other raw materials is unchanged.
The modified polyacrylamide papermaking retention and drainage aids obtained in examples 1 to 9 and the polyacrylamides obtained in comparative examples 1 to 4 were dried and ground to obtain samples, and the samples were placed in water to test the dissolution time and the retention, the white water turbidity and the white water viscosity retention, and the test data are shown in tables 1 and 2.
Specifically, the retention of the fines is determined with reference to the determination standard tappi 261CM-94, specifically: respectively adding the samples into 100mL of experimental slurry (the water quality pH of the experimental slurry is 7.0-7.2, the turbidity is 162 NTU), controlling the addition amount of the samples in the experimental slurry to be 1500ppm, then filtering by using filter paper, drying the obtained product at 120 ℃ for 60min, measuring the dried mass, and calculating the retention rate;
testing the turbidity of the white water by using a turbidity measurement analyzer;
the test data in table 2 are measured for white water after 3 cycles.
As can be seen from Table 1, the dissolution time of the modified polyacrylamide colloid powder prepared in the embodiment of the present invention in water is not more than 30 min. Meanwhile, through comparative examples and comparative examples, the inventors found that the sulfonated modified melamine polycondensate significantly improves the retention of the prepared modified polyacrylamide on fine fibers as a papermaking retention and drainage aid and also reduces the white water turbidity.
TABLE 2
It should be noted that the content of inorganic salts in the white water after 3 cycles is increased, and therefore, as can be seen from table 2, compared with the comparative example, the modified polyacrylamide colloid powder prepared in the embodiment of the present invention has a retention rate of white water viscosity of more than 90% at 50 ℃ and 80 ℃ after 3 cycles, and thus the modified polyacrylamide has excellent temperature resistance and salt tolerance.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. The preparation method of the modified polyacrylamide papermaking retention and drainage aid is characterized by comprising the following steps:
(1) carrying out polycondensation reaction on melamine and aldehyde compounds to obtain a melamine polycondensate; the mass ratio of the melamine to the aldehyde compound is 1 (3-3.5);
(2) carrying out copolymerization reaction on the melamine polycondensate and p-methylstyrene to obtain a modified melamine polycondensate; the mass ratio of the p-methylstyrene to the melamine polycondensate is 1 (10-1000);
(3) carrying out sulfonation reaction on the modified melamine polycondensate and a sulfonating agent to obtain a sulfonated modified melamine polycondensate;
(4) adding the sulfonated modified melamine polycondensate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride, a structure regulator, a surfactant, a chain transfer agent, deionized water and an initiator into a reactor to carry out copolymerization reaction to obtain the modified polyacrylamide papermaking retention and drainage aid; the structure regulator is N, N-methylene bisacrylamide;
the modified polyacrylamide papermaking retention and drainage aid is prepared from the following raw materials in parts by weight: 5-50 parts of sulfonated modified melamine polycondensate, 150-200 parts of acrylamide, 80-100 parts of methacryloyloxyethyl trimethyl ammonium chloride, 20-50 parts of structure regulator, 1-15 parts of surfactant, 300-800 parts of deionized water, 0.01-1 part of chain transfer agent and 0.001-1 part of initiator.
2. The production method according to claim 1, wherein in step (1):
the aldehyde compound is at least one of formaldehyde and paraformaldehyde;
and/or
The polycondensation reaction is carried out for 1-3 h at the temperature of 60-90 ℃.
3. The method of claim 1, wherein:
the step (1) comprises the following steps:
putting the melamine into deionized water, uniformly stirring, and then adding the aldehyde compound to perform polycondensation reaction;
wherein the temperature for uniformly stirring is 40-60 ℃; the mass ratio of the melamine to the deionized water is 1 (1-2).
4. The production method according to claim 1, wherein in step (2):
the copolymerization reaction is carried out for 0.5-2 h at 70-100 ℃.
5. The production method according to claim 1, wherein in step (3):
the sulfonating agent is at least one of sodium sulfite and sodium bisulfite;
the mass ratio of the modified melamine polycondensate to the sulfonating agent is 1 (1-1.5); and/or
The sulfonation reaction is carried out for 1-3 h at 80-100 ℃.
6. The production method according to claim 1, wherein in step (4):
the surfactant is at least one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate;
and/or the presence of a gas in the atmosphere,
the initiator is persulfate; the persulfate is potassium persulfate, sodium persulfate, ammonium persulfate, calcium persulfate, potassium hydrogen persulfate, sodium hydrogen persulfate, ammonium hydrogen persulfate or calcium hydrogen persulfate;
the chain transfer agent is formate and thioglycollic acid; the formate is at least one of ammonium formate, sodium formate and potassium formate.
7. The method of claim 1, wherein:
the step (4) comprises the following steps:
adding the sulfonated modified melamine polycondensate, acrylamide, methacryloyloxyethyl trimethyl ammonium chloride, the structure regulator, the surfactant and deionized water into a reactor, uniformly mixing to obtain a mixed solution, introducing nitrogen into the mixed solution, and then adding the initiator and the chain transfer agent to perform copolymerization reaction to obtain the modified polyacrylamide papermaking retention and drainage aid.
8. The method of claim 7, wherein:
in the step (4), after the mixed solution is obtained, the method further comprises the following steps:
adjusting the pH value of the mixed solution to 7-7.5;
adjusting the temperature of the mixed solution to 0-5 ℃; and/or
In the step (4), introducing nitrogen for 30-40 min;
the reaction time of the copolymerization reaction is 1.5-2.5 h.
9. A modified polyacrylamide papermaking retention and drainage aid characterized in that it is prepared by the process according to any one of claims 1 to 8.
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