CN112979871A - Synthesis method of anti-degradation cationic polyacrylamide - Google Patents
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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Abstract
The invention belongs to the technical field of polyacrylamide, and particularly relates to a method for synthesizing anti-degradation cationic polyacrylamide, which comprises the steps of adding an inorganic salt auxiliary agent, acrylamide and acryloyloxyethyl trimethyl ammonium chloride into deionized water according to the mass percentage of dry matters to be dissolved and mixed, thus obtaining a material solution with a certain mass concentration, pumping the solution into a polymerization kettle, introducing nitrogen for 40min, adding a composite initiator, continuously introducing nitrogen for 3min, thickening the feed liquid, carrying out pressure-holding polymerization for 3h, granulating, drying, grinding and the like on colloid to obtain a granular product, wherein the granular product is the anti-degradation cationic polyacrylamide. The invention adopts a composite initiation system and free radical aqueous solution polymerization to improve the viscosity and the charge binding force of the product and improve the degradation resistance of the product; the product yield is improved, the yield and the quality are improved, the production cost and the use cost are reduced, and the cost performance is higher.
Description
Technical Field
The invention belongs to the technical field of polyacrylamide, and particularly relates to a synthetic method of anti-degradation cationic polyacrylamide.
Background
The acyloxy group (ester group) in the macromolecular structure of the cationic Polyacrylamide (PAM) has the tendency of being easily hydrolyzed into carboxyl and hydroxyl, a calcium-magnesium ion solution in tap water is weak in alkalinity, the hydrolysis is promoted, and the hydrolyzed carboxylate is an anion and forms flocculation with a cationic group to whiten the solution and reduce the viscosity.
The general degradation reason of the cationic polyacrylamide is caused by too long dissolving and standing time after dilution preparation, the cationic polyacrylamide is dissolved and used along with the preparation, and the dissolution solution begins to degrade after being placed for 8 hours. The factors influencing the degradation of the cationic polyacrylamide solution mainly include three factors: 1. the solution is contacted with iron metal for a long time, because ions generated by the contact of iron with oxygen and moisture can directly influence amide groups in polyacrylamide, molecular branched chains cannot be completely stretched after the solution is dissolved, and natural degradation is caused; 2. after the solution is exposed to sunlight, ultraviolet rays in the sunlight can also cause the degradation of products, the breakage and hydrolysis of molecular chains, the storage requirement of common solid PAM is to store in a well-ventilated warehouse and avoid the humidity and the sunlight exposure, and a sealing cover is added if the PAM solution is not used up after the PAM solution is prepared, so that the natural degradation caused by direct sunlight is avoided; 3. the influence of the aqueous solution and the environmental temperature on the solution, the temperature higher than 40 ℃ is easy to promote the molecular chain of the product to be broken, the viscosity of the product is reduced, and the flocculation effect is influenced.
The degradation of the cationic polyacrylamide is aggravated by combining the three factors, and the flocculation effect of the product is seriously influenced and even completely lost.
Disclosure of Invention
The invention aims to provide a method for synthesizing anti-degradation cationic polyacrylamide with high viscosity, good anti-degradation and flocculation effects and small using amount.
The technical scheme adopted by the invention for solving the technical problems is as follows: a synthetic method of degradation-resistant cationic polyacrylamide comprises the following steps: adding an inorganic salt auxiliary agent, acrylamide and acryloyloxyethyl trimethyl ammonium chloride into deionized water according to the mass percentage of dry matters to be dissolved and mixed so as to obtain a material solution with a certain mass concentration, pumping the solution into a polymerization kettle, introducing nitrogen for 40min, adding a composite initiator, continuously introducing nitrogen for 3min, thickening the feed liquid, carrying out pressure-holding polymerization for 3h, and carrying out granulation, drying, grinding and other processes on colloid to obtain a granular product, wherein the granular product is the anti-degradation cationic polyacrylamide.
Further, the mass percent of the inorganic salt auxiliary agent is 3-5wt%, the mass percent of the acrylamide is 5-92 wt%, and the mass percent of the acryloyloxyethyl trimethyl ammonium chloride is 3-92 wt%.
Further, the inorganic salt auxiliary agent is an inorganic aluminum salt.
Further, the inorganic salt auxiliary agent is aluminum chloride.
Further, the mass concentration of the material solution is 28-40%.
Further, the composite initiator is a composite initiation system consisting of an azo initiator and a redox initiator.
Further, the composite initiator takes potassium persulfate as an oxidizing agent, sodium sulfite as a reducing agent, azodiisobutyronitrile as an azo initiator, and a shielding agent EDTA-2Na and a molecular weight regulator sodium formate are also required to be added.
Further, the addition amount of the composite initiator is as follows: the dosage of the potassium persulfate is 12-90 mg/L, the dosage of the sodium sulfite is 20-180 mg/L, the dosage of the azo initiator is 5-18mg/L, the dosage of the EDTA-2Na is 30-400mg/L, and the dosage of the sodium formate is 300-800 mg/L.
The principle of the synthesis method of the degradation-resistant cationic polyacrylamide is as follows: adding a certain amount of inorganic salt auxiliary agent into the mixed solution of Acrylamide (AM) and acryloyloxyethyl trimethyl ammonium chloride (DAC) to carry out polymerization of a composite initiator to produce the novel anti-degradation cationic polyacrylamide. As the product is a linear high molecular polymer, the product polymerization meets the general rule of free radical chain polymerization reaction and is initiated by chain, extended by chain, terminated by chain or transferred by chain. In the process of binary polymerization or multi-polymerization, the structure of the generated polymer depends on chain growth reaction, and the performance of the product is greatly influenced. The product has the advantages that the temperature resistance and the salt resistance of the product are improved, the degradation resistance of the product is improved, a larger group is required to be added from a branched chain structure of a linear main chain of the product, so that the steric hindrance and the charge constraint force of the product are improved, meanwhile, a certain charge density is generated by small molecular charges locally concentrated on the branched chain, so that the viscosity of the product is improved, the charges are compensated, the application reaction speed of the product is improved, the attacking force of the small molecules on sewage colloid and colloidal particles is stronger, the treatment effect of the same product is finally improved, and the product dosage is reduced.
The novel anti-degradation cationic polyacrylamide is mainly used in the field of water treatment, and the using method comprises the following steps: the degradation-resistant cationic polyacrylamide is dissolved in tap water according to the mass concentration of 0.1-0.2% to form a product solution, the product solution is fully mixed with sewage to react, the charge neutralization and adsorption bridging mechanism is taken as a leading factor, and the flocculation reaction is carried out through the intramolecular and intermolecular action to enable particles and colloidal particles in the sewage to float or sink in a layered manner, so that the solid-liquid separation is realized to enable the sewage to be clear. When the water is required to be dissolved, the water is fully stirred and then the medicinal powder is slowly and uniformly added, so that the phenomena of large flocs and fish eyes are prevented from blocking pipelines and pumps; the stirring speed is generally 200 revolutions per minute, and the time is not less than 60 minutes; a small amount of product is added to achieve a great flocculation effect, and generally only 0.01-10 ppm (0.01-10 g/m) of product is added3) Thus, the function can be fully exerted.
The invention has the following beneficial effects: the novel anti-degradation cationic polyacrylamide disclosed by the invention is reasonable in structure and clear in principle, the preparation meets the requirements of the process and equipment, the viscosity and the charge binding force of the product can be effectively improved, and the anti-degradation performance of the product is improved; under the condition of complete dissolution, the addition of the inorganic salt auxiliary agent is improved, and the degradation resistance is better. Under the condition of similar products, the dosage of the same application effect is less, and the application effect of the same dosage is better. The product has high viscosity, smooth and non-stick surface, convenient subsequent granulation and drying, small amount of generated fine powder, improved product yield, improved yield and quality, reduced production cost and use cost, and higher cost performance.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the scope of the present invention is not limited to these examples. All changes, modifications and equivalents that do not depart from the spirit of the invention are intended to be included within the scope thereof.
Example 1
20% cationicity product: adding deionized water into a clean beaker, sequentially adding 3wt% of inorganic aluminum salt auxiliary agent, 5wt% of acrylamide and 92wt% of acryloyloxyethyl trimethyl ammonium chloride according to the mass percentage of dry matters, dissolving and mixing to obtain a material solution with the mass concentration of 30%, uniformly stirring, dissolving, cooling, pouring all the materials into a polymerization container, introducing nitrogen for 40min to remove oxygen, adding a composite initiator consisting of an azo initiator and a redox initiator after the materials are fully removed with oxygen, wherein the adding amount of the composite initiator is specifically as follows: the using amount of potassium persulfate is 60mg/L, the using amount of sodium sulfite is 100mg/L, the using amount of azo initiator is 10mg/L, the using amount of EDTA-2Na is 200mg/L, the using amount of sodium formate is 500mg/L, oxygen is continuously removed until the material liquid is thickened, the pressure is held for polymerization for 3 hours, pressurization and smooth discharging are carried out after the polymerization is finished, colloid granulation, drying, grinding and packaging are carried out, and the product index meets the design requirement and is improved. Specific product indexes and anti-degradation indexes are as follows: the product has a molecular weight of 1310 ten thousand and excellent solubility, the initial viscosity of the product is 12.6mPa & s, the viscosity of the product is 11.5mPa & s after 24 hours in a 42 ℃ environment, and the viscosity retention rate is 91.26%.
Example 2
40% cationicity product: adding deionized water into a clean beaker, sequentially adding 5wt% of inorganic aluminum salt auxiliary agent, 30wt% of acrylamide and 65wt% of acryloyloxyethyl trimethyl ammonium chloride according to the mass percentage of dry matters, dissolving and mixing to obtain a material solution with the mass concentration of 40%, uniformly stirring, dissolving, cooling, pouring all the materials into a polymerization container, introducing nitrogen for 40min to remove oxygen, adding a composite initiator consisting of an azo initiator and a redox initiator after the materials are fully removed with oxygen, wherein the adding amount of the composite initiator is specifically as follows: the using amount of potassium persulfate is 90mg/L, the using amount of sodium sulfite is 180mg/L, the using amount of azo initiator is 15mg/L, the using amount of EDTA-2Na is 300mg/L, the using amount of sodium formate is 300mg/L, oxygen is continuously removed until the material liquid is thickened, the pressure is held for polymerization for 3 hours, pressurization and smooth discharging are carried out after the polymerization is finished, colloid granulation, drying, grinding and packaging are carried out, and the product index meets the design requirement and is improved. Specific product indexes and anti-degradation indexes are as follows: the product has the molecular weight of 1257 ten thousand and excellent solubility, the initial viscosity of the product is 16.3mPa & s, the viscosity of the product is 14.7mPa & s after 24 hours in 42 ℃, and the viscosity retention rate is 90.18%.
Example 3
50% cationicity product: adding deionized water into a clean beaker, sequentially adding 5wt% of inorganic aluminum salt auxiliary agent, 92wt% of acrylamide and 3wt% of acryloyloxyethyl trimethyl ammonium chloride according to the mass percentage of dry matters, dissolving and mixing to obtain a material solution with the mass concentration of 28%, uniformly stirring, dissolving, cooling, pouring all the materials into a polymerization container, introducing nitrogen for 40min to remove oxygen, adding a composite initiator consisting of an azo initiator and a redox initiator after the materials are fully removed with oxygen, wherein the adding amount of the composite initiator is specifically as follows: the using amount of potassium persulfate is 12mg/L, the using amount of sodium sulfite is 20mg/L, the using amount of azo initiator is 18mg/L, the using amount of EDTA-2Na is 30mg/L, the using amount of sodium formate is 800mg/L, oxygen is continuously removed until the material liquid is thickened, the pressure is held for polymerization for 3 hours, pressurization and smooth discharging are carried out after the polymerization is finished, colloid granulation, drying, grinding and packaging are carried out, and the product index meets the design requirement and is improved. Specific product indexes and anti-degradation indexes are as follows: the product has a molecular weight of 1150 ten thousand and excellent solubility, the initial viscosity of the product is 17.8mPa & s, the viscosity of the product is 16.1mPa & s after 24 hours in a 42 ℃ environment, and the viscosity retention rate is 90.44%.
Example 4
20% cationicity product: adding deionized water into a clean beaker, sequentially adding 4wt% of inorganic aluminum salt auxiliary agent, 40wt% of acrylamide and 56wt% of acryloyloxyethyl trimethyl ammonium chloride according to the mass percentage of dry matters, dissolving and mixing to obtain a material solution with the mass concentration of 35%, uniformly stirring, dissolving, cooling, pouring all the materials into a polymerization container, introducing nitrogen for 40min to remove oxygen, adding a composite initiator consisting of an azo initiator and a redox initiator after the materials are fully removed with oxygen, wherein the adding amount of the composite initiator is specifically as follows: the using amount of potassium persulfate is 55mg/L, the using amount of sodium sulfite is 80mg/L, the using amount of azo initiator is 5mg/L, the using amount of EDTA-2Na is 400mg/L, the using amount of sodium formate is 400mg/L, oxygen is continuously removed until the material liquid is thickened, the pressure is held for polymerization for 3 hours, pressurization and smooth discharging are carried out after the polymerization is finished, colloid granulation, drying, grinding and packaging are carried out, and the product index meets the design requirement and is improved. Specific product indexes and anti-degradation indexes are as follows: the product has the molecular weight of 1232 ten thousand and excellent solubility, the initial viscosity of the product is 11.8mPa & s, the viscosity of the product is 11.2mPa & s after 24 hours in a 42 ℃ environment, and the viscosity retention rate is 94.91%.
Example 5
50% cationicity product: adding deionized water into a clean beaker, sequentially adding 5wt% of inorganic aluminum salt auxiliary agent, 80wt% of acrylamide and 15wt% of acryloyloxyethyl trimethyl ammonium chloride according to the mass percentage of dry matters, dissolving and mixing to obtain a material solution with the mass concentration of 38%, uniformly stirring, dissolving, cooling, pouring all the materials into a polymerization container, introducing nitrogen for 40min to remove oxygen, adding a composite initiator consisting of an azo initiator and a redox initiator after the materials are fully removed with oxygen, wherein the adding amount of the composite initiator is specifically as follows: the using amount of potassium persulfate is 70mg/L, the using amount of sodium sulfite is 150mg/L, the using amount of azo initiator is 14mg/L, the using amount of EDTA-2Na is 150mg/L, the using amount of sodium formate is 600mg/L, oxygen is continuously removed until the material liquid is thickened, the pressure is held for polymerization for 3 hours, pressurization and smooth discharging are carried out after the polymerization is finished, colloid granulation, drying, grinding and packaging are carried out, and the product index meets the design requirement and is improved. Specific product indexes and anti-degradation indexes are as follows: the product has a molecular weight of 1075 thousands, excellent solubility, an initial viscosity of 16.5mPa & s, a viscosity of 15.1mPa & s after 24 hours in a 42 ℃ environment, and a viscosity retention rate of 91.51%.
Comparative example 1
20% cationicity product: adding deionized water into a clean beaker, sequentially adding 8wt% of acrylamide and 92wt% of acryloyloxyethyl trimethyl ammonium chloride according to the mass percentage of dry substances, dissolving and mixing to obtain a material solution with the mass concentration of 30%, uniformly stirring, dissolving, cooling, pouring all the materials into a polymerization container, introducing nitrogen for 40min to remove oxygen, adding a composite initiator consisting of an azo initiator and a redox initiator after the materials are fully deoxygenated, wherein the adding amount of the composite initiator specifically comprises the following steps: the using amount of potassium persulfate is 60mg/L, the using amount of sodium sulfite is 100mg/L, the using amount of azo initiator is 10mg/L, the using amount of EDTA-2Na is 200mg/L, the using amount of sodium formate is 500mg/L, continue deoxidization until the feed liquid thickens, build pressure and polymerize for 3h, pressurize and smoothly unload after polymerization is completed, colloid granulation, drying, grinding and packaging, specific product indexes and anti-degradation indexes: the product has a molecular weight of 1285 ten thousand and excellent solubility, the initial viscosity of the product is 12.8mPa & s, the viscosity of the product is 9.6mPa & s after 24 hours in a 42 ℃ environment, and the viscosity retention rate is 75.00 percent.
Comparative example 2
40% cationicity product: adding deionized water into a clean beaker, sequentially adding 35wt% of acrylamide and 65wt% of acryloyloxyethyl trimethyl ammonium chloride according to the mass percentage of dry substances, dissolving and mixing to obtain a material solution with the mass concentration of 40%, uniformly stirring, dissolving, cooling, pouring all the materials into a polymerization container, introducing nitrogen for 40min to remove oxygen, adding a composite initiator consisting of an azo initiator and a redox initiator after the oxygen is fully removed, wherein the adding amount of the composite initiator is specifically as follows: the using amount of potassium persulfate is 90mg/L, the using amount of sodium sulfite is 180mg/L, the using amount of azo initiator is 15mg/L, the using amount of EDTA-2Na is 300mg/L, the using amount of sodium formate is 300mg/L, continue deoxidization until the feed liquid thickens and then build pressure and polymerize for 3h, pressurize and smoothly unload after polymerization is completed, colloid granulation, drying, grinding and packaging, specific product indexes and anti-degradation indexes: the product has the molecular weight of 1211 ten thousand and excellent solubility, the initial viscosity of the product is 15.8mPa & s, the viscosity of the product is 9.9mPa & s after 24 hours in a 42 ℃ environment, and the viscosity retention rate is 62.65%.
Comparative example 3
50% cationicity product: adding deionized water into a clean beaker, sequentially adding 80wt% of acrylamide and 20wt% of acryloyloxyethyl trimethyl ammonium chloride according to the mass percentage of dry substances, dissolving and mixing to obtain a material solution with the mass concentration of 38%, uniformly stirring, dissolving, cooling, pouring all the materials into a polymerization container, introducing nitrogen for 40min to remove oxygen, adding a composite initiator consisting of an azo initiator and a redox initiator after the oxygen is fully removed, wherein the adding amount of the composite initiator is specifically as follows: the using amount of potassium persulfate is 70mg/L, the using amount of sodium sulfite is 150mg/L, the using amount of azo initiator is 14mg/L, the using amount of EDTA-2Na is 150mg/L, the using amount of sodium formate is 600mg/L, continue deoxidization until the feed liquid thickens, build pressure and polymerize for 3h, pressurize and smoothly unload after polymerization is completed, colloid granulation, drying, grinding and packaging, specific product indexes and anti-degradation indexes: the product has the advantages of molecular weight 1217 ten thousand and excellent solubility, the initial viscosity of the product is 17.8 mPa.s, the viscosity of the product is 9.2 mPa.s after 24h in 42 ℃, and the viscosity retention rate is 51.68%.
Claims (6)
1. The method for synthesizing the degradation-resistant cationic polyacrylamide is characterized by comprising the following steps of: adding an inorganic salt auxiliary agent, acrylamide and acryloyloxyethyl trimethyl ammonium chloride into deionized water according to the mass percent of dry matters to be dissolved and mixed so as to obtain a material solution with a certain mass concentration, pumping the solution into a polymerization kettle, introducing nitrogen for 40min, adding a composite initiator, continuously introducing nitrogen for 3min, thickening the feed liquid, carrying out pressure-holding polymerization for 3h, and carrying out granulation, drying and grinding on colloid to obtain a granular product, wherein the granular product is the anti-degradation cationic polyacrylamide;
the composite initiator is a composite initiation system consisting of an azo initiator and a redox initiator, wherein the composite initiator takes potassium persulfate as an oxidant, sodium sulfite as a reducing agent, azodiisobutyronitrile as the azo initiator, and a shielding agent EDTA-2Na and a molecular weight regulator sodium formate are also required to be added.
2. The method for synthesizing the degradation-resistant cationic polyacrylamide of claim 1, wherein the mass percent of the inorganic salt auxiliary agent is 3-5wt%, the mass percent of the acrylamide is 5-92 wt%, and the mass percent of the acryloyloxyethyl trimethyl ammonium chloride is 3-92 wt%.
3. The method for synthesizing degradation-resistant cationic polyacrylamide according to claim 1, wherein the inorganic salt assistant is an inorganic aluminum salt.
4. The method for synthesizing degradation-resistant cationic polyacrylamide of claim 3 wherein said inorganic salt promoter is aluminum chloride.
5. The method for synthesizing degradation-resistant cationic polyacrylamide according to claim 1, wherein the mass concentration of the material solution is 28-40%.
6. The method for synthesizing degradation-resistant cationic polyacrylamide according to claim 1, wherein the addition amount of the composite initiator is as follows: the dosage of the potassium persulfate is 12-90 mg/L, the dosage of the sodium sulfite is 20-180 mg/L, the dosage of the azo initiator is 5-18mg/L, the dosage of the EDTA-2Na is 30-400mg/L, and the dosage of the sodium formate is 300-800 mg/L.
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| CN116854223A (en) * | 2023-09-04 | 2023-10-10 | 杭州尚善若水环保科技有限公司 | Combined medicament and process for preventing degradation of cationic polymeric flocculant after dissolution |
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