CN112480310A - Cross-linked cationic polyacrylamide sludge dehydrating agent and preparation method thereof - Google Patents
Cross-linked cationic polyacrylamide sludge dehydrating agent and preparation method thereof Download PDFInfo
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- CN112480310A CN112480310A CN202011421171.3A CN202011421171A CN112480310A CN 112480310 A CN112480310 A CN 112480310A CN 202011421171 A CN202011421171 A CN 202011421171A CN 112480310 A CN112480310 A CN 112480310A
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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
- 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
- C02F11/147—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents using organic substances
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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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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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
- 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
Abstract
The invention relates to a cross-linking type cationic polyacrylamide sludge dehydrating agent, which comprises the following components: deionized water, acrylamide, acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, ammonium sulfate, adipic acid, a coagent, a chelating agent, an azo initiator, a crosslinking agent, a chain transfer agent, an oxidant and a reducing agent. Mixing and stirring deionized water, acrylamide, acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, N-2, 2-propenyl-2-acrylamide, ammonium sulfate, adipic acid, an active assistant and other auxiliary cross-linking agents, and adjusting the pH value of the solution; cooling, introducing nitrogen and discharging oxygen, adding an azo initiator, a chelating agent, a chain transfer agent, an oxidant and a reducing agent, and closing a nitrogen introducing valve after reaction initiation to obtain a flocculant colloid; and (4) crushing the colloid, drying at high temperature and sieving to obtain flocculant powder. The dehydrating agent is safe and environment-friendly, and can effectively improve the dehydrating effect of sewage.
Description
Technical Field
The invention belongs to the technical field of flocculant preparation, and particularly relates to a cross-linked cationic polyacrylamide sludge dehydrating agent and a preparation method thereof.
Background
The sludge is a byproduct generated in the sewage treatment process, contains a large amount of pathogenic bacteria, heavy metals and refractory organics, and has the characteristics of small sludge particles, poor settling property, high water content and the like. If the treatment is improper, serious secondary pollution can be caused to water sources and the atmosphere, and the environment is damaged for a long time and is difficult to repair. The institutional research shows that the estimated 2020 year can reach about 6500 million tons of sludge in China. According to the requirements of "notice on strengthening sludge pollution control work in urban sewage treatment plants", sludge is transported from factories by sewage treatment plants for storage, and the sludge must be dewatered to a water content of 50% or less. At present, the water content of the sludge of the urban sewage plant is more than 90 percent, and the water content is still more than 80 percent after the sludge is treated by a concentration or mechanical dehydration process, and obviously the water content of the sludge does not meet the requirements of resource utilization and disposal.
Currently, sludge dewatering conditioners fall into two categories: one is inorganic flocculant mainly comprising ferric salt, aluminum salt and polyaluminium chloride, and the other is organic polymeric flocculant comprising nonionic, cationic, anionic and amphoteric organic polymeric agents, most commonly Polyacrylamide (PAM). Patent CN1769221A discloses a cationic sludge dehydrating agent, which uses many organic play components such as formaldehyde and organic amine, and is not friendly to human and environment, and the sludge treatment effect is not obvious. Patent CN104261651A discloses a modified cationic polyacrylamide sewage treatment agent, which has a dehydration rate of about 70% although the dehydration effect is better than that of the traditional polyacrylamide dehydrating agent. Patent CN101172748A discloses a composite sludge dehydrating agent, which can only control the dehydration rate to about 72% when being used after being compounded with other patent products, and the process is relatively complicated; the ionic dispersants used in the sludge dewatering agent disclosed in patent CN101100345A are up to 5, and the filtrate causes secondary pollution. In addition, although the literature 'test of graft copolymerization and flocculation property of acrylamide and D-fructose acrylamide derivatives' mentions that crosslinking agents such as MBA can be used, the grafting rate is low during grafting, and it is difficult to achieve the desired application effect.
Disclosure of Invention
Aiming at the defects, the invention provides the crosslinking type cationic polyacrylamide sludge dehydrating agent which is convenient to use, safe and environment-friendly and can effectively improve the sewage dehydrating effect and the preparation method thereof.
The technical scheme adopted by the invention is as follows: the cross-linking type cationic polyacrylamide sludge dehydrating agent is characterized by being prepared from the following components in parts by weight: 30-80 parts of deionized water; 10-60 parts of acrylamide; 30-80 parts of acryloyloxyethyl trimethyl ammonium chloride; 2-8 parts of methacryloyloxyethyl trimethyl ammonium chloride; 2-6 parts of ammonium sulfate; 1-5 parts of adipic acid; 0.001-0.1 part of active auxiliary agent ZINC; 0.005-0.1 part of chelating agent; 0.01-0.5 part of azo initiator; 0.002-8 parts of a cross-linking agent; 0.001-0.035 parts of a chain transfer agent; 0.001-0.08 part of an oxidant; 0.001-0.05 part of reducing agent.
The chelating agent is one or two of diethylenetriamine pentaacetic acid pentasodium (Versenex 80) and Ethylene Diamine Tetraacetic Acid (EDTA).
The azo initiator is azo, such as one or more of Azobisisobutyronitrile (AZDN), azobisisobutylimidazoline hydrochloride (VA044), azobisisobutylamidine hydrochloride (V50), azobisisopropylimidazoline (VA061) and azobiscyanovaleric acid (ACVA).
The cross-linking agent is one or two of N-2, 2-propenyl-2-acrylamide, Triallylamine (TAA), N, N, N ', N' -Tetraallylethylenediamine (TAEDA), Tetraallyloxyethane (TAE), pentaerythritol triacrylate (PETA) and tetraallylammonium chloride (TAAC). Preferably, N-2, 2-propenyl-2-acrylamide is used as the main crosslinking agent, and others are used as the auxiliary crosslinking agents.
The chain transfer agent is one or two of sodium Hypophosphite (HYPO), sodium formate and amino ethanol.
The oxidant is one or two of Sodium Persulfate (SPS) and potassium persulfate (KPS).
The reducing agent is one or two of sodium Metabisulfite (MBS), Sodium Bisulfite (SBS) and ferrous ammonium sulfate (MS).
A preparation method of a cross-linking type cationic polyacrylamide sludge dehydrating agent comprises the steps of firstly preparing a reaction solution, mixing and stirring deionized water, acrylamide, acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, ammonium sulfate, adipic acid, a coagent ZINC and other auxiliary cross-linking agents until the ammonium sulfate is completely dissolved, and then adding phosphoric acid to adjust the pH value of the whole solution to 3-6; cooling to-5 ℃, injecting into a reaction device, introducing nitrogen, discharging oxygen, adding an azo initiator, a chelating agent, a chain transfer agent, an oxidant and a reducing agent, after reaction initiation, closing a nitrogen introducing valve, reacting for 1-4 hours, and then preserving heat for 1-3 hours to obtain a flocculant colloid; then the colloid is crushed, dried at the high temperature of 60-80 ℃, crushed and sieved to obtain flocculant powder.
The particle size of the powder is less than 0.5 mm.
According to the invention, two cross-linking agents are selected for cross-linking to obtain a cationic polyacrylamide product, so that the molecular chain of the cationic polyacrylamide product can carry more charges, the charges carried by sludge particles can be better neutralized, the sludge particles are separated from water molecules, and the dehydration performance of the cationic polyacrylamide product is improved; the probability of collision between the neutralized sludge flocs and the flocs is increased, so that the sludge is easy to agglomerate and rapidly settle. Therefore, the sedimentation performance of the sludge can be improved. Finally, the dehydration rate of the sludge can be minimized through the mechanical action.
The crosslinking type cationic polyacrylamide sludge dehydrating agent provided by the invention is added with adipic acid and zinc sulfate as an active additive in the reaction process. The adipic acid has strong coordination effect, can form a soluble complex with Fe3+ in a reducing agent generated by redox reaction, and can increase the solubility of the product; the addition of zinc sulfate promotes the polymerization reaction to be more complete and reduces the residual monomer content.
The invention adopts the aqueous solution internal crosslinking rapid polymerization method for preparation, the reaction process is easy to control, the operation is simple, the product quality is stable, the energy consumption in the production and drying processes is low, and the environment is not polluted.
When the crosslinking type cationic polyacrylamide sludge dehydrating agent provided by the invention is used for dehydrating sludge, the sludge settling rate is high, the dehydrating performance is good, the filterability is strong, and the dehydrating rate is high; the operation is simple, no other harmful agents are added, no secondary pollution exists, and the defect of the conventional sludge dehydrating agent can be overcome.
Detailed Description
The present invention is further illustrated by the following examples.
Examples
A cross-linking type cationic polyacrylamide sludge dehydrating agent and a preparation method thereof are carried out according to the following steps:
1. the reaction solution was prepared, and the composition of each set of examples is shown in the following table:
2. respectively and uniformly mixing the components of each group of examples, and then adjusting the pH value of the whole solution to 3-6 by using phosphoric acid; cooling to-5 deg.C
3. Pouring the solution cooled in the step (2) into a heat preservation reaction device, introducing nitrogen, discharging oxygen, firstly adding 800mg of azo initiator and 60mg of chelating agent, adding 10mg of chain transfer agent after 5min, and adding 40mg of oxidant and 20mg of reducing agent after continuously separating for 5 min; after the reaction is initiated, closing the nitrogen valve, reacting for 4 hours, and then preserving heat for 2 hours to obtain a flocculant colloid; wherein the azo initiator is azobisisobutylimidazoline hydrochloride VA 044; the chelating agent is diethylene triamine pentaacetic acid pentasodium Versenex 80; the chain transfer agent is sodium hypophosphite HYPO; the oxidant is sodium persulfate SPS; the reducing agent is ferrous ammonium sulfate MS;
4. and (4) finally, crushing the colloid in the step (3), drying at high temperature, crushing and sieving to obtain flocculant powder which is numbered as CPAM 1-5.
Comparative example 1
The preparation of the conventional cationic flocculant is carried out according to the following steps:
(1) the reaction solution was prepared, and the composition of each set of examples is shown in the following table:
(2) respectively and uniformly mixing the components in each group of proportion, and then adjusting the pH value of the whole solution to 3-6 by using phosphoric acid; cooling to-5 deg.C
(3) Pouring the solution cooled in the step (2) into a heat preservation reaction device, introducing nitrogen, discharging oxygen, firstly adding 800mg of azo initiator and 60mg of chelating agent, adding 10mg of chain transfer agent after 5min, and adding 40mg of oxidant and 20mg of reducing agent after continuously separating for 5 min; after the reaction is initiated, closing the nitrogen valve, reacting for 4 hours, and then preserving heat for 2 hours to obtain a flocculant colloid; wherein the azo initiator is azobisisobutylimidazoline hydrochloride VA 044; the chelating agent is diethylene triamine pentaacetic acid pentasodium Versenex 80; the active auxiliary agent is ZINC; the chain transfer agent is sodium hypophosphite HYPO; the oxidant is sodium persulfate SPS; the reducing agent is ferrous ammonium sulfate MS;
(4) and (4) finally, crushing the colloid in the step (3), drying at high temperature, crushing and sieving to obtain flocculant powder which is numbered as Contrast 1-5.
The sludge is an activated sludge sample of a water treatment tank of a certain chemical plant, and the water sample amount of the sludge is 200 ml. The characteristics are shown in table 1:
TABLE 1 basic characteristics of the sludge
The crosslinked cationic flocculants prepared in examples 1, 2, 3, 4, and 5 and the conventional cationic flocculants prepared in comparative examples 1, 2, 3, and 4, and the like were subjected to sludge dewatering performance evaluation. The flocculation procedure in this experiment was as follows: the addition amount of PAC is 5ppm, and the addition amount of PAM is 2 ppm; firstly, taking a mud water sample with the volume of 200ml, adding PAC (polyaluminium chloride) for rapid stirring for 30s (200 r/min), then adding PAM (polyacrylamide), slowly stirring for 60s (40 r/min), putting the sample into a corresponding device after stirring is finished, and measuring necessary parameters: filtration rate (mass of filtered liquid within 30 s), sludge supernatant turbidity (RTS), sludge moisture content (FCMC) and sludge Specific Resistance (SRF), results are as in table 2:
TABLE 2 evaluation table of sludge dewatering performance
The results of the above example applications show the best choice of the combination of the crosslinking agents N-2, 2-propenyl-2-acrylamide and N, N, N ', N' -tetraallylethylenediamine TAEDA used in example two. In all products, the effect is best, the quality of the filtered liquid within 30s can be improved by 3 times of that of the conventional cationic flocculant dehydrating agent, the water content of the sludge can be reduced to about 60.13 percent, which is far lower than 93.66 percent of that of the conventional cationic flocculant dehydrating agent, and the performance is improved excellently.
Claims (9)
1. The cross-linking type cationic polyacrylamide sludge dehydrating agent is characterized by being prepared from the following components in parts by weight: 30-80 parts of deionized water; 10-60 parts of acrylamide; 30-80 parts of acryloyloxyethyl trimethyl ammonium chloride; 2-8 parts of methacryloyloxyethyl trimethyl ammonium chloride; 2-6 parts of ammonium sulfate; 1-5 parts of adipic acid; 0.001-0.1 part of active auxiliary agent ZINC; 0.005-0.1 part of chelating agent; 0.01-0.5 part of azo initiator; 0.002-8 parts of a cross-linking agent; 0.001-0.035 parts of a chain transfer agent; 0.001-0.08 part of an oxidant; 0.001-0.05 part of reducing agent.
2. The cross-linking type cationic polyacrylamide sludge dewatering agent according to claim 1, wherein: the chelating agent is one or two of diethylenetriamine pentaacetic acid pentasodium (Versenex 80) and Ethylene Diamine Tetraacetic Acid (EDTA).
3. The cross-linking type cationic polyacrylamide sludge dewatering agent according to claim 1, wherein: the azo initiator is azo, such as one or more of Azobisisobutyronitrile (AZDN), azobisisobutylimidazoline hydrochloride (VA044), azobisisobutylamidine hydrochloride (V50), azobisisopropylimidazoline (VA061) and azobiscyanovaleric acid (ACVA).
4. The cross-linking type cationic polyacrylamide sludge dewatering agent according to claim 1, wherein: the cross-linking agent is one or two of N-2, 2-propenyl-2-acrylamide, Triallylamine (TAA), N, N, N ', N' -Tetraallylethylenediamine (TAEDA), Tetraallyloxyethane (TAE), pentaerythritol triacrylate (PETA) and tetraallylammonium chloride (TAAC),
preferably, N-2, 2-propenyl-2-acrylamide is used as the main crosslinking agent, and others are used as the auxiliary crosslinking agents.
5. The cross-linking type cationic polyacrylamide sludge dewatering agent according to claim 1, wherein: the chain transfer agent is one or two of sodium Hypophosphite (HYPO), sodium formate and amino ethanol.
6. The cross-linking type cationic polyacrylamide sludge dewatering agent according to claim 1, wherein: the oxidant is one or two of Sodium Persulfate (SPS) and potassium persulfate (KPS).
7. The cross-linking type cationic polyacrylamide sludge dewatering agent according to claim 1, wherein: the reducing agent is one or two of sodium Metabisulfite (MBS), Sodium Bisulfite (SBS) and ferrous ammonium sulfate (MS).
8. A preparation method of a cross-linking type cationic polyacrylamide sludge dehydrating agent is characterized by comprising the following steps: firstly, preparing a reaction solution, mixing and stirring deionized water, acrylamide, acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, N-2, 2-propenyl-2-acrylamide, ammonium sulfate, adipic acid, a coagent ZINC and other auxiliary cross-linking agents until the ammonium sulfate is completely dissolved, and then adding phosphoric acid to adjust the pH of the whole solution to 3-6; cooling to-5 ℃, injecting into a reaction device, introducing nitrogen, discharging oxygen, adding an azo initiator, a chelating agent, a chain transfer agent, an oxidant and a reducing agent, after reaction initiation, closing a nitrogen introducing valve, reacting for 1-4 hours, and then preserving heat for 1-3 hours to obtain a flocculant colloid; then the colloid is crushed, dried at the high temperature of 60-80 ℃, crushed and sieved to obtain flocculant powder.
9. The method for preparing the cross-linking type cationic polyacrylamide sludge dewatering agent according to claim 8, wherein the method comprises the following steps: the particle size of the powder is less than 0.5 mm.
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Cited By (3)
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| CN113754832A (en) * | 2021-11-10 | 2021-12-07 | 江苏富淼科技股份有限公司 | Solid organic dehydrating agent and preparation method thereof |
| CN113754234A (en) * | 2021-09-14 | 2021-12-07 | 巢湖市爱华环保科技有限公司 | Method for treating phosphorus-containing sludge |
| CN116284565A (en) * | 2023-05-26 | 2023-06-23 | 东营市北陆生物科技有限公司 | Cationic polymer for sludge dewatering and preparation method thereof |
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