CN1994943A - Amphoteric ion high polymer sludge dehydration agent and its preparation method - Google Patents
Amphoteric ion high polymer sludge dehydration agent and its preparation method Download PDFInfo
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- CN1994943A CN1994943A CN 200610123899 CN200610123899A CN1994943A CN 1994943 A CN1994943 A CN 1994943A CN 200610123899 CN200610123899 CN 200610123899 CN 200610123899 A CN200610123899 A CN 200610123899A CN 1994943 A CN1994943 A CN 1994943A
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Abstract
The invention discloses a new typed amphiprotic ion macromolecular sludge dehydrant and making method, which is characterized by the following: adopting non-ion monomer, anion monomer and cation monomer free-radiacal solution to copolymer; initiating soluble oxidizing reducing initiator and azo-initiator; adding cation monomer first and anion monomer then; synthesizing cation-biased amphiprotic ion macromolecular sludge dehydrant.
Description
Technical field
The present invention relates to a kind of new type amphoteric ion high polymer sludge dehydration agent and preparation method thereof.
Background technology
At present, sludge dehydrating agent is divided into two classes usually, and a class is inorganic medicament, mainly comprises molysite, aluminium salt, and another kind of is the organic polymer medicament, and cationic, anionic and non-ionic type are arranged.Increase and sludge characteristics variation along with sewage, sludge quantity that sludge treatment produces, cationic polymer flocculent is to being rich in the processing of organic production, sanitary wastewater, there are problems such as the stripping performance of dewatered cake water ratio height, flco weak strength (the SS rate of recovery is low), dewatered sludge mud cake is not good, are difficult to obtain sufficient dehydrating effect.
For overcoming the defective of above-mentioned cationic polymer flocculent, the common method of using of existing people has proposed the clear 58-215454 patent disclosure of terms of settlement: Ri Tekai a kind of cation polymeric flocculant and anionic polymer flocculation agent, but aforesaid method each composition blending ratio, add in the operation very loaded down with trivial details; The spy opens clear 53-149292 communique and discloses the Amphiphatic high polymer dewatering agent that comprises quaternary ammonium group, this method gained mud moisture content of the cake height, and the filter cloth separability is not good; The spy opens the Amphiphatic high polymer dewatering agent that clear 62-205112 communique discloses the tertiary amine base, but the tertiary amine base do not dissociate in high pH value scope, and this method is for the mud with high pH value, and its performance significantly descends; Te Kaiping 3-18900 communique discloses the Amphiphatic high polymer dewatering agent that has tertiary amine base and quaternary ammonium group simultaneously, has improved the shortcoming of above-mentioned patent, but it still can not be satisfactory aspect dosage and mud moisture content of the cake.
Domestic patent of invention 97123344.6 discloses a kind of amphoteric polyacrylamide flocculating agent and preparation method thereof, and the colloid rebound resilience of this method preparation is poor, is difficult to granulating and forming, is unwell to the powder-like product preparation; 99111315.2 disclose the preparation method that employing " precedingly adds the alkali copolymerization; the posthydrolysis polymerization technique " and synthesized the amphoteric ion polymer of ultra-high molecular weight, but in sludge dewatering is used, partially the multipolymer dewatering of cationic is superior, and partially the multipolymer of cationic should be under the condition of slant acidity initiated polymerization.
Summary of the invention
The objective of the invention is to overcome that the prior art married operation is loaded down with trivial details, sludge dewatering weak effect, the not wide shortcoming of pH value scope, a kind of preparation method of the new type amphoteric ion high polymer sludge dehydration agent that is applied to sewage sludge processing aspect of inclined to one side cationic is provided.
The present invention also aims to provide above-mentioned preparation method's synthetic new type amphoteric ion high polymer sludge dehydration agent.
The preparation method of new type amphoteric ion high polymer sludge dehydration agent of the present invention, the mechanism that it is characterized in that polyreaction is that the mechanism of its polyreaction of free radical aqueous solution terpolymerization is free radical aqueous solution terpolymerization, adopt redox initiator and the compound initiation of azo initiator, comprise the steps:
(1) by percentage to the quality, respectively non-ionic monomer, anionic monomer and cationic monomer are made into the aqueous solution that concentration is 10%～40% quality with deionized water, earlier the cationic monomer aqueous solution and the part non-ionic monomer aqueous solution are added in the reactor logical nitrogen; In the monomer solution of preparation, non-ionic monomer accounts for 40%～85% of monomer total mass, and anionic monomer accounts for 7.5%～30% of monomer total mass, and cationic monomer accounts for 7.5%～30% of monomer total mass.
(2) add persulfuric acid salt initiator, sulfites reductive agent and the azo initiator that all is equivalent to monomer total mass 0.1%～1% respectively in the solution that step (1) makes, add the EDTA-2Na that is equivalent to monomer total mass 0.1%～1% again, control reaction temperature is 5 ℃～50 ℃, inspires chain initiation and transfer reaction;
(3) add the pH value that step (1) obtains in the reaction soln of step (2) and be adjusted to 2～6 the anionic monomer aqueous solution and the remaining non-ionic monomer aqueous solution, reacted 3～10 hours, discharging obtains colloid drying, pulverizing, granulation and promptly gets amphoteric ion high polymer sludge dehydration agent;
In the monomer solution of step (1) preparation, non-ionic monomer accounts for 40%～85% of monomer total mass, and anionic monomer accounts for 7.5%～30% of monomer total mass, and cationic monomer accounts for 7.5%～30% of monomer total mass.
The described non-ionic monomer of step (1) is acrylamide or Methacrylamide preferably; Anionic monomer is 2-acrylamido-2-methyl propane sulfonic acid, 2-acrylamido-2-methyl propane sulfonic acid sodium, vinylformic acid or sodium acrylate; Cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac, methylacryoyloxyethyl trimethyl ammonium chloride, dimethyl diallyl trimethyl ammonium chloride or trimethylamine groups methyl acrylate ammonium chloride.
Persulfuric acid salt initiator described in the step (2) is ammonium persulphate, Sodium Persulfate or Potassium Persulphate preferably, the sulfites reductive agent is sodium bisulfite or S-WAT, and azo initiator is two NSC 18620 hydrochlorides of azo or the two Methylimidazole quinoline propane hydrochloride salt of azo.
The preparation method of new type amphoteric ion high polymer sludge dehydration agent, the pH value of polyreaction is carried out under the slant acidity condition, and this macromolecular chain is inclined to one side cationic.When pH＞7, hydrolysis can take place in monomer molecule or polymkeric substance, forms the polymkeric substance that contains carboxyl.Therefore the multipolymer of expecting inclined to one side cationic should select initiated polymerization in the pH value slant acidity scope under the condition of slant acidity.
The preparation method of new type amphoteric ion high polymer sludge dehydration agent, polyreaction " add cationic monomer earlier, add anionic monomer again " step by step.In order to obtain forming uniform multipolymer, press composition requirement design feed ratio, add part non-ionic monomer and cationic monomer earlier, restock non-ionic monomer and adding anionic monomer in the reaction process are to guarantee that proportioning keeps constant relatively substantially.
The present invention compared with prior art has following advantage:
(1), preparation method of the present invention takes " add earlier cationic monomer, add anionic monomer again ", makes the molecular structure of multipolymer form more even.
(2), preparation method of the present invention takes initiated polymerization under the condition of slant acidity, makes the amphoteric ion high polymer sludge dehydration agent of inclined to one side cationic.
(3), the amphoteric ion high polymer sludge dehydration agent that provides of the present invention is used for sludge treatment, it is little to have a consumption, the pH scope of application is wide, flco is thick, handles advantages such as the back moisture percentage in sewage sludge is low.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1 one
(1) respectively 1.6 kilograms of acrylamides (industrial refining pure pulvis) is made into 16 kg water solution with deionized water, 0.15 kilogram 2-acrylamido-2-methyl propane sulfonic acid (industrial refining pure pulvis) is made into 1.5 kg water solution, 0.32 kilogram of acrylyl oxy-ethyl-trimethyl salmiac (concentration is 80% industrial refined soln) is made into 2.5 kg water solution.Earlier 2.5 kilograms of acrylyl oxy-ethyl-trimethyl salmiac aqueous solution and 8 kilograms of acrylamide solutions addings are had in the enamel reactor of agitator and heating jacket, start stirring, logical nitrogen;
(2) in the solution of reactor, add 0.008 kilogram of ammonium persulphate respectively, 0.002 the kilogram sodium bisulfite, the two NSC 18620 hydrochlorides of 0.014 kilogram of azo add 0.02 kilogram EDTA-2Na again, control reaction temperature is 25 ℃, inspires chain initiation and transfer reaction;
(3) add in still internal reaction solution that to regulate the pH value through hydrochloric acid and sodium hydroxide be 1.5 kilograms of 2-acrylamido-2-methyl propane sulfonic acid aqueous solution and 8 kilograms of acrylamide solutions of 2, reacted 5 hours, discharging obtains colloid drying, pulverizing, granulation and promptly gets amphoteric ion high polymer sludge dehydration agent.
Embodiment 2 two
(1) respectively 1.6 kilograms of Methacrylamides (industrial refining pure pulvis) is made into 8 kg water solution with deionized water, 1.2 kilogram 2-acrylamido-2-methyl propane sulfonic acid sodium (industrial refining pure pulvis) is made into 6 kg water solution, 1.5 kilograms of methylacryoyloxyethyl trimethyl ammonium chlorides (concentration is 80% industrial refined soln) are made into 6 kg water solution.Earlier 6 kilograms of methylacryoyloxyethyl trimethyl ammonium chloride aqueous solution and 3 kilograms of methacryloyl amine aqueous solutions addings are had in the enamel reactor of agitator and heating jacket, start stirring, logical nitrogen;
(2) in the solution of reactor, add 0.016 kilogram of Sodium Persulfate respectively, 0.004 the kilogram S-WAT, the two Methylimidazole quinoline propane hydrochloride salt of 0.028 kilogram of azo add 0.04 kilogram EDTA-2Na again, control reaction temperature is 5 ℃, inspires chain initiation and transfer reaction;
(3) add in still internal reaction solution that to regulate the pH value through hydrochloric acid and sodium hydroxide be 6 kilograms of 2-acrylamido-2-methyl propane sulfonic acid sodium water solutions and 5 kilograms of methacryloyl amine aqueous solutions of 4, reacted 10 hours, discharging obtains colloid drying, pulverizing, granulation and promptly gets amphoteric ion high polymer sludge dehydration agent.
Embodiment 3 three
(1) respectively 3.6 kilograms of acrylamides (industrial refining pure pulvis) is made into 12 kg water solution with deionized water, 1.02 kilogram vinylformic acid (industrial refining pure solution) is made into 3.4 kg water solution, 2.3 kilograms of dimethyl diallyl trimethyl ammonium chlorides (concentration is 60% industrial refined soln) are made into 4.6 kg water solution.Earlier 4.6 kilograms of dimethyl diallyl trimethyl ammonium chloride aqueous solution and 8 kilograms of acrylamide solutions addings are had in the enamel reactor of agitator and heating jacket, start stirring, logical nitrogen;
(2) in the solution of reactor, add 0.024 kilogram of Potassium Persulphate respectively, 0.006 the kilogram sodium bisulfite, the two NSC 18620 hydrochlorides of 0.042 kilogram of azo add 0.06 kilogram EDTA-2Na again, control reaction temperature is 50 ℃, inspires chain initiation and transfer reaction;
(3) add in still internal reaction solution that to regulate the pH value through hydrochloric acid and sodium hydroxide be 3.4 kilograms of acrylic acid aqueous solutions and 4 kilograms of acrylamide solutions of 6, reacted 3 hours, discharging obtains colloid drying, pulverizing, granulation and promptly gets amphoteric ion high polymer sludge dehydration agent.
Embodiment 4 four
(1) respectively 6.8 kilograms of Methacrylamides (industrial refining pure pulvis) is made into 17 kg water solution with deionized water, 0.6 kilogram sodium acrylate (industrial refining pure solution) is made into 1.5 kg water solution, 0.75 kilogram of trimethylamine groups methyl acrylate ammonium chloride (concentration is 80% industrial refined soln) is made into 1.5 kg water solution.Earlier 1.5 kilograms of trimethylamine groups methyl acrylate aqueous ammonium chloride solutions and 17 kilograms of methacryloyl amine aqueous solutions addings are had in the enamel reactor of agitator and heating jacket, start stirring, logical nitrogen;
(2) in the solution of reactor, add 0.032 kilogram of ammonium persulphate respectively, 0.008 the kilogram S-WAT, the two Methylimidazole quinoline propane hydrochloride salt of 0.056 kilogram of azo add 0.08 kilogram EDTA-2Na again, control reaction temperature is 35 ℃, inspires chain initiation and transfer reaction;
(3) add in still internal reaction solution that to regulate the pH value through hydrochloric acid and sodium hydroxide be 1.5 kilograms of sodium acrylate aqueous solution of 3, reacted 8 hours, discharging obtains colloid drying, pulverizing, granulation and promptly gets amphoteric ion high polymer sludge dehydration agent.
The amphoteric ion high polymer sludge dehydration agent that embodiment 1 one is made is applied to certain city domestic sewage treatment plant mud to be drained off (water ratio 97～98%, pH value 6.8), the result shows: use amphoteric ion high polymer sludge dehydration agent, when dosage was 40mg/L, the mud resistivity was from 28.4 * 10
12M/kg drops to 7.8 * 10
12M/kg, water ratio drops to 77.2%; Under the similarity condition, certain commercially available CPAM handles back mud resistivity 16.1 * 10
12M/kg, water ratio 79.7%.This sludge pH value was transferred to 8.5 o'clock, and this patent amphoteric ion high polymer sludge dehydration agent is handled back mud resistivity 13.2 * 10
12M/kg, water ratio 79.5%; Certain commercially available CPAM handles back mud resistivity 23.5 * 10
12M/kg, water ratio 84.6%; The pH value transferred to 9.5 o'clock, and this patent amphoteric ion high polymer sludge dehydration agent is handled back mud resistivity 18.2 * 10
12M/kg, water ratio 81.5%; Certain commercially available CPAM handles back mud resistivity 35.5 * 10
12M/kg, water ratio 87.6%.
Claims (5)
1, a kind of preparation method of amphoteric ion high polymer sludge dehydration agent, the mechanism that it is characterized in that polyreaction adopts redox initiator and the compound initiation of azo initiator to make for by free radical aqueous solution terpolymerization, comprises the steps:
(1) by percentage to the quality, respectively non-ionic monomer, anionic monomer and cationic monomer are made into the aqueous solution that concentration is 10%～40% quality with deionized water, earlier the cationic monomer aqueous solution and the part non-ionic monomer aqueous solution are added in the reactor logical nitrogen; In the monomer solution of preparation, non-ionic monomer accounts for 40%～85% of monomer total mass, and anionic monomer accounts for 7.5%～30% of monomer total mass, and cationic monomer accounts for 7.5%～30% of monomer total mass.
(2) add persulfuric acid salt initiator, sulfites reductive agent and the azo initiator that all is equivalent to monomer total mass 0.1%～1% respectively in the solution that step (1) makes, add the EDTA-2Na that is equivalent to monomer total mass 0.1%～1% again, control reaction temperature is 5 ℃～50 ℃, inspires chain initiation and transfer reaction;
(3) add the pH value that step (1) obtains in the reaction soln of step (2) and be adjusted to 2～6 the anionic monomer aqueous solution and the remaining non-ionic monomer aqueous solution, reacted 3～10 hours, discharging obtains colloid drying, pulverizing, granulation and promptly gets amphoteric ion high polymer sludge dehydration agent;
In the monomer solution of step (1) preparation, non-ionic monomer accounts for 40%～85% of monomer total mass, and anionic monomer accounts for 7.5%～30% of monomer total mass, and cationic monomer accounts for 7.5%～30% of monomer total mass.
2, method according to claim 1 is characterized in that described non-ionic monomer is acrylamide or Methacrylamide; Anionic monomer is 2-acrylamido-2-methyl propane sulfonic acid, 2-acrylamido-2-methyl propane sulfonic acid sodium, vinylformic acid or sodium acrylate; Cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac, methylacryoyloxyethyl trimethyl ammonium chloride, dimethyl diallyl trimethyl ammonium chloride or trimethylamine groups methyl acrylate ammonium chloride.
3, method according to claim 1 and 2, it is characterized in that the persulfuric acid salt initiator described in the step (2) is ammonium persulphate, Sodium Persulfate or Potassium Persulphate, the sulfites reductive agent is sodium bisulfite or S-WAT, and azo initiator is two NSC 18620 hydrochlorides of azo or the two Methylimidazole quinoline propane hydrochloride salt of azo.
4, method according to claim 3 is characterized in that adopting in the step (3) hydrochloric acid or sodium hydroxide to regulate the pH value.
5, the amphoteric ion high polymer sludge dehydration agent of the described method preparation of one of claim 1-4.
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| CN104004130A (en) * | 2014-05-29 | 2014-08-27 | 华南理工大学 | Composite macromolecular sludge dehydrating agent and preparation method thereof |
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| CN108083613A (en) * | 2017-12-27 | 2018-05-29 | 广州再森新材料科技有限公司 | A kind of sewage sludge high-efficiency dehydration agent and its preparation method and application |
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| CN110981160A (en) * | 2019-12-23 | 2020-04-10 | 广东慧信环保有限公司 | Novel composite sludge dehydrating agent and preparation and use methods thereof |
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| CN102144955A (en) * | 2011-04-16 | 2011-08-10 | 华南理工大学 | Polymer conditioner for hairs as well as preparation method and application thereof |
| CN102144955B (en) * | 2011-04-16 | 2013-09-25 | 华南理工大学 | Polymer conditioner for hairs as well as preparation method and application thereof |
| CN104004130A (en) * | 2014-05-29 | 2014-08-27 | 华南理工大学 | Composite macromolecular sludge dehydrating agent and preparation method thereof |
| CN106976941A (en) * | 2017-04-12 | 2017-07-25 | 芜湖扬展新材料科技服务有限公司 | A kind of preparation method of novel cation composite flocculant |
| CN108083613A (en) * | 2017-12-27 | 2018-05-29 | 广州再森新材料科技有限公司 | A kind of sewage sludge high-efficiency dehydration agent and its preparation method and application |
| CN109180863A (en) * | 2018-07-18 | 2019-01-11 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of both sexes organic polymer coargulator and products thereof and application |
| CN109180863B (en) * | 2018-07-18 | 2020-12-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of amphoteric organic polymeric flocculant, product and application thereof |
| CN110981160A (en) * | 2019-12-23 | 2020-04-10 | 广东慧信环保有限公司 | Novel composite sludge dehydrating agent and preparation and use methods thereof |
| CN115322281A (en) * | 2022-07-26 | 2022-11-11 | 中海石油环保服务（天津）有限公司 | Amphoteric sludge dehydrating agent and preparation method thereof |
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