CN104986939A - Preparing method for modified wood powder amphiprotic dehydrating agent - Google Patents
Preparing method for modified wood powder amphiprotic dehydrating agent Download PDFInfo
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- CN104986939A CN104986939A CN201510382972.6A CN201510382972A CN104986939A CN 104986939 A CN104986939 A CN 104986939A CN 201510382972 A CN201510382972 A CN 201510382972A CN 104986939 A CN104986939 A CN 104986939A
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Abstract
The invention provides a preparing method for a modified wood powder amphiprotic dehydrating agent. The method is characterized by comprising the steps that dispersing treatment is carried out on wood powder, after alkalization is carried out, etherification reaction is carried out by adding a certain amount of 3-chloropropionic acid, a carboxyethylation product is obtained, graft copolymerization reaction is carried out on the carboxyethylation product and acrylamide, a graft copolymerization product is obtained, mannich reaction is further carried out on the graft copolymerization product, and the modified amphiprotic dehydrating agent is obtained. According to the amphiprotic dehydrating agent, due to the fact that the hydration effect and the electrostatic repulsion effect between particles with different sizes in sludge are lowered, the mutual structural constitution is improved, new sludge particles with appropriate sizes are formed, the sludge positive pressure dehydrating effect is achieved, the good dissoluvability is achieved, during processing of the sludge, generated flocculating constituents are big, the sedimentation is rapid, the water yield is high, and the processing efficiency of the sludge is improved. Compared with a traditional dehydrating agent, the amphiprotic dehydrating agent has the advantages that the pollution is low, the degradation is easy to carry out, the toxicity does not exist, the effect is good, the application range is wide, and the secondary pollution in the sludge processing process is avoided.
Description
Technical field
The present invention relates to and belongs to sludge dehydrating agent, relates generally to a kind of preparation method of modified wood powder both sexes dewatering agent.
Background technology
At present, in worldwide, the disposal mainstream technology of mud has three kinds: stablize landfill, Land_use change, burning, also has quite a few to throw aside in environment without any process.In China's specific resistance to filtration method, agricultural sludge accounts for 44.8%, land landfill accounts for 31.0%, burning disposal accounts for 3.5%, other process account for 6.9%, unprocessedly accounts for 13.8%.Water ratio is high, it is large to account for volume, and moisture to be difficult to remove be the most significant feature of municipal sewage sludge.Ordinary meaning being said, in order to reduce sludge moisture content, processed must be carried out to mud, specifically comprise concentrated, digestion and dehydration etc.But only pass through the sludge moisture content after above-mentioned steps still very high, now need to improve its solid content as far as possible, mud is become semi-solid state from liquid state.The features such as have different kinds and character according to mud, variability is large, dehydration difficulty, the method for lignin-sludge also has many kinds, and the chemical dehydration of mud realizes the most frequently used treatment step of mud decrement.In mud, adding flocculation agent to improve the dewatering of mud is conventional sludge chemical dewatering.The principle of sludge dehydrating agent is exactly make with the inorganic of electric charge or organic medicament at mud colloid surface react with, in and mud granule electric charge, water is separated from mud granule, makes mud granule condense into large particle flco simultaneously, improve the dewatering of mud.Therefore also flocculation agent can be called because sludge dehydrating agent mainly plays throwing out.
Ordinary meaning is said, sludge dehydrating agent must possess the effect of increase-volume and dispersion, and wherein dissemination refers to Bound moisture in order to discharge former flco inside and structure flco disperseed or disintegrates; Solubilising is to make dewatering speed accelerate, and dehydrating effect improves and makes ECP hydrolysis in solution, and the avidity of flco to water is reduced greatly.But the dewatering agent of high-quality also must possess the collaborative work effect of dewatering agent constitutive material, this effect is similar to catalyst action, can accelerate or chemical reaction between catalytic specie, make dehydrating effect fast and obviously, this sludge dehydrating agent often makes the sludge moisture content after dewatering be reduced to less than 55% after a procedure, substantially reduces the volume of mud.Current sludge treatment flocculation agent used is mainly divided into organic polymer type, biotype and inorganic type.Usual inorganic flocculating agent large usage quantity, effect is undesirable, and metal ion can be brought among the final process product of mud, causes secondary pollution to environment; Organic synthesis polymeric flocculant biological degradation difficulty, residue is toxic, can to environment, very large to the harm of HUMAN HEALTH.Therefore, development of new flocculation agent has become the key of sludge drying process.
Summary of the invention
For currently available technology Problems existing, the object of the invention is to a kind of preparation method of modified wood powder both sexes dewatering agent, it is mainly the natural polymer dewatering agent of Material synthesis with wood powder, compared with conventional dehydration agent, this both sexes dewatering agent have pollute little, easy degraded, there is no toxicity, effective and be widely used, belong to environmentally friendly dewatering agent, reduce sludge handling process and introduce secondary pollution.
The present invention solves the problems of the technologies described above adopted technical scheme:
A kind of preparation method of modified wood powder both sexes dewatering agent, it is characterized in that, first wood powder is carried out dispersion treatment, through alkalization, add quantitative 3-chloropropionic acid and carry out etherification reaction, the carboxyethylated product obtained, carry out graft copolymerization with acrylamide again, by the graft copolymerization product obtained, then carry out mannich reaction, obtain the both sexes dewatering agent of modification, its concrete operation steps is as described below:
(1) carboxymethylation reaction: get in a certain amount of wood powder and beaker, add in proportion dehydrated alcohol wood powder is moistening, be uniformly dispersed, then the alkalization of quantitative alkali lye is added, alkalization time is 0.5 ~ 1h, and temperature controls at 45 ~ 55 DEG C, then adds quantitative 3-chloropropionic acid, keep temperature of reaction, carry out etherification reaction 1.5 ~ 2h, obtain carboxyethylated product, wherein alkali lye: wood powder: 3-chloropropionic acid feeds intake (weight ratio)=1:2:2;
(2) graft copolymerization: add carboxyethylated product and deionized water in there-necked flask, logical nitrogen is also heated to preset temperature, with Potassium Persulphate (K under at the uniform velocity stirring
2s
2o
8) be initiator, with a certain amount of acrylamide for reaction monomers carries out graft copolymerization, reaction 2 ~ 3h, temperature of reaction is 45 ~ 55 DEG C, obtains graft copolymerization product C GAA, wherein acrylamide: (the weight ratio)=5:2 that feeds intake of wood powder;
(3) mannich reaction: a certain amount of graft copolymer is dissolved in deionized water, then the there-necked flask in thermostat water bath is poured into, add a certain amount of formaldehyde solution again, stirring reaction for some time under certain temperature, drip a certain amount of triethylene tetramine (diethylamine), continue reaction 1 ~ 2h, after cooling, product is neutralized to pH=6 ~ 7, obtain Amphiphatic high polymer dewatering agent CGAAC, wherein graft copolymerization product (CGAA): formaldehyde: (the mol ratio)=1:0.9:1 that feeds intake of triethylene tetramine (diethylamine).
The product that this experiment adds triethylene tetramine synthesis is both sexes dewatering agent-c, and the product adding diethylamine synthesis is both sexes dewatering agent-d.
Further, the alkali lye in step (1) is sodium hydroxide solution or potassium hydroxide solution, and massfraction is 40 ~ 60%.
Further, the charging capacity of initiator accounts for the massfraction of carboxyethylated product is 3 ~ 5%.
Further, the massfraction of dehydrated alcohol is 95%.
The invention has the advantages that: both sexes dewatering agent prepared by the present invention, by the hydration in reduction mud between size particles and electrostatic repulsion, improve mutual structure composition, form the new mud granule that volume size is suitable, thus reach mud malleation dehydrating effect, there is good solubility, the process of mud is generated to flocs unit is large, sedimentation is fast, water rate is high, improves the processing efficiency of mud significantly.Compared with conventional dehydration agent, this both sexes dewatering agent have pollute little, easy degraded, there is no toxicity, effective and be widely used, avoid sludge handling process and introduce secondary pollution.
Embodiment
For specific embodiment, concrete introduction is done to the present invention below.
Embodiment 1: a kind of preparation method of triethylene tetramine type dewatering agent:
(1) carboxymethylation reaction: get in 240g wood powder and beaker, add 140mL 95% dehydrated alcohol in proportion wood powder is moistening, be uniformly dispersed, then add 240g sodium hydroxide and carry out 0.5h alkalization, temperature controls at 50 DEG C, then adds the 3-chloropropionic acid of 240g, keeps temperature of reaction, carry out etherification reaction 2h, obtain carboxyethylated product.
(2) graft copolymerization: add carboxyethylated product and deionized water in there-necked flask, logical nitrogen is also heated to preset temperature, under at the uniform velocity stirring, adds 50g Potassium Persulphate (K
2s
2o
8) be initiator, with the acrylamide of 600g for reaction monomers carries out graft copolymerization, reaction 2.5h, temperature of reaction is 50 DEG C, obtains graft copolymerization product C GAA.
(3) mannich reaction: a certain amount of graft copolymer is dissolved in deionized water, then the there-necked flask in thermostat water bath is poured into, add a certain amount of formaldehyde solution again, stirring reaction for some time at 50 DEG C of temperature, drip a certain amount of triethylene tetramine, continue reaction 1.5h, after cooling, product is neutralized to pH=6 ~ 7, obtain Amphiphatic high polymer dewatering agent CGAAC, wherein graft copolymerization product (CGAA): formaldehyde: (the mol ratio)=1:0.9:1 that feeds intake of triethylene tetramine.
Embodiment 2:
(1) carboxymethylation reaction: get in 240g wood powder and beaker, add 140mL 95% dehydrated alcohol in proportion wood powder is moistening, be uniformly dispersed, then add 240g sodium hydroxide and carry out 0.5h alkalization, temperature controls at 50 DEG C, then adds the 3-chloropropionic acid of 240g, keeps temperature of reaction, carry out etherification reaction 2h, obtain carboxyethylated product.
(2) graft copolymerization: add carboxyethylated product and deionized water in there-necked flask, logical nitrogen is also heated to preset temperature, under at the uniform velocity stirring, adds 50g Potassium Persulphate (K
2s
2o
8) be initiator, with the acrylamide of 600g for reaction monomers carries out graft copolymerization, reaction 2.5h, temperature of reaction is 50 DEG C, obtains graft copolymerization product C GAA.
(3) mannich reaction: a certain amount of graft copolymer is dissolved in deionized water, then the there-necked flask in thermostat water bath is poured into, add a certain amount of formaldehyde solution again, stirring reaction for some time at 50 DEG C of temperature, drip a certain amount of diethylamine, continue reaction 1.5h, after cooling, product is neutralized to pH=6 ~ 7, obtain Amphiphatic high polymer dewatering agent CGAAD, wherein graft copolymerization product (CGAA): formaldehyde: (the mol ratio)=1:0.9:1 that feeds intake of diethylamine.
Embodiment 3:
Sludge dewatering experiment is carried out by implementing the sharp 1 and 2 both sexes sludge dehydrating agents obtained, get 1kg mud, the both sexes dewatering agent of 6g is added at it, stirring velocity is 300r/min, and churning time is 20min, and time of repose is 10min, pH scope 6 ~ 9 range of application is wider, dewatering agent uses not by temperature limitation, and flocs unit is large, and in mud, the clearance of water is between 81.3 ~ 85.4%.
The present invention is not limited to above-mentioned embodiment, and those skilled in the art also can make multiple change accordingly, but to be anyly equal to the present invention or similar change all should be encompassed in the scope of the claims in the present invention.
Claims (4)
1. the preparation method of a modified wood powder both sexes dewatering agent, it is characterized in that, first wood powder is carried out dispersion treatment, through alkalization, add quantitative 3-chloropropionic acid and carry out etherification reaction, the carboxyethylated product obtained, carry out graft copolymerization with acrylamide again, by the graft copolymerization product obtained, then carry out mannich reaction, obtain the Amphiphatic high polymer dewatering agent of modification, its concrete operation steps is as described below:
(1) carboxymethylation reaction: get in a certain amount of wood powder and beaker, add in proportion dehydrated alcohol wood powder is moistening, be uniformly dispersed, then the alkalization of quantitative alkali lye is added, alkalization time is 0.5 ~ 1h, and temperature controls at 45 ~ 55 DEG C, then adds quantitative 3-chloropropionic acid, keep temperature of reaction, carry out etherification reaction 1.5 ~ 2h, obtain carboxyethylated product, wherein alkali lye: wood powder: 3-chloropropionic acid feeds intake (weight ratio)=1:2:2;
(2) graft copolymerization: add carboxyethylated product and deionized water in there-necked flask, logical nitrogen is also heated to preset temperature, with Potassium Persulphate (K under at the uniform velocity stirring
2s
2o
8) be initiator, with a certain amount of acrylamide for reaction monomers carries out graft copolymerization, reaction 2 ~ 3h, temperature of reaction is 45 ~ 55 DEG C, obtains graft copolymerization product C GAA, wherein acrylamide: (the weight ratio)=5:2 that feeds intake of wood powder;
(3) mannich reaction: a certain amount of graft copolymer is dissolved in deionized water, then the there-necked flask in thermostat water bath is poured into, add a certain amount of formaldehyde solution again, stirring reaction for some time under certain temperature, drip a certain amount of triethylene tetramine (diethylamine), continue reaction 1 ~ 2h, after cooling, product is neutralized to pH=6 ~ 7, obtain Amphiphatic high polymer dewatering agent CGAAC, wherein graft copolymerization product (CGAA): formaldehyde: (the mol ratio)=1:0.9:1 that feeds intake of triethylene tetramine (diethylamine).
2. the preparation method of a kind of modified wood powder both sexes dewatering agent according to claim 1, it is characterized in that, the alkali lye in step (1) is sodium hydroxide solution or potassium hydroxide solution, and massfraction is 40 ~ 60%.
3. the preparation method of a kind of modified wood powder both sexes dewatering agent according to claim 1, is characterized in that, the massfraction that the charging capacity of initiator accounts for carboxyethylated product is 3 ~ 5%.
4. the preparation method of a kind of modified wood powder both sexes dewatering agent according to claim 1, is characterized in that, the massfraction of dehydrated alcohol is 95%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108948271A (en) * | 2018-08-31 | 2018-12-07 | 昆明理工大学 | A kind of preparation method and application of potato residues inorganic agent |
| CN108947201A (en) * | 2018-08-31 | 2018-12-07 | 昆明理工大学 | A kind of sludge treating agent and application |
| CN109019946A (en) * | 2018-06-22 | 2018-12-18 | 确成硅化学股份有限公司 | A method of reducing wet process white carbon black industrial wastewater suspended particulate |
| CN110028143A (en) * | 2019-03-25 | 2019-07-19 | 爱环吴世（苏州）环保股份有限公司 | A kind of preparation method of environmentally friendly functional Amphiphatic high polymer coagulant |
| CN110092570A (en) * | 2019-05-14 | 2019-08-06 | 吉林建筑大学 | A kind of sludge concentration and dewatering agent and preparation method thereof |
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| CN101357970A (en) * | 2008-09-23 | 2009-02-04 | 浙江林学院 | Carboxymethyl wood flour water absorbent and preparation method thereof |
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| CN101357970A (en) * | 2008-09-23 | 2009-02-04 | 浙江林学院 | Carboxymethyl wood flour water absorbent and preparation method thereof |
Non-Patent Citations (1)
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| 王杰等: "两性高分子絮凝剂对造纸混合污泥的絮凝脱水性能的研究", 《环境污染治理技术与设备》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019946A (en) * | 2018-06-22 | 2018-12-18 | 确成硅化学股份有限公司 | A method of reducing wet process white carbon black industrial wastewater suspended particulate |
| CN109019946B (en) * | 2018-06-22 | 2022-02-15 | 确成硅化学股份有限公司 | Method for reducing suspended particles in wastewater produced by wet white carbon black production |
| CN108948271A (en) * | 2018-08-31 | 2018-12-07 | 昆明理工大学 | A kind of preparation method and application of potato residues inorganic agent |
| CN108947201A (en) * | 2018-08-31 | 2018-12-07 | 昆明理工大学 | A kind of sludge treating agent and application |
| CN110028143A (en) * | 2019-03-25 | 2019-07-19 | 爱环吴世（苏州）环保股份有限公司 | A kind of preparation method of environmentally friendly functional Amphiphatic high polymer coagulant |
| CN110092570A (en) * | 2019-05-14 | 2019-08-06 | 吉林建筑大学 | A kind of sludge concentration and dewatering agent and preparation method thereof |
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Application publication date: 20151021 |