CN102352256A - Saline-alkali tolerant functional water-retaining agent and preparation method thereof - Google Patents
Saline-alkali tolerant functional water-retaining agent and preparation method thereof Download PDFInfo
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- CN102352256A CN102352256A CN2011102147469A CN201110214746A CN102352256A CN 102352256 A CN102352256 A CN 102352256A CN 2011102147469 A CN2011102147469 A CN 2011102147469A CN 201110214746 A CN201110214746 A CN 201110214746A CN 102352256 A CN102352256 A CN 102352256A
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Abstract
The invention relates to a saline-alkali tolerant functional water-retaining agent and a preparation method thereof. The water-retaining agent is graft copolymer of sulfonated humic acid, N-N'-methylenebisacrylamide and crylic acid; the structural formula of the water-retaining agent is shown in the specifications; and the water-retaining agent has high saline-alkali tolerance, and can absorb tap water in an amount which is 123 times that of the water-retaining agent and absorb sodium carbonate saline, with the pH value of 9, in an amount which is 85 times that of the water-retaining agent. The water-retaining agent can effectively adsorb free sodium ions and heavy metal ions and can effectively reduce alkalinity of soil so as to improve the physical and chemical structure of the soil. The water-retaining agent is prepared by a normal temperature polymerization method, and has a simple process and mild reaction conditions. The crylic acid and the humic acid serve as main raw materials; potassium, nitrogen and organic matters required by plant growth can be supplemented; and the sulfonated humic acid is released slowly, so that growth of plants is promoted.
Description
Technical field
The present invention relates to a kind of salt tolerant alkali functional type water-holding agent and preparation method thereof, function of dominant macromolecular material synthesizes the field.
Background technology
China is one of the most serious country of soil erosion in the world, and national soil erosion area 3,560,000 sq-kms account for 37.1% of area.Control soil erosion and prevent and control desertification, become the important content of China's Sustainable development.In implementing numerous methods of soil conservation, using the super absorbent resin conservation of soil and water, preventing and treating arid and desertification is the new direction of research at present.
Humic acids has good chemically reactive and biological activity; Humic acids is carried out sulfonation modifying contains humic acids later on as the feedstock production of synthetic water-holding agent water-absorbing resin; Can improve the water-retaining capacity of water-absorbing resin; Can improve the anti-saline and alkaline ability of water-absorbing resin again; Can bring into play the effect that humic acids promotes plant-growth, improves the soil physical chemistry structure, improves the fertilizer-preserving ability of soil, the improvement alkaline land soil is had important effect.Document [1] has been announced a kind of synthesis method that contains the humic acid High hydrophilous resin, is raw material with Sodium salts humic acids and acrylamide, with N; N '-methylene-bisacrylamide is a linking agent; Initiator is a Potassium Persulphate, adds certain density NaOH solution then, feeds nitrogen 5min and sealing orifice.Take out product behind 65 ℃ of reaction 6h and cut into dices, wash repeatedly with distilled water and be placed on the dry xerogel that gets in 65 ℃ of vacuum drying ovens.Document [2] has also been announced a kind of synthesis method that contains the humic acids High hydrophilous resin; With humic acids and vinylformic acid is raw material; N; N '-methylene-bisacrylamide is a linking agent; Ammonium persulphate is an initiator; Adopt free radicals copolymerization reaction, 65 ℃ are reacted 2h, have synthesized the humic acids absorbent resin of multi-hole type.Document [3] adopts humic acid solution-treated acrylic acid or the like super-strong moisture absorbing resin particle, and acrylic acid or the like super-strong moisture absorbing resin particle is carried out surface graft modification, and 75 ℃, react 60min, obtained a kind of superpower resin of humic acids modification.But this resinoid can not effectively reduce the alkalescence of soil, no ion exchanging function shortcoming, and because heated polymerizable, easy generation gathers cruelly, reacts wayward.(reference: [1] Yi Juzhen, Liang Ziqian, Zhang Liming; The research [J] of Sodium salts humic acids/polyacrylamide hydrophilic gel water absorbing properties; Zhongshan University's journal; 2007,3.[2] Shi Jun, Wang Tao; Synthetic and the performance study [J] of humic acids absorbent resin; Xi'an Petroleum University's journal; 2008,7.[3] Jia Zhenyu, Cui Yingde, Li Xinming, Yin Guoqiang, Zhang Cuirong; The humic acid surface grafting is to the study on the modification [J] of acrylic acid or the like super-strong moisture absorbing resin; The chemical industry progress; 2005,7.)
Summary of the invention
In order to overcome the existing not strong shortcoming of water-holding agent salt tolerant alkaline resistance properties; Simultaneously in order to improve desert, saltings, the needed Soil structure of loess area plant-growth; Provide plant-growth required organic matter; The purpose of this invention is to provide a kind of cheapness; Gentle, the control easily of synthesis condition; Can effectively reduce the alkalescence of soil; Keep soil water content; Effectively reduce free sodium ion and heavy metal ion in the salt affected soil, improve a kind of salt tolerant alkali functional type water-holding agent and preparation method thereof of the physics and chemistry structure of soil.
A kind of salt tolerant alkali functional type water-holding agent provided by the invention is sulfonation humic acid, N, N '-methylene-bisacrylamide and acrylic acid graft copolymer; The prescription of water-holding agent is sulfonation humic acid: N; N '-methylene-bisacrylamide (MBA): ammonium persulphate-ammonium bisulfite initiator: acrylic acid mass ratio is: 2-10: 0.1-1: 0.01-10: 100, and preferred mass is than being 4-8: 0.1-0.4: 1-2: 100; Its structural formula is:
Wherein, R
1, R
2, R
3Independently be hydroxyl, enol base, sulfonic group, methoxyl group, carboxyl, amino, quinone oxygen base or semiquinone base respectively;
Described ammonium persulphate-ammonium bisulfite initiator system, the mol ratio of ammonium persulphate and ammonium bisulfite are 3: 1;
Described sulfonation humic acid is prepared by following method: count by weight; Getting 100-200 part humic acid puts into thermometer is housed; Dropping funnel; In the four-hole reactor of electronics agitator and condensation reflux unit; The potassium hydroxide solution that adds 0.01mol/L; Stir; Humic acid is dissolved fully, and dripping 60-200 part mass percentage concentration with the speed of 5mL/min is 25% sodium sulfite solution, stirs; 80-100 ℃ of reaction 1-3h; Be cooled to room temperature, using the dilute hydrochloric acid adjusting pH value of 0.1mol/L is 3, drying; Grinding obtains the sulfonation humic acid, and water ratio is 5-10%.
The present invention provides a kind of synthesis method of salt tolerant alkali functional type water-holding agent, and step and condition are following:
(1) the sulfonation humic acid is put into reactor, use concentration to be the dissolving of 0.01mol/L potassium hydroxide solution, obtaining mass percentage concentration is 10-30% sulfonated humic acid potassium solution;
(2) by proportioning, the sulfonated humic acid potassium solution of gained is put into reactor, the speed of vinylformic acid with 10mL/min is added drop-wise in the reactor; Stir, the adding massfraction is 20% potassium hydroxide solution, and the pH value in the solution is neutralized 4; Stir, mixed solution is cooled to normal temperature;
(3) in mixed solution, add linking agent, initiator successively, normal-temperature reaction 2-5 hour, become thick can't the stirring to solution till; Take out gains; Put into thermostatic drying chamber and dry to constant weight for 60 ℃, pulverize, obtain chocolate vesicular particle salt tolerant alkali functional type water-holding agent; Said vinylformic acid is chemical pure or technical grade, removes stopper with charcoal absorption; Said potassium hydroxide solution is that massfraction is 20% potassium hydroxide solution; Described linking agent is N, N '-methylene-bisacrylamide, and technical grade adds deionized water and is mixed with the solution that massfraction is 2-4%; Described initiator is ammonium persulphate-ammonium bisulfite initiator system, and the mol ratio of ammonium persulphate and ammonium bisulfite is 3: 1, and ammonium persulphate and ammonium bisulfite are technical grade.
Principle of the present invention is: at first under the effect of initiator and linking agent, by potassium hydroxide part neutral vinylformic acid polymerization reaction take place in solution, carry out crosslinked between the polymer chain.Then contain highly active phenolic hydroxyl group in the humic acids; When High hydrophilous resin is carried out grafting; Phenolic hydroxyl group can with the carboxyl generation condensation reaction in the water-absorbing resin; Produce aryl ester; Because have a plurality of phenolic hydroxyl groups on the same molecule of humic acids, above-mentioned condensation reaction has just formed further crosslinking structure.Available reaction formula is described as:
Beneficial effect: 1. a kind of salt tolerant alkali functional type water-holding agent provided by the invention is sulfonation humic acid, N; N '-methylene-bisacrylamide and acrylic acid graft copolymer; Extremely strong salt tolerant alkalescence is arranged, and inhaling the tap water multiple is 123 times, and the multiple of inhaling the sodium carbonate brine of pH=9 is 85 times.The yield of a kind of salt tolerant alkali of the present invention functional type water-holding agent is 83.50%.
2. the present invention provides a kind of salt tolerant alkali functional type water-holding agent; Sulfonic introducing has adsorptivity and influence of surfactant; Make the water-holding agent resin be dispersed in the water rapidly and uniformly; Effectively adsorb SOIL FREE sodium ion and heavy metal ion; Can effectively reduce the alkalescence of soil; Through ion-exchange and adsorption, reduce the content of SOIL FREE sodium ion and heavy metal ion simultaneously, thereby improve the physics and chemistry structure of soil.
3. the present invention provides a kind of salt tolerant alkali functional type water-holding agent, adopts the preparation of polymerized at normal temperature method, and it is simple to have technology, and reaction conditions is gentle, characteristics such as the easy control of reaction.
4. to adopt vinylformic acid and the humic acids be easy to get be main raw material in the present invention; The raw material that uses contains the necessary element of various plants growth; Can replenish element and organic matters such as the required potassium of plant-growth, nitrogen, the sulfonated humic acid that contains in the resin can slowly discharge, thereby promotes the growth of plant.
Description of drawings
Fig. 1 is the infrared spectrogram of a kind of salt tolerant alkali of the present invention functional type water-holding agent.Table 1 is the analysis of the infrared spectrogram of a kind of salt tolerant alkali of the present invention functional type water-holding agent.
The infrared spectra map analysis of table 1 salt tolerant alkali functional type water-holding agent
The infrared spectrogram of table 1 couple Fig. 1 is analyzed.In the infrared spectrogram of Fig. 1,1293cm
-1Charateristic avsorption band for the alkyl aromatic ester.This is because the condensation reaction that carboxyl on the High hydrophilous resin and the phenolic hydroxyl group in the sulfonation humic acid take place generates, and illustrates graft reaction has taken place, and has formed the salt tolerant alkali functional type water-holding agent of netted crosslinking structure.
Embodiment
Embodiment 1
(1) its prescription is: 6g sulfonated humic acid, 0.2g linking agent N, N '-methylene-bisacrylamide (MBA), 1.0g ammonium persulphate-ammonium bisulfite initiator, 100g vinylformic acid.
Sulfonation humic acid method for making is following: count by weight; Getting 120 parts of humic acid puts into thermometer is housed; Dropping funnel; In the four-hole reactor of electronics agitator and condensation reflux unit; The potassium hydroxide solution that adds 0.01mol/L; Stir; Humic acid is dissolved fully, and the 100 parts of sodium sulfite solutions of speed dropping with 5mL/min stir; 100 ℃ of reaction 3h; Be cooled to room temperature, using the dilute hydrochloric acid adjusting pH value of 0.1mol/L is 3, drying; Grinding obtains the sulfonation humic acid, and the mass percentage concentration of said sodium sulfite solution is 25%; Described initiator is ammonium persulphate-ammonium bisulfite initiator system, and the mol ratio of ammonium persulphate and ammonium bisulfite is 3: 1;
(2) the present invention provides a kind of synthesis method of salt tolerant alkali functional type water-holding agent, and step and condition are following:
(1) the sulfonation humic acid is put into reactor, use concentration to be the dissolving of 0.01mol/L potassium hydroxide solution, obtaining mass percentage concentration is 20% sulfonated humic acid potassium solution;
(2) by proportioning, the sulfonated humic acid potassium solution of gained is put into reactor, the speed of vinylformic acid with 10mL/min is added drop-wise in the reactor; Stir, the adding massfraction is 20% potassium hydroxide solution, and the pH value in the solution is neutralized 4; Stir, mixed solution is cooled to normal temperature;
(3) in mixed solution, add linking agent, initiator successively, normal-temperature reaction 2 hours, become thick can't the stirring to solution till; Take out gains; Put into thermostatic drying chamber and dry to constant weight for 60 ℃, pulverize, obtain chocolate vesicular particle salt tolerant alkali functional type water-holding agent.Said vinylformic acid: chemical pure or technical grade, remove stopper with charcoal absorption; Said potassium hydroxide solution is that massfraction is 20% potassium hydroxide solution; Described linking agent is N, N '-methylene-bisacrylamide (MBA), and technical grade, using deionized water to be mixed with massfraction is 4% solution; Described initiator is ammonium persulphate-ammonium bisulfite initiator system, and the mol ratio of ammonium persulphate and ammonium bisulfite is 3: 1, and ammonium persulphate and ammonium bisulfite are technical grade.
1. the present invention provides a kind of salt tolerant alkali functional type water-holding agent, is sulfonated humic acid-polyacrylic water-absorbing resin, and extremely strong salt tolerant alkalescence is arranged, and inhaling the tap water multiple is 123 times, and the multiple of inhaling the sodium carbonate brine of pH=9 is 85 times.
Embodiment 2-8
The proportioning of a kind of salt tolerant alkali functional type water-holding agent that embodiment 2-8 provides and preparing method's reaction times such as table 2, remaining is with embodiment 1.Liquid absorbency rate is as shown in table 2.
Quality proportioning, reaction times and the liquid absorbency rate table of table 2 salt tolerant alkali functional type water-holding agent
Claims (3)
1. a salt tolerant alkali functional type water-holding agent is characterized in that it is sulfonation humic acid, N, N '-methylene-bisacrylamide and acrylic acid graft copolymer; The prescription of water-holding agent is sulfonation humic acid: N, N '-methylene-bisacrylamide: ammonium persulphate-ammonium bisulfite initiator system: acrylic acid mass ratio is: 2-10: 0.1-1: 0.01-10: 100; Its structural formula is:
Wherein, R
1, R
2, R
3Independently be hydroxyl, enol base, sulfonic group, methoxyl group, carboxyl, amino, quinone oxygen base or semiquinone base respectively;
Described ammonium persulphate-ammonium bisulfite initiator system, the mol ratio of ammonium persulphate and ammonium bisulfite are 3: 1;
Described sulfonation humic acid is prepared by following method: count by weight; Getting 100-200 part humic acid puts into thermometer is housed; Dropping funnel; In the four-hole reactor of electronics agitator and condensation reflux unit; The potassium hydroxide solution that adds 0.01mol/L; Stir; Humic acid is dissolved fully, and dripping 60-200 part mass percentage concentration with the speed of 5mL/min is 25% sodium sulfite solution, stirs; 80-100 ℃ of reaction 1-3h; Be cooled to room temperature, using the dilute hydrochloric acid adjusting pH value of 0.1mol/L is 3, drying; Grinding obtains the sulfonation humic acid, and water ratio is 5-10%.
2. a kind of salt tolerant alkali functional type water-holding agent as claimed in claim 1; It is characterized in that; The prescription of water-holding agent is sulfonation humic acid: N, N '-methylene-bisacrylamide: ammonium persulphate-ammonium bisulfite initiator system: acrylic acid mass ratio is 4-8: 0.1-0.4: 1-2: 100.
3. the preparation method of a kind of salt tolerant alkali functional type water-holding agent as claimed in claim 1 is characterized in that step and condition are following:
(1) the sulfonation humic acid is put into reactor, use concentration to be the dissolving of 0.01mol/L potassium hydroxide solution, obtaining mass percentage concentration is 10-30% sulfonated humic acid potassium solution;
(2) by proportioning, the sulfonated humic acid potassium solution of gained is put into reactor, the speed of vinylformic acid with 10mL/min is added drop-wise in the reactor; Stir, the adding massfraction is 20% potassium hydroxide solution, and the pH value in the solution is neutralized 4; Stir, mixed solution is cooled to normal temperature;
(3) in mixed solution, add linking agent, initiator successively, normal-temperature reaction 2-5 hour, become thick can't the stirring to solution till; Take out gains; Put into thermostatic drying chamber and dry to constant weight for 60 ℃, pulverize, obtain chocolate vesicular particle salt tolerant alkali functional type water-holding agent; Said vinylformic acid is chemical pure or technical grade, removes stopper with charcoal absorption; Said potassium hydroxide solution is that massfraction is 20% potassium hydroxide solution; Described linking agent is N, N '-methylene-bisacrylamide, and technical grade adds deionized water and is mixed with the solution that massfraction is 2-4%; Described initiator is ammonium persulphate-ammonium bisulfite initiator system, and the mol ratio of ammonium persulphate and ammonium bisulfite is 3: 1, and ammonium persulphate and ammonium bisulfite are technical grade.
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| CN103539952A (en) * | 2012-07-10 | 2014-01-29 | 厦门大学 | Novel humic acid sulfonatiion process |
| CN105254454A (en) * | 2015-11-23 | 2016-01-20 | 江苏省农业科学院 | Rapid water-storage and fertilization compound material for hill soil and preparation method of rapid water-storage and fertilization compound material |
| CN105802638A (en) * | 2016-05-16 | 2016-07-27 | 农业部规划设计研究院 | Biological-carbon-based water retaining agent and preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103539952A (en) * | 2012-07-10 | 2014-01-29 | 厦门大学 | Novel humic acid sulfonatiion process |
| CN105254454A (en) * | 2015-11-23 | 2016-01-20 | 江苏省农业科学院 | Rapid water-storage and fertilization compound material for hill soil and preparation method of rapid water-storage and fertilization compound material |
| CN105802638A (en) * | 2016-05-16 | 2016-07-27 | 农业部规划设计研究院 | Biological-carbon-based water retaining agent and preparing method thereof |
| WO2018137596A1 (en) * | 2017-01-24 | 2018-08-02 | 福州大学 | Method for preparing thinned ceramic additive using refuse leachate |
| US10759686B2 (en) | 2017-01-24 | 2020-09-01 | Fuzhou University | Method for preparing thinning ceramic additive using landfill leachate |
| JP2019531895A (en) * | 2017-01-24 | 2019-11-07 | 福州大学 | Preparation method of thinning ceramic additive using waste leachate |
| CN107552009A (en) * | 2017-09-27 | 2018-01-09 | 安徽金叶碳素科技有限公司 | Recyclable soil heavy mental adsorbent of a kind of magnetic and preparation method thereof |
| CN107794048A (en) * | 2017-09-27 | 2018-03-13 | 安徽金叶碳素科技有限公司 | A kind of attapulgite/lignite compounding absorbent-type soil oxygenation agent and preparation method thereof |
| CN107602780A (en) * | 2017-09-27 | 2018-01-19 | 安徽金叶碳素科技有限公司 | A kind of lignite humic acid base super absorbent resin epoxy-type agricultural water-loss reducer and preparation method thereof |
| CN111587282A (en) * | 2018-02-11 | 2020-08-25 | 北京紫光英力化工技术有限公司 | Use of biobased sulfonates as nutrient sources and conditioners |
| CN108948293A (en) * | 2018-06-15 | 2018-12-07 | 陕西省土地工程建设集团有限责任公司 | A kind of humic acid base compound water retaining agent and preparation method thereof |
| CN108948293B (en) * | 2018-06-15 | 2021-02-26 | 陕西省土地工程建设集团有限责任公司 | Humic acid-based composite water-retaining agent and preparation method thereof |
| CN116082095A (en) * | 2023-02-24 | 2023-05-09 | 新疆锦华农药有限公司 | Long-acting stable humic acid water-soluble fertilizer and preparation method thereof |
| CN116082095B (en) * | 2023-02-24 | 2024-02-02 | 新疆锦华农药有限公司 | Long-acting stable humic acid water-soluble fertilizer and preparation method thereof |
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Application publication date: 20120215 |