CN102875727A - Preparation method for micro-crystal muscovite compounded and crylic acid-acrylamide-itaconic acid polymerized super absorbent resin - Google Patents
Preparation method for micro-crystal muscovite compounded and crylic acid-acrylamide-itaconic acid polymerized super absorbent resin Download PDFInfo
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Abstract
The invention relates to a preparation method for a micro-crystal muscovite compounded and crylic acid-acrylamide-itaconic acid polymerized super absorbent resin. The method comprises the following steps of: neutralizing crylic acid and acrylamide monomers in a mass ratio of (1-5):1 by using NaOH, wherein the molar ratio of the crylic acid and acrylamide monomers to NaOH is 1:(0.5-0.8); adding micro-crystal muscovite in an amount which is 20 to 80 percent based on the total mass of the crylic acid and acrylamide monomers, uniformly stirring to form stable suspension, and then adding acrylamide and a cross-linking agent in an amount which is 0.1 to 0.8 percent based on the total mass of the crylic acid, itaconic acid and acrylamide monomers, wherein the mass ratio of the crylic acid monomer to the itaconic acid monomer to the acrylamide monomer is (1-5):1:(1-5),and heating to 50 to 80 DEG C; adding redox initiator in an amount which is 0.1 to 2.0 percent based on the total mass of the crylic acid, itaconic acid and acrylamide monomers to initiate polymerization; and after polymerization is finished, precipitating, washing and drying to obtain the micro-crystal muscovite compounded and crylic acid-acrylamide-itaconic acid polymerized super absorbent resin. The resin has the advantages of strong water absorbing capacity, high salt absorbing performance, high gel strength, high water retention capacity and the like.
Description
Technical field
The present invention relates to the preparation method of compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of a kind of microcrystal muscovite, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of the microcrystal muscovite of the present invention's preparation is applicable to agricultural gardening Bao Shui ﹑ soil improvement, Zhi tree Zao Lin ﹑ deserted mountain transformation and the desert afforestation etc. of the industries such as farming, woods.
Background technology
Super absorbent resin is a kind of polymkeric substance that contains the hydrophilic radicals such as carboxyl, hydroxyl and have certain degree of crosslinking, it is water insoluble, also be insoluble to organic solvent, have the characteristics such as water-intake rate is high, water-retentivity is strong, absorption speed is fast, gel-strength is large, thereby be widely applied in fields such as articles for daily use, agricultural, industry, building, health cares, can say " there is its ample scope for abilities in every field relevant with water ".
In the medical and hygiene article field, utilize super absorbent resin to make absorbing material, as defend living towel ﹑ baby and urinate the medical absorbent cotton of cloth ﹑ etc., its consumption accounts for more than 95% of all super absorbent resin annual production.At building field, the water-resisting layer that can be used for anti-seep water in the construction work and underwater pipeline by the sealing material that Xiang Jiao ﹑ super absorbent resin and auxiliary agent etc. are mixed to get is made.In the agroforestry field, no matter be water or water-soluble thing, such as fertilizer, agricultural chemicals, root-growing agent, even cold and hot amount can both be stored and slowly-releasing at super absorbent resin molecule grid, therefore can greatly improve the utilization ratio of rainwater and irrigation water, reduce fertilizer and agricultural chemicals and run off, alleviate environmental pollution.Super absorbent resin has function and the slowly-releasing root-growing agent of activation phosphorus, more can urge root, therefore after using water-holding agent, root system is particularly flourishing, particularly fibrous root.The super absorbent resin large water gaging of can attracting deposits has reduced the variation of edatope temperature, the certain insulation effect of tool also, i.e. cooling in summer, Winter protection.Super absorbent resin contraction and imbibition repeatedly causes a large amount of holes to soil, ventilation property, the water-permeable of soil have been improved, improved rhizospheric environment, also strengthened simultaneously the activity of rhizospheric microorganism, accelerate the rhizosphere decomposition of humatite matter on every side, be conducive to Root Absorption, promoted growing of root system and plant, improved soil matrix, kept soil from packing together.The super absorbent resin that adds 0.1wt% in the soil can make soil have in a long time suff water to provide plants to need, and improves crop yield.In the Gai Zao ﹑ desert afforestation of Zhi tree Zao Lin ﹑ deserted mountain, can utilize super absorbent resin to keep soil moisture to improve plant germination rate and surviving rate.Super absorbent resin also has increasing application at artificial snow Zao ﹑ processed perfume Huan Shi ﹑ Shi product Tian Jia ﹑ fresh-keeping of vegetables etc. in addition.
The Composite of material is the trend of development, and is mutually compound by multiple material, can realize performance optimization and complementation, remedies some shortcoming of single-material, therefore compares with single-material, and composite material combination property is better.The organic and inorganic composite highly-absorbent resin has become one of present study hotspot in recent years, the compound High hydrophilous resin of a series of wilkinites, kaolin, illite, sericite and diatomite occurred.Microcrystal muscovite (Microcrystal muscovite) is a kind of novel white mica mineral wealth with microlitic structure (crystallographic dimension is 1 μ m～10 μ m approximately) of discovered in recent years.Microcrystal muscovite how in the form of sheets, en plaque, flakey, certain radius-thickness ratio is arranged, and the toughness of sheet mica and good springiness, slip ability are large, tension, ultimate compression strength are high, simultaneously acid and alkali-resistance, protection against corrosion, thermal expansivity is little, resistance toheat good, can shielding ultraviolet rays and ir radiation.When using in rubber, plastics as filler, because its special microtexture, good physicals can when reducing material cost simultaneously, be improved the mechanical property of high polymer material.Have than the low-dielectric loss because of it again, anti-electric-arc, anti-corona, insulation strength is high, can be used as functional stuffing, improves the electric property of material.But because crystal grain is little, crystallization degree is high, and activity group content is few, is not easy modification, and therefore the at present high added value development and use research of microcrystal muscovite in High hydrophilous resin is less.Patent of invention (patent No. ZL2010102221941) is with vinylformic acid, acrylamide and Sodium styrene sulfonate are comonomer, adopt aqueous solution polymerization to prepare microcrystal muscovite composite sulfonic acid type High hydrophilous resin, water-intake rate and salt absorbing rate reach respectively 780～1150 times and 80～140 times, temperature resistance is greater than 220 ℃, patent of invention (patent No. ZL201010222180X) is take 2-hydroxy-2-methyl-1-phenyl-1-propyl group ketone or michaelis ketone and benzophenone mixed light initiator as light trigger, vinylformic acid, acrylamide and Sodium styrene sulfonate are comonomer, the photopolymerization of room temperature original position prepares microcrystal muscovite composite sulfonic acid type High hydrophilous resin, and water-intake rate and salt absorbing rate reach respectively 380～560 times and 50～70 times.More wait on the Shen take the superfine powder of microcrystal muscovite and vinylformic acid as main raw material, adopt solution polymerization process to prepare microcrystal muscovite/sodium polyacrylate superabsorbency matrix material, inhaling the distilled water multiplying power is 420 g/g, inhaling the tap water multiplying power is 220 g/g, inhaling the physiological saline multiplying power is 55 g/ g, up to the present is that the research that comonomer prepares the microcrystal muscovite composite highly-absorbent resin yet there are no report both at home and abroad with vinylformic acid, acrylamide and methylene-succinic acid.
Summary of the invention
In view of this, purpose of the present invention is exactly in the preparation method that compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of a kind of microcrystal muscovite is provided.Methylene-succinic acid is a kind of unsaturated dicarboxylic acid, generally is to adopt cheap starch, and sucrose, molasses, the agricultural byproducts such as wood chip and straw are starting material, select suitable bacterial classification to produce through biological fermentation.Increasingly mature along with fermentation technique, the production cost of methylene-succinic acid is also more and more lower, and its wide material sources, environmentally friendly, do not rely on petroleum resources.Methylene-succinic acid has two carboxyls that wetting ability is stronger, therefore introduce biodegradable, gel-strength, water-intake rate and the salt absorbing rate that the 3rd monomer methylene-succinic acid and acrylamide, acrylic acid copolymer can further improve High hydrophilous resin, obtain compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of better, the eco-friendly microcrystal muscovite of water-intake rate, salt absorbing rate and gel-strength.
According to purpose of the present invention, the method for compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of a kind of microcrystal muscovite has been proposed, its feature has following processing step:
A) a certain amount of solid NaOH is dissolved in the 200mL deionized water, then in ice bath, vinylformic acid and methylene-succinic acid slowly are added drop-wise in the NaOH aqueous solution, fully stir, reaction 0.5～2h, then add microcrystal muscovite, 30～60 ℃ of uniform stirring 2～24h form stable suspension; The mass ratio of vinylformic acid and methylene-succinic acid is 1～5:1, and the mol ratio of vinylformic acid and methylene-succinic acid monomer and NaOH is 1:0.5～0.8, and microcrystal muscovite accounts for 20～80% of vinylformic acid and methylene-succinic acid monomer mass total amount;
B) in above-mentioned suspension, add acrylamide and linking agent, fully stir 30min, be warming up to 50～60 ℃, then redox initiator slowly is added drop-wise in the polymerization system initiated polymerization 2～4 hours; The mass ratio of vinylformic acid and acrylamide is 1～5:1～5; Linking agent accounts for 0.1～0.8% of vinylformic acid, methylene-succinic acid and acrylamide monomer quality total amount; Redox initiator accounts for 0.1%～2.0% of vinylformic acid, methylene-succinic acid and acrylamide monomer quality total amount;
C) compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of synthetic microcrystal muscovite is precipitated with ethanol, washing with alcohol 2～3 times, 70～110 ℃ of oven dry, pulverize and namely get particulate state, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of lurid microcrystal muscovite, equilibrium water absorption and balance salt absorbing rate can reach respectively 500～1300 times and 40～100 times, and the water-intake rate of 20min and salt absorbing rate can reach respectively 50～80% of equilibrium water absorption and balance salt absorbing rate.The gel-strength of water absorbent gel reaches 3～10Pa.s, and the water retention behind 80～90 ℃ of dry 200min of water absorbent gel is 30～50%.
Linking agent used in the present invention is selected from N, N '-methylene-bisacrylamide, ethylene glycol diacrylate, diethylene glycol double methacrylate, tirethylene glycol double methacrylate, 1,3-PD double methacrylate, Viscoat 295, pentaerythritol triacrylate, glycidyl methacrylate and polyethyleneglycol diacrylate.
Redox initiator used in the present invention comprises Oxidizing and Reducing Agents, and the mol ratio of Oxidizing and Reducing Agents is 1～2:1.Oxygenant is selected from ammonium persulphate, Potassium Persulphate and Sodium Persulfate, and reductive agent is selected from sodium bisulfite, S-WAT, Sulfothiorine, ferrous sulfate and formaldehyde and closes Sodium Thiosulfate.
Advantage of the present invention and effect are:
1) reaction is directly carried out in the aqueous solution, non-environmental-pollution, and method is simple, need not nitrogen protection, therefore saved the nitrogen device, reduced the Meteorological of equipment;
2) introduce biodegradable, gel-strength, water-intake rate and the salt absorbing rate that the 3rd monomer methylene-succinic acid and acrylamide, acrylic acid copolymer have further improved High hydrophilous resin;
3) compare with normally used acrylic acid-acrylamide High hydrophilous resin, owing to having added microcrystal muscovite, salt tolerance, thermotolerance and the gel-strength of High hydrophilous resin have been improved, also reduced cost, further expanded simultaneously the Application Areas of microcrystal muscovite, improved the added value of microcrystal muscovite, for the Sustainable development of China's agricultural and the aspects such as improvement in desert and saltings great meaning has been arranged.
The measuring method of water-intake rate, salt absorbing rate, water-retentivity and the gel-strength of compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of microcrystal muscovite of the present invention is as follows.
Water-intake rate is measured:
Compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of microcrystal muscovite that is cut into certain particle size that takes a morsel is put into baking oven, about 110 ℃ of baking 2h, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of the dry microcrystal muscovite of accurate weighing 0.5g, put into the beaker of 1000mL, then add 1000mL distilled water, at ambient temperature fully suction, water-absorbing resin is water white transparency shape jelly.Filter with 100 order stainless steel sifts, adopt the natural filtration method to measure, to substantially anhydrous drippage.Measure the quality of water after filtering, calculate water-intake rate according to following formula.
Salt absorbing rate is measured:
Compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of microcrystal muscovite that takes by weighing the 0.5g drying is put into beaker, adding 500mL concentration is 0.9% the NaCl aqueous solution, at room temperature leave standstill suction, reach the unnecessary salt solution of saturated rear filtering, and claim its quality, calculate salt absorbing rate according to following formula.
The mensuration of water retention property:
Compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin water absorbent gel of microcrystal muscovite after fully absorbing water is placed culture dish, (80-90 ℃) oven drying at a certain temperature, survey at regular intervals its quality, calculate water retention according to following formula.
The mensuration of gel-strength:
Compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of microcrystal muscovite that takes a morsel and pulverize, put into baking oven, baking under 100 ℃ of temperature condition about 3 hours, accurately take by weighing compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of microcrystal muscovite dry about 0.2g, put into the beaker of 500mL, then add 300mL distilled water, at ambient temperature fully suction, after gelinite reaches the suction balance, filter out the not water of absorption with 100 order stainless steel sifts, to anhydrous drippage, then adopt the apparent viscosity of rotary viscosity design determining water absorbent gel body, be the gel-strength of compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin water absorbent gel body of microcrystal muscovite.
Four, embodiment
In order to understand better the present invention, further set forth content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
1.82g NaOH is dissolved in the 200mL deionized water, then in ice bath, 4.80g vinylformic acid and 1.20g methylene-succinic acid slowly is added drop-wise in the NaOH aqueous solution, fully stir, reaction 2h, then add the 4.50g microcrystal muscovite, 40 ℃ of uniform stirring 10h form stable suspension.In above-mentioned suspension, add 24.00g acrylamide and 0.12g
N,
N'-methylene-bisacrylamide fully stirs 30min, is warming up to 50 ℃, then 0.18g ammonium persulphate and 0.06g sodium bisulfite slowly is added drop-wise in the polymerization system initiated polymerization 4 hours.React and compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of synthetic microcrystal muscovite is precipitated with ethanol after complete, washing with alcohol 3 times, 100 ℃ of oven dry, pulverize and namely get particulate state, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of lurid microcrystal muscovite, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) the High hydrophilous resin equilibrium water absorption of microcrystal muscovite and balance salt absorbing rate can reach respectively 1250 times and 90 times, the water-intake rate of 20min and salt absorbing rate can reach respectively 80% and 70% of equilibrium water absorption and balance salt absorbing rate, the gel-strength of water absorbent gel reaches 9.5Pa.s, and the water retention behind 90 ℃ of dry 200min of water absorbent gel is 50%.
Embodiment 2:
2.60g NaOH is dissolved in the 200mL deionized water, then in ice bath, 6.3g vinylformic acid and 2.7g methylene-succinic acid slowly is added drop-wise in the NaOH aqueous solution, fully stir, reaction 1.5h, then add the 3g microcrystal muscovite, 50 ℃ of uniform stirring 5h form stable suspension.In above-mentioned suspension, add 21g acrylamide and 0.09g
N,
N'-methylene-bisacrylamide fully stirs 30min, is warming up to 55 ℃, then 0.22g Potassium Persulphate and 0.08g sodium bisulfite slowly is added drop-wise in the polymerization system initiated polymerization 4 hours.React and compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of synthetic microcrystal muscovite is precipitated with ethanol after complete, washing with alcohol 3 times, 100 ℃ of oven dry, pulverize and namely get particulate state, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of lurid microcrystal muscovite, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) the High hydrophilous resin equilibrium water absorption of microcrystal muscovite and balance salt absorbing rate can reach respectively 950 times and 80 times, the water-intake rate of 20min and salt absorbing rate can reach respectively 75% and 66% of equilibrium water absorption and balance salt absorbing rate, the gel-strength of water absorbent gel reaches 8.3Pa.s, and the water retention behind 90 ℃ of dry 200min of water absorbent gel is 43%.
Embodiment 3:
5.39g NaOH is dissolved in the 200mL deionized water, then in ice bath, 11.20g vinylformic acid and 4.80g methylene-succinic acid slowly is added drop-wise in the NaOH aqueous solution, fully stir, reaction 1h, then add the 5g microcrystal muscovite, 50 ℃ of uniform stirring 5h form stable suspension.In above-mentioned suspension, add 24g acrylamide and 0.14g
N,
N'-methylene-bisacrylamide fully stirs 30min, is warming up to 50 ℃, then 0.26g ammonium persulphate and 0.09g sodium bisulfite slowly is added drop-wise in the polymerization system initiated polymerization 4 hours.React and compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of synthetic microcrystal muscovite is precipitated with ethanol after complete, washing with alcohol 3 times, 100 ℃ of oven dry, pulverize and namely get particulate state, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of lurid microcrystal muscovite, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) the High hydrophilous resin equilibrium water absorption of microcrystal muscovite and balance salt absorbing rate can reach respectively 900 times and 62 times, the water-intake rate of 20min and salt absorbing rate can reach respectively 72% and 62% of equilibrium water absorption and balance salt absorbing rate, the gel-strength of water absorbent gel reaches 8.6Pa.s, and the water retention behind 90 ℃ of dry 200min of water absorbent gel is 46%.
Embodiment 4:
4.87g NaOH is dissolved in the 200mL deionized water, then in ice bath, 14.4g vinylformic acid and 3.6g methylene-succinic acid slowly is added drop-wise in the NaOH aqueous solution, fully stir, reaction 1.2h, then add the 5.4g microcrystal muscovite, 50 ℃ of uniform stirring 5h form stable suspension.In above-mentioned suspension, add 18g acrylamide and 0.11g
N,
N'-methylene-bisacrylamide fully stirs 30min, is warming up to 55 ℃, then 0.27g Potassium Persulphate and 0.09g sodium bisulfite slowly is added drop-wise in the polymerization system initiated polymerization 4 hours.React and compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of synthetic microcrystal muscovite is precipitated with ethanol after complete, washing with alcohol 3 times, 100 ℃ of oven dry, pulverize and namely get particulate state, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of lurid microcrystal muscovite, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) the High hydrophilous resin equilibrium water absorption of microcrystal muscovite and balance salt absorbing rate can reach respectively 780 times and 56 times, the water-intake rate of 20min and salt absorbing rate can reach respectively 65% and 60% of equilibrium water absorption and balance salt absorbing rate, the gel-strength of water absorbent gel reaches 7.2Pa.s, and the water retention behind 90 ℃ of dry 200min of water absorbent gel is 36%.
Claims (3)
1. the preparation method of compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of a microcrystal muscovite is characterized in that having following processing step:
A) a certain amount of solid NaOH is dissolved in the 200mL deionized water, then in ice bath, vinylformic acid and methylene-succinic acid slowly is added drop-wise in the NaOH aqueous solution, fully stir, reaction 0.5～2h, then add microcrystal muscovite, 30～60 ℃ of uniform stirring 2～24h form stable suspension; The mass ratio of vinylformic acid and methylene-succinic acid is 1～5:1, and the mol ratio of vinylformic acid and methylene-succinic acid monomer and NaOH is 1:0.5～0.8, and microcrystal muscovite accounts for 20～80% of vinylformic acid and methylene-succinic acid monomer mass total amount;
B) in above-mentioned suspension, add acrylamide and linking agent, fully stir 30min, be warming up to 50～60 ℃, then redox initiator slowly is added drop-wise in the polymerization system initiated polymerization 2～4 hours; The mass ratio of vinylformic acid and acrylamide is 1～5:1～5; Linking agent accounts for 0.1～0.8% of vinylformic acid, methylene-succinic acid and acrylamide monomer quality total amount; Redox initiator accounts for 0.1%～2.0% of vinylformic acid, methylene-succinic acid and acrylamide monomer quality total amount;
Compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of synthetic microcrystal muscovite is precipitated with ethanol, washing with alcohol c) 2～3 time, 70～110 ℃ of oven dry, pulverize and namely get particulate state, compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of lurid microcrystal muscovite, equilibrium water absorption and balance salt absorbing rate can reach respectively 500～1300 times and 40～100 times, and the water-intake rate of 20min and salt absorbing rate can reach respectively 50～80% of equilibrium water absorption and balance salt absorbing rate; The gel-strength of water absorbent gel reaches 3～10Pa.s, and the water retention behind 80～90 ℃ of dry 200min of water absorbent gel is 30～50%.
2. the preparation method of compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of a kind of microcrystal muscovite according to claim 1, it is characterized in that: described linking agent is selected from N, N '-methylene-bisacrylamide, ethylene glycol diacrylate, diethylene glycol double methacrylate, tirethylene glycol double methacrylate, 1,3-PD double methacrylate, Viscoat 295, pentaerythritol triacrylate, glycidyl methacrylate and polyethyleneglycol diacrylate.
3. the preparation method of compound poly-(acrylic acid-acrylamide-methylene-succinic acid) High hydrophilous resin of a kind of microcrystal muscovite according to claim 1, it is characterized in that: described redox initiator comprises Oxidizing and Reducing Agents, and the mol ratio of Oxidizing and Reducing Agents is 1～2:1; Oxygenant is selected from ammonium persulphate, Potassium Persulphate, Sodium Persulfate, and reductive agent is selected from sodium bisulfite, S-WAT, Sulfothiorine, ferrous sulfate and formaldehyde and closes Sodium Thiosulfate.
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| FR2939055A1 (en) * | 2008-12-03 | 2010-06-04 | Coatex Sas | Use of a mineral material, homopolymer or copolymer of acrylic acid, as dispersing agent and/or grinding aid agent, where the acrylic acid is obtained from glycerol |
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Application publication date: 20130116 |