CN103739784A - Diatomite composite super-absorbent resin material and preparation method thereof - Google Patents
Diatomite composite super-absorbent resin material and preparation method thereof Download PDFInfo
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- CN103739784A CN103739784A CN201410017583.9A CN201410017583A CN103739784A CN 103739784 A CN103739784 A CN 103739784A CN 201410017583 A CN201410017583 A CN 201410017583A CN 103739784 A CN103739784 A CN 103739784A
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Abstract
The invention belongs to the technical field of high polymer materials, and particularly relates to a diatomite composite super-absorbent resin material and a preparation method thereof. According to the invention, by adopting a self-exothermic crosslinking technology, and controlling the application amounts of reactants and the pH value of a polymer system, the room-temperature synthesis of super-absorbent resins is realized. The material and preparation method thereof disclosed by the invention are simple in preparation process, mild in conditions, free from nitrogen protection and heating and low in energy consumption. The source of raw materials used in the invention is wide, so that the resin material has obvious cost advantages, and has a board application prospect; obtained products are high in natural component starch and diatomite contents, environmental-friendly, and good in dispersibility, can achieve the functions of absorbing and holding water, storing drugs, improving the soil structure, and adjusting the temperature and humidity of soil, and can be applied to Chinese herbal medicines and agriculture, forestry and gardening.
Description
Technical field
The invention belongs to technical field of polymer materials.Be specifically related to compound super absorbent resin material of a kind of diatomite and preparation method thereof.
Background technology
Super absorbent resin (being called for short SAP) is that the class developing rapidly in recent years has good water suction and the new functional macromolecule material of water retention property, is widely used in the various fields such as agricultural gardening, physiological hygiene articles for use, medicine, oil, chemical industry, environmental protection, building materials and food.
The diatomite resource of China is abundant, and reserves are only second to the U.S., occupy the 2nd, the world.You Yi Jilin Province reserves are maximum, account for 54.8% of national reserves.Diatomite resource is mainly used as flocculating aids, heat-insulating heat-preserving material and functional stuffing etc. in China.In recent years, diatomite is causing extensive concern aspect biotechnology, medicine industry, non-toxic pesticide production.
Current China diatomite resource utilizes level not high, mainly take exploitation one-level diatomite as flocculating aids product as main.Carry out diatomite comprehensive utilizating research, widen diatomite Application Areas, improve its application added value, especially secondary and three grades of diatomaceous reasonable utilizations, there are ecological benefits significantly, can realize the coordinated development of the utilization of resources and environment optimization.
The physical strength of tradition agricultural high-hygroscopicity resin own is low, and anti-extraneous solution interference performance is poor, is subject to the such environmental effects such as ambient pressure, temperature larger, causes its water-holding slow-release effect to decline, and has greatly affected its effect.We,, for this problem, make improvements, and utilize first the abundant diatomite resource in Jilin Province, and super absorbent resin and tripolite compound are combined, and have synthesized the compound degradable macromolecule water-keeping material of yolk-eggshell structure diatomite.Use diatomite and traditional High hydrophilous resin compound, not only can reduce costs, and can effectively improve the gel-strength of resin, improve its salt tolerance and water retention property, can significantly improve SAP over-all properties.
Simple synthetic method of the present invention, has reduced cost, and economical efficiency is considerable.Thereby the scale operation that makes super absorbent resin is able to better realization.Also improve raw materials for production simultaneously, increased the physical strength of water-absorbing material, improved the performance of product, be more conducive to the application of product.
Summary of the invention
The object of the invention is compound super absorbent resin material of a kind of diatomite and preparation method thereof.
Technical scheme of the present invention comprises following concrete steps:
1). take the diatomite of 10～20 parts of mistake 300 mesh sieves, add suitable quantity of water, mix, standby;
2). in the mixed solution obtaining to step 1), add 40～80 parts of propenyl compounds, vinylformic acid or acrylamide, be at room temperature uniformly mixed 1～2 h, is configured to diatomite/propenyl compound presoma mixed solution;
3). take 20～40 weight part sodium hydrate solids, be mixed with sodium hydroxide solution;
4). under the condition constantly stirring, the sodium hydroxide solution that step 3) is obtained joins step 2) carry out neutralization reaction in diatomite/propenyl compound presoma mixed solution of obtaining, question response completely after, stop stirring and make neutralizer cooling gradually;
5). under mechanical stirring condition, the starch of certain mass is joined to the step 4 that is cooled to certain temperature) in the mixed solution that obtains, continue to stir 30～60min, starch is uniformly dispersed;
6). respectively the initiator potassium persulfate having prepared and linking agent MBA solution are slowly added to step 5) in the reaction solution that obtains, continue to stir 1～1.5h, reaction solution fades to translucent viscous fluid;
7). in the mixed solution obtaining to step 6), add a certain amount of ammoniacal liquor, system pH is adjusted between 7～8; After static 10～15min, system reaction, emits gas to completing;
8). the product that step 7) is obtained is processed into little bulk, 100
oin C thermostatic drying chamber, be dried to constant weight; Through broken, pulverizing, obtain particle or Powdered silicon-dioxide/SAP composite high-water uptake material.
The temperature of reaction system is in the scope of 20-40 ℃, and the weight proportion between raw material is: diatomite 2-15g, Semen Maydis powder 3-20g, propenyl compound acrylic acid or acrylamide 40-60g, sodium hydroxide 20-30g, initiator 0.35-1.6g, linking agent 0.1-0.8g and 25% ammoniacal liquor 10-20ml.
Accompanying drawing explanation
The technological process block-diagram that accompanying drawing 1 is prepared for the compound high absorbency material of diatomite;
Accompanying drawing 2 is diatomite SEM photo;
Accompanying drawing 3 is the compound high absorbency material SEM of diatomite photo.
Embodiment
Take diatomite original soil 50 g, under 600 ℃ of high temperature, calcine 2 h, after being down to room temperature, this pressed powder is added in 70 % aqueous sulfuric acids, be uniformly mixed 4 h, after washing more after filtration,, oven dry, this pressed powder is dropped in the CTAB aqueous solution of 200 mL 2%, 60 ℃ of constant temperature stir 2 h, more after filtration, washing, dry, solid is crossed to 200 mesh sieves after pulverizing.
Compound concentration is 26% sodium hydroxide solution 16 mL, slowly joins in the vinylformic acid of 10 mL after cool to room temperature, constantly stirs and makes to react completely.Under the condition constantly stirring, 3 g modification infusorial earth powder are joined in neutralizer, stir 30 min, it is uniformly dispersed.
With prolong, temperature is taken into account in 250 mL tetra-neck flasks of nitrogen conduit, adds 50 mL hexanaphthenes and 1.5 g dispersion agents (Span 60), and logical nitrogen 20 min, remove the oxygen in solution.Four-necked bottle is put in 40 ℃ of oil baths and mixes 30min under mechanical stirring subsequently.To be mixed evenly after, successively appropriate aforesaid propylene acid/diatomite mixing solutions, 0.1 g initiator (Potassium Persulphate) and 0.1 g linking agent (MBA) are added in flask successively, stir after 30 min, be warming up to 70 ℃, react 2.5 h, after having reacted, heating installation is turned off, be stirred to solution always and be cooled to room temperature, then reaction solution suction filtration is separated, with deionized water wash, resulting white precipitate is dry 24 h in 100 ℃ of vacuum drying ovens, obtain diatomite/super absorbent resin Material cladding macromolecular material.
Specific embodiment 2
Take diatomite original soil 100 g, under 700 ℃ of high temperature, calcine 3 h, after being down to room temperature, this pressed powder is added in 75 % aqueous sulfuric acids, be uniformly mixed 4 h, after washing more after filtration,, oven dry, this pressed powder is dropped in the CTAB aqueous solution of 300 mL 2 %, 60 ℃ of constant temperature stir 2 h, more after filtration, washing, dry, solid is crossed to 200 mesh sieves after pulverizing.
Compound concentration is 26% sodium hydroxide solution 15 mL, slowly joins in the vinylformic acid of 12 mL after cool to room temperature, constantly stirs and makes to react completely.Under the condition constantly stirring, 4 g modification infusorial earth powder are joined in neutralizer, stir 30 min, it is uniformly dispersed.
With prolong, temperature is taken into account in 250 mL tetra-neck flasks of nitrogen conduit, adds 60mL hexanaphthene and 2.0 g dispersion agents (Span 60), and logical nitrogen 30 min, remove the oxygen in solution.Four-necked bottle is put in 40 ℃ of oil baths and mixes 30 min under mechanical stirring subsequently.To be mixed evenly after, successively appropriate aforesaid propylene acid/diatomite mixing solutions, 0.2 g initiator (Potassium Persulphate) and 0.15 g linking agent (MBA) are added in flask successively, stir after 30 min, be warming up to 70 ℃, react 3 h, after having reacted, heating installation is turned off, be stirred to solution always and be cooled to room temperature, then reaction solution suction filtration is separated, with deionized water wash, resulting white precipitate is dry 30 h in 100 ℃ of vacuum drying ovens, obtain diatomite/super absorbent resin Material cladding macromolecular material.
About the compound High hydrophilous resin material applications of diatomite: this seminar is engaged in treated starch research from the nineties.Through exploration for many years, complete lab scale and the pilot scale of serial water-retaining agent product, and batch production.Farm-forestry crop in these series product is taked precautions against drought agent by provincial-level appraisal (identify number 2004086), completes, and obtain national inventing patent (patent No. Z L 03127061.1) with the research of W-Gum direct production super absorbent resin.But because the strong water-absorbing material of starch base self physical strength is lower, in use procedure, be easily subject to the factors such as ambient pressure temperature to affect larger, cause its water-holding slow-release effect to decline, based on this reason, the diatomite that we rank first in the whole country the strong water-absorbing material of starch base and Jilin Province's reserves is combining, utilizing self-control biodegradable starch base strong absorptive resin is coating material, adopt original creation from heat release crosslinking process, realized the controlledly synthesis of different-grain diameter and the compound degradable macromolecule water-keeping material of coated thickness yolk-eggshell structure diatomite.This matrix material not only keeps water-absorbing material and diatomaceous primary characteristic, also mutual quasi-complement water-absorbing material machinery slightly low, the shortcoming that diatomite water-holding slow-release function is poor, makes this material have the advantages such as plasticity-is high, applied range.Be mainly used in agriculture, forestry plant plantation, and be applicable to ginseng and plant herbal medicine plantation, this material contributes to solve drought and water shortage, the severe water and soil erosion running in ginseng planting in recent years, the problems such as decline in benefits of using chemical fertilizer, contributes to improve ginseng output and quality, increases the income of ginseng agriculture.
Claims (2)
1. a synthetic method for the compound High hydrophilous resin material of diatomite, is characterized in that comprising following concrete steps:
1). take the diatomite of 10～20 parts of mistake 300 mesh sieves, add suitable quantity of water, mix, standby;
2). in the mixed solution obtaining to step 1), add 40～80 parts of propenyl compounds, vinylformic acid or acrylamide, be at room temperature uniformly mixed 1～2 h, is configured to diatomite/propenyl compound presoma mixed solution;
3). take 20～40 weight part sodium hydrate solids, be mixed with sodium hydroxide solution;
4). under the condition constantly stirring, the sodium hydroxide solution that step 3) is obtained joins step 2) carry out neutralization reaction in diatomite/propenyl compound presoma mixed solution of obtaining; After question response is complete, stops stirring and make neutralizer cooling gradually;
5). under mechanical stirring condition, the starch of certain mass is joined to the step 4 that is cooled to certain temperature) in the mixed solution that obtains, continue to stir 30～60min, starch is uniformly dispersed;
6). respectively the initiator potassium persulfate having prepared and linking agent MBA solution are slowly added to step 5) in the reaction solution that obtains, continue to stir 1～1.5h, reaction solution fades to translucent viscous fluid;
7). in the mixed solution obtaining to step 6), add a certain amount of ammoniacal liquor, system pH is adjusted between 7～8; After static 10～15min, system reaction, emits gas to completing;
8). the product that step 7) is obtained is processed into little bulk, 100
oin C thermostatic drying chamber, be dried to constant weight; Through broken, pulverizing, obtain particle or Powdered silicon-dioxide/SAP composite high-water uptake material,
The temperature of reaction system is in the scope of 20-40 ℃, and the weight proportion between raw material is: diatomite 2-15 g, Semen Maydis powder 3-20g, propenyl compound acrylic acid or acrylamide 40-60g, sodium hydroxide 20-30g, initiator 0.35-1.6g, linking agent 0.1-0.8g and 25% ammoniacal liquor 10-20ml.
2. the compound High hydrophilous resin material of diatomite of preparing by method claimed in claim 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417858A (en) * | 2017-07-21 | 2017-12-01 | 南京理工大学 | A kind of preparation method of the composite high-water-absorptivresin resin comprising diatomite and cellulose |
| CN111793169A (en) * | 2020-08-11 | 2020-10-20 | 李方 | High-salt-tolerance super absorbent resin and preparation process thereof |
| CN113413482A (en) * | 2018-05-28 | 2021-09-21 | 中山火炬职业技术学院 | Sanitary nursing pad with bedsore growth preventing function |
| CN113622201A (en) * | 2021-08-23 | 2021-11-09 | 胡玉婷 | Polyurethane synthetic leather with high moisture absorption and air permeability and preparation method thereof |
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| CN1468866A (en) * | 2003-06-06 | 2004-01-21 | 东北师范大学 | One-step synthesis process of producing biodegradable high-hydroscopicity resin directly with corn powder |
| CN101270179A (en) * | 2008-04-30 | 2008-09-24 | 东北师范大学 | Process for synthesizing modified starch series polymeric flocculant |
| CN101319031A (en) * | 2008-07-23 | 2008-12-10 | 哈尔滨工业大学 | Starch graft acrylic acid/modified verdelite high-water-absorption resin and preparing method thereof |
| CN101712785A (en) * | 2008-10-06 | 2010-05-26 | 常琛 | Novel super absorbent resin/inorganic nanoparticle composite material, preparation method thereof and usage thereof |
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2014
- 2014-01-15 CN CN201410017583.9A patent/CN103739784A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1468866A (en) * | 2003-06-06 | 2004-01-21 | 东北师范大学 | One-step synthesis process of producing biodegradable high-hydroscopicity resin directly with corn powder |
| CN101270179A (en) * | 2008-04-30 | 2008-09-24 | 东北师范大学 | Process for synthesizing modified starch series polymeric flocculant |
| CN101319031A (en) * | 2008-07-23 | 2008-12-10 | 哈尔滨工业大学 | Starch graft acrylic acid/modified verdelite high-water-absorption resin and preparing method thereof |
| CN101712785A (en) * | 2008-10-06 | 2010-05-26 | 常琛 | Novel super absorbent resin/inorganic nanoparticle composite material, preparation method thereof and usage thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417858A (en) * | 2017-07-21 | 2017-12-01 | 南京理工大学 | A kind of preparation method of the composite high-water-absorptivresin resin comprising diatomite and cellulose |
| CN113413482A (en) * | 2018-05-28 | 2021-09-21 | 中山火炬职业技术学院 | Sanitary nursing pad with bedsore growth preventing function |
| CN111793169A (en) * | 2020-08-11 | 2020-10-20 | 李方 | High-salt-tolerance super absorbent resin and preparation process thereof |
| CN112961281A (en) * | 2020-08-11 | 2021-06-15 | 李方 | High-salt-tolerance super absorbent resin |
| CN111793169B (en) * | 2020-08-11 | 2021-09-17 | 乐清市川嘉电气科技有限公司 | High-salt-tolerance super absorbent resin and preparation process thereof |
| CN113622201A (en) * | 2021-08-23 | 2021-11-09 | 胡玉婷 | Polyurethane synthetic leather with high moisture absorption and air permeability and preparation method thereof |
| CN113622201B (en) * | 2021-08-23 | 2023-04-14 | 东阳德彩纺织品有限公司 | Polyurethane synthetic leather with high moisture absorption and air permeability and preparation method thereof |
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Application publication date: 20140423 |