A kind of plant growing preparation method of cross-linking foaming water-retaining resin
Technical field
The present invention relates to the preparation method of water-retaining resin, a kind of specifically plant growing preparation method of cross-linking foaming water-retaining resin.
Background technology
The polymer water-retaining resin is the lightly crosslinked hydrophilic high molecular polymer of a class, can absorb the hundred times of own wt and even thousands of times distilled water, and water retention capacity is strong.Wherein, polyacrylic acid salt resin (comprising polyacrylamide, polyacrylic acid potassium, sodium polyacrylate) has that water absorbent rate is higher, absorption speed is fast, release characteristics such as water speed is slow, water retention property is good, use in fields such as farming, forestry plant cultivation, keeping crop seedling from drought, desertification control more and more, play an important role for drought and water shortage area and the geographic arviculture of Desertification, afforestation.Yet because the densification of polyacrylic acid salt resin in-house network pore structure, the aperture is small, and the water in the soil is being mingled with materials such as silt, mineral substance, fertilizer, in absorbing water, release the water process repeatedly, easily causes mesh to stop up, cause water absorbent rate to descend significantly, water retention is on the low side.According to relevant researchist's test, the polyacrylic acid salt resin of agroforestry use at present, inhaling muddy water (containing 5% earth) multiplying power only is 72~153g/g, protecting the muddy water rate is 53~70%.For this reason, farming, forestry plantation family adopt the way that increases resin demand to remedy usually, cause planting cost higher, and the big area that has influenced water-retaining resin is promoted.In recent years, research unit and manufacturing enterprise adopt the whole bag of tricks research and development modified polypropene hydrochlorate water-retaining resin both at home and abroad, to improve suction muddy water multiplying power and the water retention of resin in soil, reduce use cost.As: with starch, Mierocrystalline cellulose, vinylformic acid and polyvinyl alcohol is raw material, adopts microwave radiation, the synthetic water-retaining resin of inverse suspension polymerization method; And for example: with the methylene-bisacrylamide is linking agent, and ammonium persulphate and sodium bisulfite are redox agent, adopts the synthetic kaolin composite polypropylene acid of water solution polymerization process sodium-acrylamide composite water conservation resin; For another example: with vinylformic acid and magnesium hydroxide is raw material, and Potassium Persulphate is an initiator, and benzene disulfonic acid amide and nitrourea are composite foamable agent, synthetic foaming type magnesium polyacrylate imbibition resin.Retrieve a large amount of patent documentations and the research paper of publishing, do not find that as yet adopting potassium hydroxide and vinylformic acid is raw material, add silicon-dioxide, epoxy chloropropane, to sulfonyl azide, sodium bisulfite, make the report of plant growing with cross-linking foaming water-retaining resin.
Summary of the invention
In order to overcome existing polyacrylic acid salt resin in farming, the suction repeatedly that exists in the forestry plant cultivation, mesh easily stops up after releasing water, it is low with guarantor's muddy water rate to inhale the muddy water multiplying power, defectives such as use cost is higher, the invention provides the preparation method of a kind of plant growing with cross-linking foaming water-retaining resin, it is characterized in that: with potassium hydroxide and vinylformic acid is basic raw material, add silicon-dioxide, epoxy chloropropane, to sulfonyl azide, sodium bisulfite, by in and chemical reaction, initiated polymerization, crosslinked foaming, extrude pelletizing, boiled bed drying, cooling packing technology is made water-retaining resin.Mesh-structured loose, aperture of the water-retaining resin that this preparation method produces and specific surface area increase, compare with non-expanded polypropylene acid potassium resin, density reduces by 15~18%, inhale muddy water (5% earth) multiplying power and improve 38~45%, protect muddy water (5% earth) rate and improve 16~20%, be specially adapted to farming, forestry plant cultivation.
For realizing that the concrete technical scheme that the object of the invention adopted is:
Material purity is 99.0~99.9% potassium hydroxide, and purity is 99.5~99.9% ACRYLIC EMULSION, and granularity is the silicon-dioxide of 2~5 μ m, epoxy chloropropane, and to sulfonyl azide, sodium bisulfite.
Prescription potassium hydroxide 23~28 mass parts, ACRYLIC EMULSION 63~70 mass parts, silicon-dioxide 5~10 mass parts, epoxy chloropropane 0.05~0.12 mass parts, to sulfonyl azide 0.3~0.6 mass parts, sodium bisulfite 0.4~0.8 mass parts.
The preparation method will place reactor with the potassium hydroxide solution of distilled water diluting to 25% concentration, and control reactor stirring velocity 60r/min adds ACRYLIC EMULSION, 70 ± 1 ℃ of control temperature in the kettle, neutralization reaction 40~45min; Add silicon-dioxide, epoxy chloropropane, mix 8~10min; Add again sulfonyl azide, continue to stir 3~5min; Place the disc type reactor, add sodium bisulfite, initiated polymerization, 112~118 ℃ of controlled polymerization temperature, polymerization time 4~6min; After treating the polymer formation gelinite, place airtight constant temperature cupboard to carry out crosslinked foaming, 138 ± 1 ℃ of control blowing temperatures, foamed time 25~30min; Then, naturally cooling 90~120min places incorgruous tapered twin screw extruder, is cut into the particulate material of φ 0.15 * 2mm, and behind 115~120 ℃ of drying 200~240min of ebullated bed, again through naturally cooling, packing forms cross-linking foaming water-retaining resin.
The invention has the beneficial effects as follows: be basic raw material 1. with potassium hydroxide and vinylformic acid, in having designed and chemical reaction → initiated polymerization → crosslinked foaming → and extrude the production technique and the operational condition of pelletizing → boiled bed drying → cooling packing process, make the cross-linking foaming water-retaining agent realize suitability for industrialized production; 2. adopting epoxy chloropropane is linking agent, silicon-dioxide is filling modifying agent, sodium bisulfite is an initiator, to sulfonyl azide is whipping agent, the control blowing temperature is 138 ± 1 ℃, and foamed time is 25~30min, and the polyacrylic acid potassium resin is foamed in airtight constant temperature cupboard, increased the mesh aperture and the specific surface area of polyacrylic acid potassium resin inside, thereby improved suction muddy water multiplying power and protected the muddy water rate; 3. the cross-linking foaming water-retaining resin made of the present invention, compare with non-expanded polypropylene acid potassium resin, density reduces by 15~18%, inhales muddy water (5% earth) multiplying power and improves 38~45%, protect muddy water (5% earth) rate and improve 16~20%, be specially adapted to the agroforestry plant growing.
Embodiment
Embodiment 1:
With 24kg purity is the distilled water diluting that 99.0% potassium hydroxide adds 72kg, be made into potassium hydroxide solution 96kg, place reactor, 69 ℃ of reactor temperatures of control, stirring velocity 60r/min, adding 65kg purity is 99.5% ACRYLIC EMULSION, neutralization reaction 40min; Adding the 6kg granularity is silicon-dioxide and the 0.06kg epoxy chloropropane of 2 μ m, mixes 8 minutes; Add 0.4kg again to sulfonyl azide, continue to stir 3min; Place the disc type reactor, add the 0.5kg sodium bisulfite, initiated polymerization, 112 ℃ of controlled polymerization temperature, polymerization time 5min, treat the polymer formation gelinite after, place airtight constant temperature cupboard to carry out crosslinked foaming, 137 ℃ of control blowing temperatures, foamed time 25min; Then, naturally cooling 90min places incorgruous tapered twin screw extruder, is cut into the particulate material of φ 0.15 * 2mm, behind 115 ℃ of dry 200min of ebullated bed, forms cross-linking foaming water-retaining resin through naturally cooling, packing again.
Embodiment 2:
With 27kg purity is the distilled water diluting that 99.9% potassium hydroxide adds 81kg, is made into potassium hydroxide solution 108kg, places reactor, control reactor stirring velocity 60r/min, adding 68kg purity is 99.9% ACRYLIC EMULSION, 71 ℃ of control temperature in the kettle, neutralization reaction 45min; Adding the 9kg granularity is silicon-dioxide and the 0.11kg epoxy chloropropane of 5 μ m, mixes 10 min; Add 0.55kg again to sulfonyl azide, continue to stir 5min; Place the disc type reactor, add the 0.7kg sodium bisulfite, initiated polymerization, 118 ℃ of controlled polymerization temperature, polymerization time 6min, treat the polymer formation gelinite after, place airtight constant temperature cupboard to carry out crosslinked foaming, 139 ℃ of control blowing temperatures, foamed time 30min; Then, naturally cooling 120min places incorgruous tapered twin screw extruder, is cut into the particulate material of φ 0.15 * 2mm, behind 120 ℃ of dry 240min of ebullated bed, forms cross-linking foaming water-retaining resin through naturally cooling, packing again.
Embodiment 3:
With 28kg purity is the distilled water diluting that 99.0% potassium hydroxide adds 72kg, be made into potassium hydroxide solution 100kg, place reactor, 69 ℃ of reactor temperatures of control, stirring velocity 60r/min, adding 65kg purity is 99.5% ACRYLIC EMULSION, neutralization reaction 40min; Adding the 7.5kg granularity is silicon-dioxide and the 0.08kg epoxy chloropropane of 2 μ m, mixes 8 minutes; Add 0.3kg again to sulfonyl azide, continue to stir 3min; Place the disc type reactor, add the 0.6kg sodium bisulfite, initiated polymerization, 112 ℃ of controlled polymerization temperature, polymerization time 5min, treat the polymer formation gelinite after, place airtight constant temperature cupboard to carry out crosslinked foaming, 137 ℃ of control blowing temperatures, foamed time 25min; Then, naturally cooling 90min places incorgruous tapered twin screw extruder, is cut into the particulate material of φ 0.15 * 2mm, behind 115 ℃ of dry 200min of ebullated bed, forms cross-linking foaming water-retaining resin through naturally cooling, packing again.
Embodiment 4:
With 23kg purity is the distilled water diluting that 99.9% potassium hydroxide adds 77kg, is made into potassium hydroxide solution 100kg, places reactor, control reactor stirring velocity 60r/min, adding 70kg purity is 99.9% ACRYLIC EMULSION, 70 ℃ of control temperature in the kettle, neutralization reaction 45min; Adding the 10kg granularity is silicon-dioxide and the 0.11kg epoxy chloropropane of 5 μ m, mixes 10 min; Add 0.3kg again to sulfonyl azide, continue to stir 5min; Place the disc type reactor, add the 0.4kg sodium bisulfite, initiated polymerization, 115 ℃ of controlled polymerization temperature, polymerization time 6min, treat the polymer formation gelinite after, place airtight constant temperature cupboard to carry out crosslinked foaming, 138 ℃ of control blowing temperatures, foamed time 30min; Then, naturally cooling 120min places incorgruous tapered twin screw extruder, is cut into the particulate material of φ 0.15 * 2mm, behind 120 ℃ of dry 240min of ebullated bed, forms cross-linking foaming water-retaining resin through naturally cooling, packing again.