CN103819615B - Irradiation prepares the method for starch base high-absorbent material - Google Patents
Irradiation prepares the method for starch base high-absorbent material Download PDFInfo
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Abstract
The present invention relates to a kind of method that irradiation prepares starch base high-absorbent material.Irradiation prepares the method for starch base high-absorbent material, it is characterized in that comprising the steps: 1) according to starch: vinylformic acid: sodium hydroxide solution: mass ratio=6 ~ 9:44:47.6 ~ 60.9:40 ~ 80 of water, choose raw material; 2) water and starch mixing, Heat Gelatinization, repeated hydrogenation sodium hydroxide solution, obtains starch paste; 3) sodium hydroxide solution of remainder is placed in ice bath, in hydrogen injecting sodium hydroxide solution, obtains neutralizer; 4) starch paste and neutralizer mix; 5) mixture is under normal temperature, irradiation source after irradiation 1 ~ 4kGy, and room temperature places 8h, obtains colloid; 6) colloid is placed in mincer and rubs into strips, obtains strip colloid; 7) strip colloid is placed in microwave drying oven, and substep is dried to constant weight; 8) pulverizer pulverising step 7 is adopted) drying material that obtains, cross 20 ~ 100 mesh sieves, obtain irradiation and prepare starch base high-absorbent material.The water-absorbing material performance of preparation is high, cost is low.
Description
Technical field
The invention belongs to chemical industry, health, agricultural technical field, relate to the preparation of water-absorbing material, be specifically related to a kind of method that irradiation prepares starch base high-absorbent material.
Background technology
Water-absorbing material is the macromole that a class contains hydrophilic radical and crosslinking structure, is mainly divided into starch-series, cellulose-based, several large class of synthesized polymer system, and wherein starch-series has that raw material is common, cost is low, the advantage of easy degraded, is a most widely used class.Traditional starch acrylic water-absorbing material preparation method adopts the anti-phase solution polymerization process of chemical method, take Heavy Metal Reagent as initiator, a large amount of organic solvents needs recycling, and hybrid reaction condition is difficult to control, and also there is the problem of heavy-metal residual in water-absorbing material in addition.Irradiation method with untouchable ray be initiator, water solution polymerization process, avoid that facility investment is large, the problem of difficult solvent recovery, chemical residual, therefore, irradiation method extremely water-absorbing material prepares enterprises pay attention.Owing to adopting water polymerization, need a large amount of water to participate in reaction, exist according to problems such as rear colloid cutting adhesion, dry difficulties in irradiation method water-absorbing material trial production process.The invention provides the method that irradiation prepares starch base high-absorbent material, the operation problem of irradiation method can be solved, be applicable to enterprise practical need of production.
Summary of the invention
The object of the present invention is to provide a kind of irradiation to prepare the method for starch base high-absorbent material, the method can solve that water content in water-absorbing material preparation process is large, colloid cutting difficulty, drying and dehydrating problem, and the water-absorbing material performance of preparation is high, cost is low.
For achieving the above object, the technical solution used in the present invention is: irradiation prepares the method for starch base high-absorbent material, it is characterized in that comprising the steps:
1) according to starch: vinylformic acid: sodium hydroxide solution (aqueous sodium hydroxide solution): the preferred 7:44:60.9:60 of mass ratio=6 ~ 9:44:47.6 ~ 60.9:40 ~ 80(of water), choose raw material;
2) starch that water step 1) chosen and step 1) are chosen mixes, and stirs, Heat Gelatinization, then adds a small amount of sodium hydroxide solution (about 5 grams, now starch paste becomes more transparent), obtains starch paste;
3) sodium hydroxide solution of remainder is placed in ice bath, in the slow hydrogen injecting sodium hydroxide solution of vinylformic acid that step 1) is chosen, stirs heat radiation, obtain neutralizer;
4) by step 2) neutralizer prepared of the starch paste prepared and step 3) mixes, and pours in plastics bag, excluding air, and sealing, obtains mixture;
5) mixture step 4) prepared is under normal temperature, irradiation source after irradiation 1 ~ 4kGy, and room temperature places about 8h (7.9-8.1h), obtains colloid;
6) colloid that step 5) obtains is placed in mincer rubs into strips, obtain strip colloid;
7) strip colloid step 6) obtained is laid in plastic pallet, and be placed in microwave drying oven, stage drying is to constant weight;
8) pulverizer pulverising step 7 is adopted) drying material (namely dry strip colloid) that obtains, cross 20 ~ 100 mesh sieves, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag to encapsulate).
Starch in step 1) is any one in fry starch of konjak, W-Gum etc.
The concentration of the sodium hydroxide solution in step 1) is 32wt%.
Step 2) in heating temperature be 90 DEG C.
Step 2) in sodium hydroxide solution add-on be the 8.2-10.5% of the sodium hydroxide solution total mass that step 1) is chosen, the pH regulating starch paste is about 8.
In step 5), irradiation source is
60any one in Co-gamma-rays, x-ray, electron beam etc., preferably
60co-gamma-rays.
Point three sections of dryings in step 7), enter microwave the 1st time: control microwave drying temperature and be no more than 80 DEG C, strip colloid evenly tiles within thickness 2 centimetres, and the water content of dried strip colloid reduces to 35-50%; Enter microwave 2nd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 2nd dried strip colloid reduces to 20-30%; Enter microwave 3rd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 3rd dried strip colloid reduces to 8-12%.
Step 2) in a small amount of sodium hydroxide solution add in starch paste, the pH of adjustable starch paste, about 8, is conducive to the abundant exposure of starch group.Vinylformic acid slowly injects by step 3) under condition of ice bath in sodium hydroxide, and stirs, and reduces acrylic acid volatilization loss.Excluding air during step 4) sealing, plays the effect of nitrogen protection equally, can reduce the link of inflated with nitrogen, and improve percentage of grafting to product.Adopt mincer to pulverize according to rear blob of viscose in step 6), solve the difficult problem according to rear blob of viscose cutting.Strip blob of viscose individual layer tiles by step 7), within colloid thickness 2 centimetres, adopts micro-wave drying method, can solve the difficult problem that forced air drying time long, colloid is difficult to parch; Adopt microwave stage drying, avoid high frequency microwave drying to cause product performance sharply to reduce.After step 5) irradiation, room temperature places 8h, and performance improves about 10%.
Several places of the present invention to existing technique are improved to: 1) keep the ratio of vinylformic acid mass ratio 44 to become, adjustment starch: sodium hydroxide solution: the mass ratio of water is: 6 ~ 9:47.6 ~ 60.9:40 ~ 80 scope, reduce water content in 50%-70% scope, save drying cost more than 20%; 2) preparation of neutralizer adopts condition of ice bath, reduces vinylformic acid volatilization loss during normal temperature mixing, improves percentage of grafting and decreasing pollution; 3) excluding air [step 4) of the present invention] during mixing filling, can play the effect of nitrogen protection, reduces routine and fills nitrogen cost; 4) increase the storage period (after irradiation, room temperature places 8h) according to rear colloid, enhance product performance about 10%; 5) adopt the broken blob of viscose of mincer to be strip, solve adhesion difficult problem when other machines or manual cutting blob of viscose, energy-efficient; 6) adopt microwave stage drying method, solve the forced air drying time long, be difficult to the difficult problem that parches and the temperatures involved that conventional microwave primary drying causes, during energy-saving.
The invention has the beneficial effects as follows: several improvement of the present invention solves four difficult problems in water solution polymerization process: the difficult problem that 1) moisture content is high; 2) a colloid cutting adhesion difficult problem; 3) a product drying dehydration difficult problem; 4) a vinylformic acid utilization ratio difficult problem that is low and environmental pollution after volatilizing.The present invention reduces the raw materials cost and production cost of preparing water-absorbing material simultaneously, water-absorbing material performance is: absorb tap water, pure water, salt solution and blood plasma and be respectively 350,687,59 and 16g/g, meet the standard GB/T/T22905-2008 of paper diaper high exhaustion, the water-absorbing material performance of preparation is high.The present invention can be applicable to the process modification that various scale water-absorbing resin manufacturing enterprises irradiation method prepares water-absorbing resin: comprise formula rate, mixing link, filling link, shine rear pulverizing link, dry link, the cost of conservation, production, transport, blowdown, improves product profit.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of water-absorbing material prepared by the present invention.
Fig. 2 is the infrared spectrogram of water-absorbing material prepared by the present invention.
Fig. 3 absorbs tap water graphic representation under the water-absorbing material differing temps prepared of the present invention.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1:
Irradiation prepares the method for starch base high-absorbent material, comprises the steps:
1) starch (fry starch of konjak) 7 grams is chosen, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 60 grams, water, stand-by;
2) mixed with water by starch, stir, be heated to 90 DEG C of gelatinizations, then add the sodium hydroxide solution 5 grams that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid step 1) chosen in ice bath slowly injects remaining sodium hydroxide solution, stirs heat radiation, obtains neutralizer;
4) by step 2) neutralizer prepared of the starch paste prepared and step 3) mixes, and fill with bag, excluding air, sealing, obtains mixture;
5) mixture after filling with bag at normal temperature, irradiation source is
60under Co-gamma-rays after irradiation 1kGy, room temperature places 8h, obtains colloid;
6) colloid after irradiation is placed in mincer and rubs into strips, and single flat is layered in pallet, obtains strip colloid;
7) strip colloid is placed in microwave drying oven together with pallet, point 3 dryings complete (note: when doing scanning electron microscope analysis, adopts lyophilize) herein;
Enter microwave 1st time: control microwave drying temperature and be no more than 80 DEG C, strip colloid evenly tiles within thickness 2 centimetres, and the water content of dried strip colloid reduces to 50%; Enter microwave 2nd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave 3rd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 3rd dried strip colloid reduces to 10%;
8) adopt pulverizer to pulverize the material of drying, cross 20-100 mesh sieve (note: when doing scanning electron microscope analysis, does not pulverize) herein, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, and paper plastic bag is packed, sealing).
One, the water-absorbing material scanning electron microscope analysis prepared of the present invention, the microscopic appearance of research water-absorbing material
Above-mentioned steps 7) according to after water-absorbing material colloid adopt lyophilize (dry without microwave drying oven), do surface topography scanning analysis by scanning electron microscope.Scanning electron microscope result: as seen from Figure 1, there occurs crosslinking reaction between radiation initiation starch molecule and sodium acrylate monomers, forms fine and close network structure, is the basis of water suction.
Two, the water-absorbing material Infrared spectroscopy prepared of the present invention, the group change of research water-absorbing material
Above-mentioned steps 8) in get 100 mesh sieve materials, with KBr mixed pressuring plate, make the infrared structure analysis of material of infrared spectrometer.The results of FT-IR shows, in Fig. 2, No. 3 is the spectrogram of starch molecule, 3390.6,1017.5cm
-1there is the stretching vibration peak of-OH, C-O in place, is the characteristic peak of starch respectively; 1796cm is there is in No. 4
-1there is the stretching vibration peak of C=O in place, 1553.8,1450.2,1409.9cm
-1there is-COO-stretching vibration peak in place, is polyacrylic characteristic peak, at 1023.3cm
-1place is the characteristic peak of starch, and this illustrates that starch and vinylformic acid there occurs graft reaction.
Three, water absorbing properties test
1) prepare the beaker that 9 are equipped with 1000 grams of tap water, be placed on respectively by beaker in-7 degree refrigerator ice milk districts, normal temperature and 70 degree of water-baths, 3 repetitions of often kind of temperature, are incubated more than 3 hours, stand-by;
2) get above-mentioned steps 8) in 40 mesh sieve material 1 gram, totally 9 parts, add in 9 beakers respectively, under being still placed on former temperature, timing immediately;
3) after this littlely to weigh constantly 0.5,1,1.5,2,2.5 and 6, claimed heavy rear colloid still to put into former water tumbler and continued water suction, weighed the weight of colloid in each beaker, the material Water absorption be designated as under this time of averaging;
4) weighing technique: the circular stainless steel and iron sieve of cut-off footpath 20cm order number 20 object, first removes the peel, pours in sieve, after being filtered dry moisture, being placed on the water in beaker by sieve on balance and weighing, record, be the Water absorption of material together with colloid on electronic balance;
Differing temps water suction result, as shown in Figure 3, temperature is higher, and Water absorption is larger, and the time of the water suction that reaches capacity is shorter.Reach 1 hour maximum Water absorption time when 70 DEG C, multiple is 350 times, and normal temperature was issued to the maximum Water absorption time at 1.5 hours, and multiple is 320 times, and-7 reach the maximum Water absorption time at 2.5 hours when spending, and are about 300 times.In lower 6 hours of each temperature environment, Water-saving effect is good.Illustrate that water-absorbing material performance prepared by the present invention is high.
Embodiment 2: regulating pondage
Irradiation prepares the method for starch base high-absorbent material, comprises the steps:
1) choose 5 parts of following raw materials, stand-by (correspondence obtains 5 parts of products), starch is W-Gum:
1st part: starch 7 grams, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 40 grams, water;
2nd part: starch 7 grams, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 50 grams, water;
3rd part: starch 7 grams, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 60 grams, water;
4th part: starch 7 grams, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 70 grams, water;
5th part: starch 7 grams, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 80 grams, water;
2) mixed with water by starch, stir, be heated to 90 DEG C of gelatinizations, then add the sodium hydroxide solution 5 grams that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid step 1) chosen in ice bath slowly injects remaining sodium hydroxide solution, stirs heat radiation, obtains neutralizer;
4) by step 2) neutralizer prepared of the starch paste prepared and step 3) mixes, and fill with bag, excluding air, sealing, obtains mixture;
5) mixture after filling with bag at normal temperature, irradiation source is
60under Co-gamma-rays after irradiation 2kGy, room temperature places about 8h, obtains colloid;
6) colloid after irradiation is placed in mincer and rubs into strips, and single flat is layered in pallet, obtains strip colloid;
7) be placed in microwave drying oven by strip colloid together with pallet, point 3 dryings are complete;
Enter microwave 1st time: control microwave drying temperature and be no more than 80 DEG C, strip colloid evenly tiles within thickness 2 centimetres, and the water content of dried strip colloid reduces to 50%; Enter microwave 2nd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave 3rd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 3rd dried strip colloid reduces to 10%;
8) adopt the material of pulverizer powder drying, cross 40 mesh sieves, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, and paper plastic bag is packed, sealing).
Water absorbing properties is tested:
1) prepare the beaker that 3 are equipped with 1000 grams of tap water, place stand-by at normal temperatures;
2) get above-mentioned steps 8) in 40 mesh sieve material 1 gram, totally 3 parts, add in 3 beakers respectively, timing, after 1 hour, weighs the weight of colloid in each beaker, and be designated as material Water absorption, weighing technique is the same;
3) Using such method weighs the Water absorption of pure water, physiological saline and urine;
4) pure water is distilled water; Physiological saline (0.9wt% sodium-chlor) is prepared: take 9 grams of sodium-chlor, adding distil water 991 grams, stirring and dissolving, be namely formulated as 1000 grams, physiological saline; Basis urine preparation: Sodium phosphate dibasic 0.2 gram, potassium primary phosphate 0.30 gram, 18 grams, sodium-chlor, adding distil water to 1000 gram, obtain 1000 grams of artificial urine;
5) water suction of other liquid is with step 2), repeat to average for 3 times.
Water suction result, in table 1.Five kinds of materials all meet national standard.When starch, vinylformic acid, alkali number are consistent, regulating pondage can reduce the production cost based on drying cost, is convenient to mincer crushing operation: colloidal materials water content is between 59.4%-67.8%, and finished product dry-matter yield is between 32.2%-40.6%.
Table 1(table 1 is the absorption multiple of water-absorbing material different solutions prepared by the present invention.）
Illustrate that water-absorbing material performance prepared by the present invention is high.
Embodiment 3: regulate alkali number
Irradiation prepares the method for starch base high-absorbent material, comprises the steps:
1) choose 2 parts of following raw materials, stand-by (correspondence obtains 2 parts of products), starch is fry starch of konjak:
1st part: choose starch 7 grams, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 47.6 grams, 60 grams, water;
2nd part: choose starch 7 grams, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 60 grams, water;
2) mixed with water by starch, stir, be heated to 90 DEG C of gelatinizations, then add the sodium hydroxide solution 5 grams that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid step 1) chosen in ice bath slowly injects 42.6 grams of remaining sodium hydroxide solutions, stirs heat radiation, obtains neutralizer;
4) by step 2) neutralizer prepared of the starch paste prepared and step 3) mixes, and fill with bag, excluding air, sealing, obtains mixture;
5) mixture after filling with bag at normal temperature, irradiation source is
60under Co-gamma-rays after 2kGy, room temperature places about 8h, obtains colloid;
6) colloid after irradiation is placed in mincer and rubs into strips, and single flat is layered in pallet, obtains strip colloid;
7) be placed in microwave drying oven by strip colloid together with pallet, point 3 dryings are complete;
Enter microwave 1st time: control microwave drying temperature and be no more than 80 DEG C, strip colloid evenly tiles within thickness 2 centimetres, and the water content of dried strip colloid reduces to 50%; Enter microwave 2nd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave 3rd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 3rd dried strip colloid reduces to 10%;
8) adopt the material of pulverizer powder drying, cross 40 mesh sieves, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, and paper plastic bag is packed, sealing).
Water absorbing properties is tested:
1) prepare the beaker that 3 are equipped with 1000 grams of tap water, place stand-by at normal temperatures;
2) get above-mentioned steps 8) in 40 mesh sieve material 1 gram, totally 3 parts, add in 3 beakers respectively, timing, after 1 hour, weighs the weight of colloid in each beaker, and be designated as material Water absorption, weighing technique is the same;
3) Using such method weighs the Water absorption of pure water, physiological saline and urine;
4) pure water is distilled water; Physiology salt (0.9% sodium-chlor) is prepared: take 9 grams of sodium-chlor, adding distil water 991 grams, stirring and dissolving, be namely formulated as 1000 grams, physiological saline; Basis urine preparation: Sodium phosphate dibasic 0.2 gram, potassium primary phosphate 0.30 gram, 18 grams, sodium-chlor, adding distil water to 1000 gram, obtain 1000 grams of artificial urine;
5) water suction of other liquid is with step 2), repeat to average for 3 times.
Water suction result, when starch, vinylformic acid, water quantity holding are consistent, suitably increase alkali number, can reduce raw materials cost, improve absorbed performance, bi-material all meets national standard.Colloidal materials water content, between 62.6%-64.1%, is convenient to mincer crushing operation, and product dry-matter yield is between 35.9%-37.4%.Absorb tap water, pure water, physiological saline and urine multiple respectively more than 300,500,45 and 55.Illustrate that water-absorbing material performance prepared by the present invention is high.
Embodiment 4: regulate amount of starch (contrasting with embodiment 1)
Irradiation prepares the method for starch base high-absorbent material, comprises the steps:
1) starch 9 grams is chosen, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 60 grams, water, stand-by;
2) mixed with water by starch, stir, be heated to 90 DEG C of gelatinizations, then add the sodium hydroxide solution 5 grams that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid step 1) chosen in ice bath slowly injects remaining sodium hydroxide solution, stirs heat radiation, obtains neutralizer;
4) by step 2) neutralizer prepared of the starch paste prepared and step 3) mixes, and fill with bag, excluding air, sealing, obtains mixture;
5) mixture after filling with bag at normal temperature, irradiation source is
60under Co-gamma-rays after irradiation 1kGy, room temperature places 8h, obtains colloid;
6) colloid after irradiation is placed in mincer and rubs into strips, and single flat is layered in pallet, obtains strip colloid;
7) strip colloid is placed in microwave drying oven together with pallet, point 3 dryings complete (note: when doing scanning electron microscope analysis, adopts lyophilize) herein;
Enter microwave 1st time: control microwave drying temperature and be no more than 80 DEG C, strip colloid evenly tiles within thickness 2 centimetres, and the water content of dried strip colloid reduces to 50%; Enter microwave 2nd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave 3rd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 3rd dried strip colloid reduces to 10%;
8) adopt pulverizer to pulverize the material of drying, cross 40 mesh sieves (note: when doing scanning electron microscope analysis, does not pulverize) herein, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, and paper plastic bag is packed, sealing).
Water absorbing properties is tested:
1) prepare the beaker that 3 are equipped with 1000 grams of tap water, place stand-by at normal temperatures;
2) get above-mentioned steps 8) in 40 mesh sieve material 1 gram, totally 3 parts, add in 3 beakers respectively, timing, after 1 hour, weighs the weight of colloid in each beaker, and be designated as material Water absorption, weighing technique is the same;
3) Using such method weighs the Water absorption of pure water, physiological saline and urine;
4) pure water is distilled water; Physiology salt (0.9wt% sodium-chlor) is prepared: take 9 grams of sodium-chlor, adding distil water 991 grams, stirring and dissolving, be namely formulated as 1000 grams, physiological saline; Basis urine preparation: Sodium phosphate dibasic 0.2 gram, potassium primary phosphate 0.30 gram, 18 grams, sodium-chlor, adding distil water to 1000 gram, obtain 1000 grams of artificial urine;
5) water suction of other liquid is with step 2), repeat to average for 3 times.
Water suction result, when vinylformic acid, sodium hydroxide, water quantity holding are consistent, suitably increase amount of starch, can reduce water-content and raw materials cost, keep certain absorbed performance, bi-material all meets national standard.Material now according to rear water content 63.4%, is convenient to mincer crushing operation, and product dry-matter yield is 36.6%.Absorb tap water, pure water, physiological saline and urine multiple respectively more than 400,900,49 and 52, meet national standard.Illustrate that water-absorbing material performance prepared by the present invention is high.
Embodiment 5: regulate amount of starch
Irradiation prepares the method for starch base high-absorbent material, comprises the steps:
1) starch 6 grams is chosen, 44 grams, vinylformic acid, 32wt% aqueous sodium hydroxide solution 60.9 grams, 60 grams, water, stand-by;
2) mixed with water by starch, stir, be heated to 90 DEG C of gelatinizations, then add the sodium hydroxide solution 6 grams that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid step 1) chosen in ice bath slowly injects remaining sodium hydroxide solution, stirs heat radiation, obtains neutralizer;
4) by step 2) neutralizer prepared of the starch paste prepared and step 3) mixes, and fill with bag, excluding air, sealing, obtains mixture;
5) mixture after filling with bag at normal temperature, irradiation source is
60under Co-gamma-rays after irradiation 4kGy, room temperature places 8h, obtains colloid;
6) colloid after irradiation is placed in mincer and rubs into strips, and single flat is layered in pallet, obtains strip colloid;
7) strip colloid is placed in microwave drying oven together with pallet, point 3 dryings complete (note: when doing scanning electron microscope analysis, adopts lyophilize) herein;
Enter microwave 1st time: control microwave drying temperature and be no more than 80 DEG C, strip colloid evenly tiles within thickness 2 centimetres, and the water content of dried strip colloid reduces to 50%; Enter microwave 2nd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave 3rd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 3rd dried strip colloid reduces to 10%;
8) adopt pulverizer to pulverize the material of drying, cross 40 mesh sieves (note: when doing scanning electron microscope analysis, does not pulverize) herein, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, and paper plastic bag is packed, sealing).
Water absorbing properties is tested:
1) prepare the beaker that 3 are equipped with 1000 grams of tap water, place stand-by at normal temperatures;
2) get above-mentioned steps 8) in 40 mesh sieve material 1 gram, totally 3 parts, add in 3 beakers respectively, timing, after 1 hour, weighs the weight of colloid in each beaker, and be designated as material Water absorption, weighing technique is the same;
3) Using such method weighs the Water absorption of pure water, physiological saline and urine;
4) pure water is distilled water; Physiology salt (0.9wt% sodium-chlor) is prepared: take 9 grams of sodium-chlor, adding distil water 991 grams, stirring and dissolving, be namely formulated as 1000 grams, physiological saline; Basis urine preparation: Sodium phosphate dibasic 0.2 gram, potassium primary phosphate 0.30 gram, 18 grams, sodium-chlor, adding distil water to 1000 gram, obtain 1000 grams of artificial urine;
5) water suction of other liquid is with step 2), repeat to average for 3 times.
Water suction result, when vinylformic acid, sodium hydroxide, water quantity holding are consistent, suitably increase amount of starch, can reduce water-content and raw materials cost, keep certain absorbed performance, bi-material all meets national standard.Material now according to rear water content 64.7%, is convenient to mincer crushing operation, product dry-matter yield 35.3%.Absorb tap water, pure water, physiological saline and urine multiple respectively more than 700,1200,65 and 70, meet national standard.Illustrate that water-absorbing material performance prepared by the present invention is high.
Claims (5)
1. irradiation prepares the method for starch base high-absorbent material, it is characterized in that comprising the steps:
1) according to starch: vinylformic acid: sodium hydroxide solution: mass ratio=6 ~ 9:44:47.6 ~ 60.9:40 ~ 80 of water, raw material is chosen;
The concentration of sodium hydroxide solution is 32wt%;
2) by step 1) water and the step 1 chosen) starch chosen mixes, and to stir, Heat Gelatinization, then add a small amount of sodium hydroxide solution, obtain starch paste;
3) sodium hydroxide solution of remainder is placed in ice bath, step 1) in the vinylformic acid hydrogen injecting sodium hydroxide solution chosen, stir heat radiation, obtain neutralizer;
4) by step 2) starch paste prepared and step 3) neutralizer prepared mixes, and pours in plastics bag, excluding air, and sealing, obtains mixture;
5) by step 4) mixture prepared is under normal temperature, irradiation source after irradiation 1 ~ 4kGy, and room temperature places about 8h, obtains colloid;
6) by step 5) colloid that obtains is placed in mincer and rubs into strips, obtains strip colloid;
7) by step 6) the strip colloid that obtains is laid in plastic pallet, and be placed in microwave drying oven, stage drying is to constant weight;
Stage drying is point three sections of dryings, enters microwave the 1st time: control microwave drying temperature and be no more than 80 DEG C, strip colloid evenly tiles within thickness 2 centimetres, and the water content of dried strip colloid reduces to 35-50%; Enter microwave 2nd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 2nd dried strip colloid reduces to 20-30%; Enter microwave 3rd time: control microwave drying temperature and be no more than 100 DEG C, the water content of the 3rd dried strip colloid reduces to 8-12%;
8) pulverizer pulverising step 7 is adopted) drying material that obtains, cross 20 ~ 100 mesh sieves, obtain irradiation and prepare starch base high-absorbent material.
2. irradiation according to claim 1 prepares the method for starch base high-absorbent material, it is characterized in that: step 1) in starch be any one in fry starch of konjak, W-Gum.
3. irradiation according to claim 1 prepares the method for starch base high-absorbent material, it is characterized in that: step 2) in heating temperature be 90 DEG C.
4. irradiation according to claim 1 prepares the method for starch base high-absorbent material, it is characterized in that: step 2) in sodium hydroxide solution add-on be step 1) 8.2-10.5% of sodium hydroxide solution total mass that chooses.
5. irradiation according to claim 1 prepares the method for starch base high-absorbent material, it is characterized in that: step 5) in irradiation source be
60any one in Co-gamma-rays, x-ray, electron beam.
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| CN201410072370.6A CN103819615B (en) | 2014-02-28 | 2014-02-28 | Irradiation prepares the method for starch base high-absorbent material |
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| CN105367723B (en) * | 2015-12-17 | 2018-02-02 | 西北师范大学 | A kind of method that water-loss reducer is prepared using biomass castoff |
| CN105884974B (en) * | 2016-06-14 | 2018-07-13 | 四川省农业科学院生物技术核技术研究所 | A kind of starch-series water-absorbing resin stage drying method |
| CN106084132B (en) * | 2016-06-14 | 2019-01-04 | 四川省农业科学院生物技术核技术研究所 | A kind of environmentally friendly, Mobyneb agricultural water-retaining agent preparation method |
| CN106279540B (en) * | 2016-08-02 | 2018-07-24 | 湖北省农业科学院农产品加工与核农技术研究所 | A kind of preparation method of fry starch of konjak drier |
| CN106800615A (en) * | 2017-02-09 | 2017-06-06 | 山东大学 | A kind of preparation method of polyacrylic water-loss reducer |
| CN108070056B (en) * | 2017-12-14 | 2019-12-03 | 合肥科拜耳新材料有限公司 | A kind of laser modified method for preparing the dedicated thermoplastic starch of biodegradable plastic |
| CN110003389A (en) * | 2019-03-25 | 2019-07-12 | 北京林业大学 | A kind of environment-friendly type agricultural water-retaining agent and preparation method thereof |
| CN109897137B (en) * | 2019-03-27 | 2021-10-26 | 武汉纺织大学 | Super water-absorbing starch and preparation method thereof |
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| CN101161695A (en) * | 2006-10-11 | 2008-04-16 | 西北师范大学 | Method for preparing absorbent material by micro-wave radiation of potato fecula industry slag grafted polymeric acrylate |
| CN101560280A (en) * | 2009-06-02 | 2009-10-21 | 夏和舟 | Method for preparing binary-graft starch by irradiation initiation |
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| CN101161695A (en) * | 2006-10-11 | 2008-04-16 | 西北师范大学 | Method for preparing absorbent material by micro-wave radiation of potato fecula industry slag grafted polymeric acrylate |
| CN101560280A (en) * | 2009-06-02 | 2009-10-21 | 夏和舟 | Method for preparing binary-graft starch by irradiation initiation |
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