CN103819615A - Method of preparing starch-base highly-water-absorbent material by radiation - Google Patents
Method of preparing starch-base highly-water-absorbent material by radiation Download PDFInfo
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- CN103819615A CN103819615A CN201410072370.6A CN201410072370A CN103819615A CN 103819615 A CN103819615 A CN 103819615A CN 201410072370 A CN201410072370 A CN 201410072370A CN 103819615 A CN103819615 A CN 103819615A
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Abstract
The invention relates to a method of preparing a starch-base highly-water-absorbent material by radiation. The method is characterized by comprising steps of: 1) preparing raw materials of starch, acrylic acid, sodium hydroxide solution and water according to a weight ratio of 6-9:44:47.6-60.9:40-80; 2) mixing the water and the starch, heating for gelatinization, and adding the sodium hydroxide solution to obtain starch paste; 3) placing the rest of the sodium hydroxide solution in an ice bath, and injecting the acrylic acid into the sodium hydroxide solution to obtain a neutralization solution; 4) uniformly mixing the starch paste and the neutralization solution; 5) radiating the mixture at room temperature under a radiation source for 1-4 kGy, and placing at room temperature for 8 h to obtain colloid; 6) adding the colloid into a meat mincer and mincing the colloid into bars to obtain bar-shaped colloid; 7) putting the bar-shaped colloid into a microwave drying oven, and drying step by step until the weight of the bar-shaped colloid is constant; and 8) smashing the dry material obtained in the step 7) by a smashing machine, and sieving with a sieve having a size of 20-100 meshes to obtain the starch-base highly-water-absorbent material. The starch-base highly-water-absorbent material is high in performance and low in cost.
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 is prepared 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 classes of synthesized polymer system, and wherein starch-series has advantages of that raw material is common, cost is low, easy degraded, is a most widely used class.Traditional starch acrylamide acids 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 has in addition the problem of heavy-metal residual in water-absorbing material.Irradiation method take untouchable ray as 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 is prepared enterprises pay attention.Owing to adopting water polymerization, need a large amount of water to participate in reaction, in irradiation method water-absorbing material trial production process, exist according to problems such as rear colloid cutting adhesion, dry difficulties.The invention provides irradiation and prepare the method for starch base high-absorbent material, can solve the operation problem of irradiation method, 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 is prepared 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 the water of step 1) being chosen is chosen with step 1) mixes, and stirs, heats gelatinization, then adds a small amount of sodium hydroxide solution (approximately 5 grams, now starch paste becomes more transparent), obtains starch paste;
3) remaining sodium hydroxide solution 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 pour in plastics bag, excluding air, sealing, obtains mixture;
5) mixture of being prepared by step 4) is under normal temperature, irradiation source after irradiation 1～4kGy, and room temperature is placed 8h left and right (7.9-8.1h), obtains colloid;
6) colloid step 5) being obtained is placed in mincer and rubs into strips, obtains strip colloid;
7) strip colloid step 6) being obtained is laid in plastic pallet, is placed in microwave drying oven, and stage drying is to constant weight;
8) adopt pulverizer pulverising step 7) drying material (i.e. dry strip colloid) that obtains, cross 20～100 mesh sieves, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation).
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 ℃.
Step 2) in sodium hydroxide solution add-on be the 8.2-10.5% of the sodium hydroxide solution total mass chosen of step 1), regulating the pH of starch paste is 8 left and right.
In step 5), irradiation source is
60any one in Co-gamma-rays, x ray, electron beam etc., preferably
60co-gamma-rays.
In step 7) points three sections dry, enter microwave the 1st time: control microwave drying temperature and be no more than 80 ℃, strip colloid evenly tiles in 2 centimetres of thickness, and the water content of dried strip colloid is reduced to 35-50%; Enter microwave the 2nd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 2nd dried strip colloid is reduced to 20-30%; Enter microwave the 3rd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 3rd dried strip colloid is reduced to 8-12%.
Step 2) in a small amount of sodium hydroxide solution add in starch paste, the pH of adjustable starch paste, in 8 left and right, is conducive to the abundant exposure of starch group.Step 3) is slowly injected vinylformic acid under condition of ice bath in sodium hydroxide, and stirs, and reduces acrylic acid volatilization loss.Excluding air when step 4) sealing, plays the effect of nitrogen protection equally to product, can reduce the link of inflated with nitrogen, and improve percentage of grafting.In step 6), adopt mincer to pulverize according to rear blob of viscose, solve the difficult problem according to rear blob of viscose cutting.Step 7) is strip blob of viscose individual layer tiling, in 2 centimetres of colloid thickness, adopts micro-wave drying method, can solve the difficult problem that the forced air drying time is long, colloid is difficult to parch; Adopt microwave stage drying, avoid high frequency microwave to be dried and cause product performance sharply to reduce.After step 5) irradiation, room temperature is placed 8h, and performance improves 10% left and right.
The present invention is improved to several places of existing technique: 1) keep the ratio of vinylformic acid mass ratio 44 to become, adjust 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, and the vinylformic acid volatilization loss while reducing normal temperature mixing improves percentage of grafting and reduces and pollute; 3) excluding air [step 4) of the present invention] when mixing filling, can play the effect of nitrogen protection, reduces routine and fills nitrogen cost; 4) increase the storage period (after irradiation, room temperature is placed 8h) according to rear colloid, 10% left and right of enhancing product performance; 5) adopting the broken blob of viscose of mincer is strip, and the adhesion difficult problem while solving other machines or manual cutting blob of viscose is energy-efficient; 6) adopt microwave stage drying method, solve the difficult problem that the forced air drying time is long, be difficult to parch, and the temperatures involved that causes of conventional microwave primary drying, when energy-saving.
The invention has the beneficial effects as follows: several improvement of the present invention have solved four difficult problems in water solution polymerization process: 1) the high difficult problem of moisture content; 2) a colloid cutting adhesion difficult problem; 3) a product drying dehydration difficult problem; 4) difficult problem of environmental pollution after the low and volatilization of vinylformic acid utilization ratio.The present invention reduces raw materials cost and the 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-absorbable resin, 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 enterprise irradiation method is prepared water-absorbing resin: comprise formula rate, mix link, filling link, according to rear pulverizing link, dry link, the cost of conservation, production, transportation, blowdown, improves product profit.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the water-absorbing material prepared of the present invention.
Fig. 2 is the infrared spectrogram of the water-absorbing material prepared of 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 better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1:
Irradiation is prepared the method for starch base high-absorbent material, comprises the steps:
1) choose 7 grams of starch (fry starch of konjak), 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 60 grams, water, stand-by;
2) starch is mixed with water, stir, be heated to 90 ℃ of gelatinizations, then add 5 grams of the sodium hydroxide solutions that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid of in ice bath, step 1) being chosen 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 fills with bag, excluding air, sealing, obtains mixture;
5) mixture of filling with after bag at normal temperature, irradiation source is
60under Co-gamma-rays, after irradiation 1kGy, room temperature is placed 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 to point 3 times dry complete (note: while doing scanning electron microscope analysis, adopt lyophilize herein) together with pallet;
Enter microwave the 1st time: control microwave drying temperature and be no more than 80 ℃, strip colloid evenly tiles in 2 centimetres of thickness, and the water content of dried strip colloid reduces to 50%; Enter microwave the 2nd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave the 3rd time: control microwave drying temperature and be no more than 100 ℃, 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: while doing scanning electron microscope analysis, do not pulverize) herein, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, paper plastic bag packing, sealing).
One, the water-absorbing material scanning electron microscope analysis that prepared by 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, between radiation initiation starch molecule and sodium acrylate monomers, crosslinking reaction having occurred, formed fine and close network structure, is the basis of water suction.
Two, the water-absorbing material Infrared spectroscopy that prepared by the present invention, the group of research water-absorbing material changes
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 spectrograms that are starch molecule, 3390.6,1017.5cm
-1place's stretching vibration peak of appearance-OH, C-O is respectively the characteristic peak of starch; In No. 4, there is 1796cm
-1there is the stretching vibration peak of C=O in place, 1553.8,1450.2,1409.9cm
-1appearance-the COO-of place stretching vibration peak is polyacrylic characteristic peak, at 1023.3cm
-1place is the characteristic peak of starch, and graft reaction has occurred for this explanation starch and vinylformic acid.
Three, water absorbing properties test
1) prepare 9 beakers that 1000 grams of tap water are housed, beaker is placed on respectively in-7 degree refrigerator ice milk districts, normal temperature and 70 degree water-baths, 3 repetitions of every kind of temperature, insulation is more than 3 hours, stand-by;
2) get above-mentioned steps 8) in 1 gram of 40 mesh sieve material, totally 9 parts, add respectively in 9 beakers, be still placed at former temperature timing immediately;
3) after this 0.5,1,1.5,2,2.5 and 6 hours time, weigh, claim heavy rear colloid still to put into former water tumbler and continued water suction, weigh the weight of colloid in each beaker, average and be designated as the material water suction multiple under this time;
4) weighing technique: the circular stainless steel and irons sieve of cut-off footpath 20cm order number 20 objects, first on electronic balance, remove the peel, the water in beaker is poured in sieve together with colloid, be filtered dry after moisture, sieve is placed on balance and is weighed, record, is the water suction multiple of material;
Differing temps water suction result, as shown in Figure 3, temperature is higher, and water suction multiple is larger, and the time of the water suction that reaches capacity is shorter.70 ℃ time, reach the maximum 1 hour multiple time of water suction, multiple is 350 times, and normal temperature was issued to the maximum water suction multiple time at 1.5 hours, and multiple is 320 times, and-7 reach the maximum water suction multiple time at 2.5 hours while spending, are 300 times of left and right.In lower 6 hours of each temperature environment, water conservation is respond well.Illustrate that water-absorbing material performance prepared by the present invention is high.
Embodiment 2: regulating pondage
Irradiation is prepared 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:
The 1st part: 7 grams of starch, 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 40 grams, water;
The 2nd part: 7 grams of starch, 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 50 grams, water;
The 3rd part: 7 grams of starch, 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 60 grams, water;
The 4th part: 7 grams of starch, 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 70 grams, water;
The 5th part: 7 grams of starch, 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 80 grams, water;
2) starch is mixed with water, stir, be heated to 90 ℃ of gelatinizations, then add 5 grams of the sodium hydroxide solutions that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid of in ice bath, step 1) being chosen 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 fills with bag, excluding air, sealing, obtains mixture;
5) mixture of filling with after bag at normal temperature, irradiation source is
60under Co-gamma-rays, after irradiation 2kGy, room temperature is placed 8h left and right, 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, divides and be dried complete 3 times;
Enter microwave the 1st time: control microwave drying temperature and be no more than 80 ℃, strip colloid evenly tiles in 2 centimetres of thickness, and the water content of dried strip colloid reduces to 50%; Enter microwave the 2nd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave the 3rd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 3rd dried strip colloid reduces to 10%;
8) adopt the pulverizer powder material of drying, cross 40 mesh sieves, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, paper plastic bag packing, sealing).
Water absorbing properties test:
1) prepare 3 beakers that 1000 grams of tap water are housed, place stand-by at normal temperatures;
2) get above-mentioned steps 8) in 1 gram of 40 mesh sieve material, totally 3 parts, add respectively in 3 beakers, timing, after 1 hour, weighs the weight of colloid in each beaker, is designated as material water suction multiple, weighing technique is the same;
3) Using such method weighs the water suction multiple of pure water, physiological saline and urine;
4) pure water is distilled water; Physiological saline (0.9wt% sodium-chlor) preparation: take 9 grams of sodium-chlor, 991 grams of adding distil waters, stirring and dissolving, is formulated as 1000 grams, physiological saline; Basis urine preparation: 0.2 gram of Sodium phosphate dibasic, 0.30 gram of potassium primary phosphate, 18 grams, sodium-chlor, adding distil water to 1000 gram, obtain 1000 grams of artificial urine;
5) other liquid absorb water with step 2), repeat to average for 3 times.
Water suction result, in table 1.Five kinds of materials all meet national standard.In the time that starch, vinylformic acid, alkali number are consistent, regulating pondage can reduce take drying cost as main production 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 the water-absorbing material different solutions prepared of the present invention.）
Illustrate that water-absorbing material performance prepared by the present invention is high.
Embodiment 3: regulate alkali number
Irradiation is prepared 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:
The 1st part: choose 7 grams of starch, 44 grams, vinylformic acid, 47.6 grams of 32wt% aqueous sodium hydroxide solutions, 60 grams, water;
The 2nd part: choose 7 grams of starch, 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 60 grams, water;
2) starch is mixed with water, stir, be heated to 90 ℃ of gelatinizations, then add 5 grams of the sodium hydroxide solutions that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid of in ice bath, step 1) being chosen 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 fills with bag, excluding air, sealing, obtains mixture;
5) mixture of filling with after bag at normal temperature, irradiation source is
60under Co-gamma-rays, after 2kGy, room temperature is placed 8h left and right, 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, divides and be dried complete 3 times;
Enter microwave the 1st time: control microwave drying temperature and be no more than 80 ℃, strip colloid evenly tiles in 2 centimetres of thickness, and the water content of dried strip colloid reduces to 50%; Enter microwave the 2nd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave the 3rd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 3rd dried strip colloid reduces to 10%;
8) adopt the pulverizer powder material of drying, cross 40 mesh sieves, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, paper plastic bag packing, sealing).
Water absorbing properties test:
1) prepare 3 beakers that 1000 grams of tap water are housed, place stand-by at normal temperatures;
2) get above-mentioned steps 8) in 1 gram of 40 mesh sieve material, totally 3 parts, add respectively in 3 beakers, timing, after 1 hour, weighs the weight of colloid in each beaker, is designated as material water suction multiple, weighing technique is the same;
3) Using such method weighs the water suction multiple of pure water, physiological saline and urine;
4) pure water is distilled water; Physiology salt (0.9% sodium-chlor) preparation: take 9 grams of sodium-chlor, 991 grams of adding distil waters, stirring and dissolving, is formulated as 1000 grams, physiological saline; Basis urine preparation: 0.2 gram of Sodium phosphate dibasic, 0.30 gram of potassium primary phosphate, 18 grams, sodium-chlor, adding distil water to 1000 gram, obtain 1000 grams of artificial urine;
5) other liquid absorb water with step 2), repeat to average for 3 times.
Water suction result, in the time that starch, vinylformic acid, the water yield are consistent, suitably increases alkali number, can reduce raw materials cost, improves absorbed performance, and 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 is prepared the method for starch base high-absorbent material, comprises the steps:
1) choose 9 grams of starch, 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 60 grams, water, stand-by;
2) starch is mixed with water, stir, be heated to 90 ℃ of gelatinizations, then add 5 grams of the sodium hydroxide solutions that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid of in ice bath, step 1) being chosen 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 fills with bag, excluding air, sealing, obtains mixture;
5) mixture of filling with after bag at normal temperature, irradiation source is
60under Co-gamma-rays, after irradiation 1kGy, room temperature is placed 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 to point 3 times dry complete (note: while doing scanning electron microscope analysis, adopt lyophilize herein) together with pallet;
Enter microwave the 1st time: control microwave drying temperature and be no more than 80 ℃, strip colloid evenly tiles in 2 centimetres of thickness, and the water content of dried strip colloid reduces to 50%; Enter microwave the 2nd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave the 3rd time: control microwave drying temperature and be no more than 100 ℃, 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: while doing scanning electron microscope analysis, do not pulverize) herein, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, paper plastic bag packing, sealing).
Water absorbing properties test:
1) prepare 3 beakers that 1000 grams of tap water are housed, place stand-by at normal temperatures;
2) get above-mentioned steps 8) in 1 gram of 40 mesh sieve material, totally 3 parts, add respectively in 3 beakers, timing, after 1 hour, weighs the weight of colloid in each beaker, is designated as material water suction multiple, weighing technique is the same;
3) Using such method weighs the water suction multiple of pure water, physiological saline and urine;
4) pure water is distilled water; Physiology salt (0.9wt% sodium-chlor) preparation: take 9 grams of sodium-chlor, 991 grams of adding distil waters, stirring and dissolving, is formulated as 1000 grams, physiological saline; Basis urine preparation: 0.2 gram of Sodium phosphate dibasic, 0.30 gram of potassium primary phosphate, 18 grams, sodium-chlor, adding distil water to 1000 gram, obtain 1000 grams of artificial urine;
5) other liquid absorb water with step 2), repeat to average for 3 times.
Water suction result, in the time that vinylformic acid, sodium hydroxide, the water yield are consistent, suitably increases amount of starch, can reduce water-content and raw materials cost, keeps certain absorbed performance, and 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%.Absorption tap water, pure water, physiological saline and urine multiple more than 400,900,49 and 52, meet national standard respectively.Illustrate that water-absorbing material performance prepared by the present invention is high.
Embodiment 5: regulate amount of starch
Irradiation is prepared the method for starch base high-absorbent material, comprises the steps:
1) choose 6 grams of starch, 44 grams, vinylformic acid, 60.9 grams of 32wt% aqueous sodium hydroxide solutions, 60 grams, water, stand-by;
2) starch is mixed with water, stir, be heated to 90 ℃ of gelatinizations, then add 6 grams of the sodium hydroxide solutions that step 1) chooses, now starch paste becomes more transparent, obtains starch paste;
3) vinylformic acid of in ice bath, step 1) being chosen 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 fills with bag, excluding air, sealing, obtains mixture;
5) mixture of filling with after bag at normal temperature, irradiation source is
60under Co-gamma-rays, after irradiation 4kGy, room temperature is placed 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 to point 3 times dry complete (note: while doing scanning electron microscope analysis, adopt lyophilize herein) together with pallet;
Enter microwave the 1st time: control microwave drying temperature and be no more than 80 ℃, strip colloid evenly tiles in 2 centimetres of thickness, and the water content of dried strip colloid reduces to 50%; Enter microwave the 2nd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 2nd dried strip colloid reduces to 30%; Enter microwave the 3rd time: control microwave drying temperature and be no more than 100 ℃, 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: while doing scanning electron microscope analysis, do not pulverize) herein, obtain irradiation and prepare starch base high-absorbent material (product adopts zip lock bag encapsulation, paper plastic bag packing, sealing).
Water absorbing properties test:
1) prepare 3 beakers that 1000 grams of tap water are housed, place stand-by at normal temperatures;
2) get above-mentioned steps 8) in 1 gram of 40 mesh sieve material, totally 3 parts, add respectively in 3 beakers, timing, after 1 hour, weighs the weight of colloid in each beaker, is designated as material water suction multiple, weighing technique is the same;
3) Using such method weighs the water suction multiple of pure water, physiological saline and urine;
4) pure water is distilled water; Physiology salt (0.9wt% sodium-chlor) preparation: take 9 grams of sodium-chlor, 991 grams of adding distil waters, stirring and dissolving, is formulated as 1000 grams, physiological saline; Basis urine preparation: 0.2 gram of Sodium phosphate dibasic, 0.30 gram of potassium primary phosphate, 18 grams, sodium-chlor, adding distil water to 1000 gram, obtain 1000 grams of artificial urine;
5) other liquid absorb water with step 2), repeat to average for 3 times.
Water suction result, in the time that vinylformic acid, sodium hydroxide, the water yield are consistent, suitably increases amount of starch, can reduce water-content and raw materials cost, keeps certain absorbed performance, and 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%.Absorption tap water, pure water, physiological saline and urine multiple more than 700,1200,65 and 70, meet national standard respectively.Illustrate that water-absorbing material performance prepared by the present invention is high.
Claims (7)
1. irradiation is prepared 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) starch that the water of step 1) being chosen is chosen with step 1) mixes, and stirs, heats gelatinization, then adds a small amount of sodium hydroxide solution, obtains starch paste;
3) remaining sodium hydroxide solution is placed in ice bath, in the vinylformic acid hydrogen injecting sodium hydroxide solution 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 pour in plastics bag, excluding air, sealing, obtains mixture;
5) mixture of being prepared by step 4) is under normal temperature, irradiation source after irradiation 1～4kGy, and room temperature is placed 8h left and right, obtains colloid;
6) colloid step 5) being obtained is placed in mincer and rubs into strips, obtains strip colloid;
7) strip colloid step 6) being obtained is laid in plastic pallet, is placed in microwave drying oven, and stage drying is to constant weight;
8) adopt pulverizer pulverising step 7) drying material that obtains, cross 20～100 mesh sieves, obtain irradiation and prepare starch base high-absorbent material.
2. irradiation according to claim 1 is prepared the method for starch base high-absorbent material, it is characterized in that: the starch in step 1) is any one in fry starch of konjak, W-Gum etc.
3. irradiation according to claim 1 is prepared the method for starch base high-absorbent material, it is characterized in that: the concentration of the sodium hydroxide solution in step 1) is 32wt%.
4. irradiation according to claim 1 is prepared the method for starch base high-absorbent material, it is characterized in that: step 2) in heating temperature be 90 ℃.
5. irradiation according to claim 1 is prepared the method for starch base high-absorbent material, it is characterized in that: step 2) in sodium hydroxide solution add-on be the 8.2-10.5% of the sodium hydroxide solution total mass chosen of step 1).
6. irradiation according to claim 1 is prepared the method for starch base high-absorbent material, it is characterized in that: in step 5), irradiation source is
60any one in Co-gamma-rays, x ray, electron beam etc., preferably
60co-gamma-rays.
7. irradiation according to claim 1 is prepared the method for starch base high-absorbent material, it is characterized in that: in step 7), divide three sections to be dried, enter microwave the 1st time: control microwave drying temperature and be no more than 80 ℃, strip colloid evenly tiles in 2 centimetres of thickness, and the water content of dried strip colloid is reduced to 35-50%; Enter microwave the 2nd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 2nd dried strip colloid is reduced to 20-30%; Enter microwave the 3rd time: control microwave drying temperature and be no more than 100 ℃, the water content of the 3rd dried strip colloid is reduced to 8-12%.
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| CN105884974A (en) * | 2016-06-14 | 2016-08-24 | 四川省农业科学院生物技术核技术研究所 | Segmented drying method for starch system water-absorbent resin |
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