CN104072670B - The method that carboxymethyl potato slag prepares nitrogenous potassium high hydroscopic resin - Google Patents
The method that carboxymethyl potato slag prepares nitrogenous potassium high hydroscopic resin Download PDFInfo
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- CN104072670B CN104072670B CN201410319553.3A CN201410319553A CN104072670B CN 104072670 B CN104072670 B CN 104072670B CN 201410319553 A CN201410319553 A CN 201410319553A CN 104072670 B CN104072670 B CN 104072670B
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- hydroscopic resin
- potato slag
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Abstract
The invention discloses the method that carboxymethyl potato slag prepares nitrogenous potassium high hydroscopic resin,Main technique is under ice-water bath cooling,With potassium hydroxide solution neutralization reaction is carried out with removing the acrylic acid of polymerization inhibitor,Solution after neutralization is added and fills carboxymethyl potato slag,Acrylamide,Potassium peroxydisulfate,Sodium hydrogensulfite,N,N ＇ methylene-bisacrylamides,In the reaction vessel of deionized water,Stir under nitrogen protection,Heating water bath,Stop stirring at 25 45 DEG C,1 2h is incubated in boiling water bath,Then logical nitrogen is stopped,Product is taken out,It is cut into small pieces,Constant weight is dried in 40 DEG C 60 DEG C of baking oven,Crush,Produce the nitrogenous potassium high hydroscopic resin of carboxymethyl potato slag preparation,High hydroscopic resin prepared by this method is compared with similar products,Its water absorption, which has, to be greatly improved and to prepare cost low,The water tariff collection of soil in arid area,Desert preventing and treating and plant growth etc. have good application prospect.
Description
Technical field
The present invention relates to the preparation method for the field such as agricultural, forestry, gardening high hydroscopic resin.High hydroscopic resin is wide
General to be applied to above-mentioned field, product of the invention is due to rationally using discarded potato residues, substantially reducing cost of material, and answer
Polymerization temperature is substantially reduced with redox initiator so that the high hydroscopic resin function admirable of preparation, is had extensively in above-mentioned field
Wealthy application prospect.
Background technology
Substantial amounts of abandoned white potato slag is produced in farina production process, general starch per ton produces 7.5 tons of waste residues,
Bed drain purge is very big, if do not recycled, not only causes the waste of resource, and cause serious environmental pollution.Discarded
Potato residues contain abundant starch and cellulose, and starch and content of cellulose are respectively in 37% He in general potato residues butt
17% or so, if these starch and cellulose can be made full use of to prepare high hydroscopic resin and carry out comprehensive development and utilization to potato slag, no
It is only capable of reducing environmental pollution, moreover it is possible to efficent use of resources, there is preferable economic benefit and social benefit.
Super absorbent resin is a kind of functional high molecule material developed rapidly in recent years, and it not only has very high
Water absorption, and dehydration is not easy in the case of pressurization after absorbing water, thus be widely used in agricultural, gardens and desert and control
The fields such as reason.Starch-series and cellulose-based high hydroscopic resin play an important role in agricultural, forestry, gardening etc., and it can
To strengthen the ability of soil water sorption and water conservation, improve the crumb structure of soil, make loosing soil so that gas permeability, the soil of soil
The day and night temperature of earth is all improved.It can also increase soil fertility, strengthen the drought-resistant ability of plant.As water-loss reducer of soil, it
Substantial amounts of water can be absorbed when soil water amount enriches, and and can discharges water outlet when soil water shortage, as formed in plant root
One small reservoir, is continuing to supply the moisture needed for plant.Greatly reduce body surface moisture evaporation simultaneously, that is applied on crops is straight
It is to improve the water holding capacity of soil to connect effect.
The content of the invention
The technical problem to be solved in the present invention is to provide the method that carboxymethyl potato slag prepares nitrogenous potassium high hydroscopic resin,
This preparation method mainly with potato residues, acrylic acid, acrylamide, potassium hydroxide, potassium peroxydisulfate, sodium hydrogensulfite, N, N ＇-
Methylene-bisacrylamide etc. is raw material, and through rational proportion, high hydroscopic resin is made by certain technical process.
The technical problem of the present invention is solved by following scheme：Carboxymethyl potato slag prepares nitrogenous potassium high hydroscopic resin
Method, it is characterized in that：Potassium hydroxide solution is prepared, under the cooling of ice-water bath, is neutralized with the potassium hydroxide solution prepared
The acrylic acid of polymerization inhibitor is removed, carboxymethyl potato slag, acrylic acid, the mass ratio of potassium hydroxide are 1：2-20：0.62-6.99,
By the acrylic acid after neutralization and its sylvite, carboxymethyl potato slag, acrylamide, potassium peroxydisulfate, sodium hydrogensulfite, N, N ＇-Asia
Bisacrylamide mixes with 50ml deionized water, stirs 1.0 hours, wherein carboxymethyl potato slag, acrylic acid, propylene
Acid amides, potassium peroxydisulfate, sodium hydrogensulfite, N, N ＇-methylene-bisacrylamide, the mass ratio of the total deionized water of system are 1:2.0-
20.0:0.5-5:0.050-0.250：0.0385-0.1925：0.015-0.050:45.0-85.0, under the protection of nitrogen, water
Bath is heated and stirred, and stops stirring when temperature rises to 25-45 DEG C, and 1-2 hours are incubated in boiling water bath, then stops logical nitrogen
Gas, product is taken out, cut into fritter, constant weight is dried in 40 DEG C -60 DEG C of baking oven, crushed, produce high hydroscopic resin.
The method that carboxymethyl potato slag described in above-mentioned technical proposal prepares nitrogenous potassium high hydroscopic resin, wherein system are total
The weight of deionized water is preparation potassium hydroxide solution, dissolving carboxymethyl potato slag, acrylamide, potassium peroxydisulfate, sulfurous acid
Hydrogen sodium, N, the summation of N ＇-deionized water needed for methylene-bisacrylamide.
Carboxymethyl potato slag described in above-mentioned technical proposal prepares carboxymethyl Ma Ling in the method for nitrogenous potassium high hydroscopic resin
Potato slag, acrylic acid, acrylamide, potassium peroxydisulfate, sodium hydrogensulfite, N, N ＇-methylene-bisacrylamide, the total deionized water of system
Mass ratio be 1:2.0-20.0:0.5-5:0.050-0.250：0.0385-0.1925：0.015-0.050:It is 45.0-85.0 excellent
It is mass ratio 1 to match ratio:10.0-18.0:2.5-4.5：0.100-0.200：0.077-0.154：0.020-0.040:55.0-
75.0。
It is an advantage of the invention that：1st, the rate of water absorption of the product is than very fast, and water absorption rate is high, up to 1500g/g, much
It has been higher by like product on the market.2nd, there is its highest water absorption using carboxymethyl potato slag as raw material in the product
Acrylic acid degree of neutralization it is higher 60%, thus substantially reduce the cost of product.3rd, due to carboxymethyl potato preparation method
Simply, raw material potato residues cost is very low so that production of resins cost substantially reduces.4th, because carboxymethyl potato slag has
It preferable dissolubility, can just be dissolved in cold water, eliminate the tedious steps of starch gelatinization when tradition prepares high hydroscopic resin, make
It is simple to obtain synthesis technique.5. the initiator of this method is the redox initiator that potassium peroxydisulfate and sodium hydrogensulfite are formed,
Initiation temperature can be significantly reduced, and initiation reaction relaxes, and greatlys save cost, reduces the requirement to equipment.
Carboxymethyl potato slag of the present invention prepares nitrogenous potassium high hydroscopic resin and is mainly used in agriculture, woods, animal husbandry, while may be used also
For water and soil conservation, high hydroscopic resin can change the crumb structure of soil, increase water penetration, the gas permeability of soil, dry
Play the role of in terms of the water tariff collection of non-irrigated Soils In The Region, desert preventing and treating it is very big, and can also provide that it grows for plant must
The nitrogen and potassium element needed.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart that carboxymethyl potato slag prepares nitrogenous potassium high hydroscopic resin；
Fig. 2 is carboxymethyl potato slag and total monomer（Fixed acrylic acid and propylene amine amide mass ratio 4:1）Mass ratio pair
The influence curve of high hydroscopic resin water absorption rate；
Fig. 3 is influence curve of the acrylic acid with the proportion of acylamide to high hydroscopic resin water absorption rate；
Fig. 4 is influence curve of the degree of neutralization to high hydroscopic resin water absorption rate of acrylic acid；
Fig. 5 is influence curve of the dosage of crosslinking agent to high hydroscopic resin water absorption rate；
Fig. 6 is redox initiator dosage（Fixed potassium peroxydisulfate and sodium hydrogensulfite mass ratio 1:0.77）To high water absorption
The influence curve of resin water absorption rate；
Fig. 7 is influence curve of the content of water in system to high hydroscopic resin water absorption rate；
Fig. 8 is the infrared spectrum of the high hydroscopic resin by taking embodiment 4 as an example.
Embodiment
Embodiment 1：3.64g potassium hydroxide is weighed, 20.0ml deionized waters is measured, is configured to potassium hydroxide solution, in ice
Under conditions of water-bath cooling and stirring, 9.375g is neutralized（8.93ml）Acrylic acid.Weigh 2.50g carboxymethyl potatos slag,
3.125g acrylamides, 150.00mg potassium peroxydisulfates, 115.5mg sodium hydrogensulfites, 25.00mg N, N ＇-methylene bisacrylamide acyl
Amine, 25.0ml deionized waters are measured, are all added in reactor, and obtained acrylic acid and its potassium salt soln are poured into instead
Device is answered, stirs 1.0h at room temperature, makes it well mixed.Stir, heat under the protection of nitrogen, while control firing rate,
Bath temperature is slowly raised, stop stirring when temperature rises to 30-35 DEG C.Hereafter gradually heating, when the water in water-bath reaches
After boiling, continuing heating makes it react 1-2h in the temperature range, stops logical nitrogen, is cooled to room temperature.Product is taken out, will
It cuts into fritter, is dried in 40 DEG C of -60 DEG C of baking ovens, and the degree of neutralization that acrylic acid is produced through crushing is 50% high hydroscopic resin,
Water absorption reaches 1175g/g.
Embodiment 2：2.91g potassium hydroxide is weighed, 20.0ml deionized waters is measured, is configured to potassium hydroxide solution, in ice
Under conditions of water-bath cooling and stirring, 7.5g is neutralized（7.14ml）Acrylic acid.Weigh 2.50g carboxymethyl potatos slag, 7.5g third
Acrylamide, 250.00mg potassium peroxydisulfates, 192.5mg sodium hydrogensulfites, 30.00mg N, N ＇-methylene-bisacrylamides, are measured
25.0ml deionized waters, are all added in reactor, and obtained acrylic acid and its potassium salt soln are poured into reactor, in
1.0h is stirred at room temperature, makes it well mixed.Stir, heat under the protection of nitrogen, while control firing rate, make water-bath temperature
Degree slowly rise, stops stirring when temperature rises to 25-30 DEG C.Hereafter gradually heating, after the water in water-bath reaches boiling, after
Continuous heating makes it react 1-2h in the temperature range, stops logical nitrogen, is cooled to room temperature.Product is taken out, cut into
Fritter, dried in 40 DEG C of -60 DEG C of baking ovens, the degree of neutralization that acrylic acid is produced through crushing is 50% high hydroscopic resin, and water absorption reaches
1200g/g。
Embodiment 3：6.12g potassium hydroxide is weighed, 20.0ml deionized waters is measured, is configured to potassium hydroxide solution, in ice
Under conditions of water-bath cooling and stirring, 13.125g is neutralized（12.5ml）Acrylic acid.Weigh 2.50g carboxymethyl potatos slag,
1.875g acrylamides, 100.00mg potassium peroxydisulfates, 77.0mg sodium hydrogensulfites, 25.00mg N, N ＇-methylene bisacrylamide acyl
Amine, 25.0ml deionized waters are measured, are all added in reactor, and obtained acrylic acid and its potassium salt soln are poured into instead
Device is answered, stirs 1.0h at room temperature, makes it well mixed.Stir, heat under the protection of nitrogen, while control firing rate,
Bath temperature is slowly raised, stop stirring when temperature rises to 40-45 DEG C.Hereafter gradually heating, when the water in water-bath reaches
After boiling, continuing heating makes it react 1-2h in the temperature range, stops logical nitrogen, is cooled to room temperature.Product is taken out, will
It cuts into fritter, is dried in 40 DEG C of -60 DEG C of baking ovens, and the degree of neutralization that acrylic acid is produced through crushing is 60% high hydroscopic resin,
Water absorption reaches 1260g/g.
Embodiment 4：5.95g potassium hydroxide is weighed, 20.0ml deionized waters is measured, is configured to potassium hydroxide solution, in ice
Under conditions of water-bath cooling and stirring, 15.313g is neutralized（14.58ml）Acrylic acid.Weigh 2.50g carboxymethyl potatos slag,
2.187g acrylamides, 200.00mg potassium peroxydisulfates, 154.0mg sodium hydrogensulfites, 20.00mg N, N ＇-methylene bisacrylamide acyl
Amine, 25.0ml deionized waters are measured, are all added in reactor, and obtained acrylic acid and its potassium salt soln are poured into instead
Device is answered, stirs 1.0h at room temperature, makes it well mixed.Stir, heat under the protection of nitrogen, while control firing rate,
Bath temperature is slowly raised, stop stirring when temperature rises to 35-40 DEG C.Hereafter gradually heating, when the water in water-bath reaches
After boiling, continuing heating makes it react 1-2h in the temperature range, stops logical nitrogen, is cooled to room temperature.Product is taken out, will
It cuts into fritter, is dried in 40 DEG C of -60 DEG C of baking ovens, and the degree of neutralization that acrylic acid is produced through crushing is 50% high hydroscopic resin,
Water absorption reaches 1300g/g.
Embodiment 5：6.99g potassium hydroxide is weighed, 20.0ml deionized waters is measured, is configured to potassium hydroxide solution, in ice
Under conditions of water-bath cooling and stirring, 15.0g is neutralized（14.29ml）Acrylic acid.Weigh 2.50g carboxymethyl potatos slag, 5.0g
Acrylamide, 250.00mg potassium peroxydisulfates, 192.5mg sodium hydrogensulfites, 20.00mg N, N ＇-methylene-bisacrylamides, amount
25.0ml deionized waters are taken, are all added in reactor, and obtained acrylic acid and its potassium salt soln are poured into reactor,
1.0h is stirred at room temperature, makes it well mixed.Stir, heat under the protection of nitrogen, while control firing rate, make water-bath
Temperature slowly raises, and stops stirring when temperature rises to 25-30 DEG C.Hereafter gradually heating, after the water in water-bath reaches boiling,
Continuing heating makes it react 1-2h in the temperature range, stops logical nitrogen, is cooled to room temperature.Product is taken out, sheared
Into fritter, dried in 40 DEG C of -60 DEG C of baking ovens, the degree of neutralization that acrylic acid is produced through crushing is 50% high hydroscopic resin, water absorption
Up to 1500g/g.
Embodiment 6：5.25g potassium hydroxide is weighed, 20.0ml deionized waters is measured, is configured to potassium hydroxide solution, in ice
Under conditions of water-bath cooling and stirring, 11.25g is neutralized（10.70ml）Acrylic acid.Weigh 2.50g carboxymethyl potatos slag,
3.75g acrylamides, 100.00mg potassium peroxydisulfates, 77.00mg sodium hydrogensulfites, 20.00mg N, N ＇-methylene bisacrylamide acyl
Amine, 25.0ml deionized waters are measured, are all added in reactor, and obtained acrylic acid and its potassium salt soln are poured into instead
Device is answered, stirs 1.0h at room temperature, makes it well mixed.Stir, heat under the protection of nitrogen, while control firing rate,
Bath temperature is slowly raised, stop stirring when temperature rises to 25-30 DEG C.Hereafter gradually heating, when the water in water-bath reaches
After boiling, continuing heating makes it react 1-2h in the temperature range, stops logical nitrogen, is cooled to room temperature.Product is taken out, will
It cuts into fritter, is dried in 40 DEG C of -60 DEG C of baking ovens, and the degree of neutralization that acrylic acid is produced through crushing is 50% high hydroscopic resin,
Water absorption reaches 1090g/g.
Embodiment 7：5.25g potassium hydroxide is weighed, 20.0ml deionized waters is measured, is configured to potassium hydroxide solution, in ice
Under conditions of water-bath cooling and stirring, 11.25g is neutralized（10.70ml）Acrylic acid.Weigh 2.50g carboxymethyl potatos slag,
3.75g acrylamides, 100.00mg potassium peroxydisulfates, 77.00mg sodium hydrogensulfites, 50.00mg N, N ＇-methylene bisacrylamide acyl
Amine, 25.0ml deionized waters are measured, are all added in reactor, and obtained acrylic acid and its potassium salt soln are poured into instead
Device is answered, stirs 1.0h at room temperature, makes it well mixed.Stir, heat under the protection of nitrogen, while control firing rate,
Bath temperature is slowly raised, stop stirring when temperature rises to 25-30 DEG C.Hereafter gradually heating, when the water in water-bath reaches
After boiling, continuing heating makes it react 1-2h in the temperature range, stops logical nitrogen, is cooled to room temperature.Product is taken out, will
It cuts into fritter, is dried in 40 DEG C of -60 DEG C of baking ovens, and the degree of neutralization that acrylic acid is produced through crushing is 50% high hydroscopic resin,
Water absorption reaches 494g/g.
By taking the product of the gained of embodiment 4 as an example, infrared spectrum is via NEXUSTM 670 FT-IR E.S.P types are red
External spectrum instrument measurement result is as shown in Figure 8.
Determined through the German type elementary analysis instruments of Elementar Vario EL III, the element by taking the product of embodiment 1 as an example
Content is：N%=2.81, C%=38.00, H%=5.128.
Claims (3)
1. the method that carboxymethyl potato slag prepares nitrogenous potassium high hydroscopic resin, it is characterized in that:Potassium hydroxide solution is prepared, in ice
Under water-bath cooling, with the acrylic acid in the potassium hydroxide solution prepared with removing polymerization inhibitor, wherein carboxymethyl potato slag, third
The mass ratio of olefin(e) acid and potassium hydroxide is 1:2~20:0.62 ~ 6.99, by the acrylic acid after neutralization and its sylvite, carboxymethyl Ma Ling
Potato slag, acrylamide, potassium peroxydisulfate, sodium hydrogensulfite, N, N '-methylene-bisacrylamide mix with 50ml deionized water,
Stirring 1 hour, wherein carboxymethyl potato slag, acrylic acid, acrylamide, potassium peroxydisulfate, sodium hydrogensulfite, N, N '-methylene
The mass ratio of the total deionized water of double acryloyls, system is 1:2.0~20.0:0.5~5:0.050~0.250:0.0385~0.1925:
0.015~0.050:45.0 ~ 85.0, under the protection of nitrogen, heating water bath simultaneously stirs, and stops stirring when temperature rises to 25 ~ 45 DEG C
Mix, 1 ~ 2 hour is incubated in boiling water bath, then stop logical nitrogen, product is taken out, cuts into fritter, in 40 DEG C ~ 60 DEG C of baking
Constant weight is dried in case, crushes, produces high hydroscopic resin.
2. the method that carboxymethyl potato slag according to claim 1 prepares nitrogenous potassium high hydroscopic resin, wherein carboxymethyl
Potato residues, acrylic acid, acrylamide, potassium peroxydisulfate, sodium hydrogensulfite, N,N methylene bis acrylamide, system always go from
Total proportioning of sub- water is 1:10.0~18.0:2.5~4.5:0.100~0.200:0.077~0.154:0.020~0.040:55.0~
75.0。
3. carboxymethyl potato slag according to claim 1 prepares the method for nitrogenous potassium high hydroscopic resin, total deionized water
Measure to prepare potassium hydroxide solution and dissolving carboxymethyl potato slag, acrylamide, potassium peroxydisulfate, sodium hydrogensulfite, N, N '-Asia
The total amount of deionized water used in bisacrylamide.
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| CN101935380A (en) * | 2010-10-09 | 2011-01-05 | 内蒙古大学 | Method for preparing potassium- and nitrogen-containing high water-absorbent resin from carboxymethyl potato starch serving as raw material |
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| CN101935380A (en) * | 2010-10-09 | 2011-01-05 | 内蒙古大学 | Method for preparing potassium- and nitrogen-containing high water-absorbent resin from carboxymethyl potato starch serving as raw material |
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| "马铃薯淀粉渣制备羧甲基纤维素和羧甲基淀粉混合物的研究;白仲兰等;《安徽农业科学》;20101120;第38卷(第33期);19063-19065 * |
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