CN101418075B - Method for preparing poly-aspartic potassium used in plant growth accelerator and use - Google Patents
Method for preparing poly-aspartic potassium used in plant growth accelerator and use Download PDFInfo
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Abstract
The invention belongs to the technical field of fertilizer, and in particular relates to a preparation method and application of poly-aspartic potassium used for plant growth accelerators. Poly-succinimide is generated from aspartate by a thermal polymerization method under the combined effect of boric acid and potassium (hydrogen) sulfate as catalysts, and the catalysts directly hydrolyze the Poly-succinimide into the poly-aspartic potassium without separation under the action of potassium hydroxide. Poly-aspartic acid synthesized by the method has the characteristics of uniform molecular weight distribution, high purity and high yield; moreover, as the boric acid and the potassium (hydrogen) sulfate added as catalysts are not separated from a product, production process is simplified; in addition, the contained boric acid and potassium (hydrogen) sulfate can be used as the plant growth accelerators and can be directly used as additives for nitrogen fertilizer synergism. Compared with the common poly-aspartic acid, the poly-aspartic potassium can improve the rate that plants utilize nitrogen fertilizer, and boron, potassium and sulfur in the poly-aspartic potassium can improve nutritional components. Experiments prove that the poly-aspartic acid synthesized by the method not only can increase the rate that plants utilize nitrogen fertilizer, but also balances the nutritional components of the nitrogen fertilizer.
Description
Technical field
The invention belongs to technical field of fertilizer, be specifically related to a kind of preparation method and application that is used for the poly-aspartic potassium of plant growth promoter.
Background technology
Chemical fertilizer plays a part crucial in crop yield increases, and according to Food and Argriculture OrganizationFAO (FAO) external statistical information is for many years shown, chemical fertilizer accounts for 40%～60% to the volume increase role.In n p k fertilizer, nitrogenous fertilizer accounts for more than 70% in the usage quantity of China.According to statistics, there is the arable land less than the world 10% in China, but the usage quantity of nitrogenous fertilizer has reached first place, the world, accounts for the nearly 30% of the world, and also has ever-increasing trend.The developed country farm crop are 50%～60% to the utilization ratio of nitrogenous fertilizer at present, and China is commonly 30%, and the rate of loss of nitrogenous fertilizer reaches about 70%, more than 80 ten thousand tons of the loss amounts of annual nitrogenous fertilizer.The research of widespread pollution from the overuse of fertilizers and pesticides in rural area control seminar of the international co-operation council draws: half of China's amount of application of nitrogen fertilizer just lost in the atmosphere or from escape canal with the gas form ease before by crop absorption and is lost to the water body environment, not only utilization rate of nitrogen fertilizer is low, and environment is caused significant damage.In order to remedy the loss of nitrogenous fertilizer, often append more nitrogenous fertilizer, the nitrogenous fertilizer of high density is higher by the speed that ammonia volatilization, nitrated-denitrification run off, and so not only farm crop is produced little effect, and causes the rising of fertilising cost, more resources waste, increasing environmental pollution or the like.U.S. Pat P5,814,582 have proposed a kind of poly aspartic acid that adds in chemical fertilizer, can improve to promote the absorption of plant to chemical fertilizer, China specially ZL200410055161.7 has proposed a kind of synergistic urea, promptly adds 0.01%～10% poly-aspartic potassium in urea.
People have recognized that poly aspartic acid has enrichment, promotes the function of plant absorbing nutrient, and because it has biodegradable performance, are a kind of plant growth promoters of environment-friendly type, have become the hot subject of fertilizer synergistic research at present.
Thermopolymerization about aspartic acid, United States Patent (USP) USP5 in the existing technology, 221,733, USP5,288,783, USP5,373,086 have all proposed to make aspartic acid carry out thermopolymerization under 220 ℃～300 ℃ in the mode of solid state reaction, reaction 6～9hr is with the poly-epoxy succinic imide of being converted into of aspartic acid, and then under the NaOH effect, be hydrolyzed to poly aspartic acid, in order to improve conversion of raw material, make aspartic acid reaction for a long time under hot conditions in these patents, the poly aspartic acid of this method preparation presents brown to Vandyke brown, temperature is higher, and color is darker, and range of molecular weight distributions is wide.
In order to reduce the pigment of temperature of reaction, shortening reaction times, reduction poly aspartic acid, U.S. Pat P5,142,062 proposed a kind of under the katalysis of phosphoric acid or polyphosphoric acid, mode with solid state reaction makes aspartic acid carry out thermopolymerization under 200 ℃, and the transformation efficiency of reaction 4hr aspartic acid is 98%.But in this method in order to improve transformation efficiency, the phosphoric acid that adds a large amount of middle strong types, wherein the ratio of phosphoric acid and raw material aspartic acid is 0.3:1～1:1, just must increase postprocessing working procedures such as some loaded down with trivial details washings, separation, drying in order to remove these catalyzer, and the required equipment of these postprocessing working procedures must be corrosion-resistant, the adding of in addition a large amount of liquid-phase catalyst phosphoric acid, making that heat polymerization is as easy as rolling off a log is clamminess or lumps, hinder carrying out smoothly of polyreaction, make that this method is difficult to use in large-scale industrial reactor.United States Patent (USP) 5,610,264 have proposed at NaHSO
4Katalysis under, carry out the solid phase thermopolymerization at 200～260 ℃, but the catalyzer in this method promptly becomes molten state when temperature surpasses 150 ℃, cause reaction mixture to be clamminess or lump, influence successful reaction and carry out, be difficult to large-scale industrial production.
U.S. Pat P5,292,864 have proposed to carry out polyreaction in the organic solvent tetramethylene sulfone, under the effect of catalyzer such as phosphoric acid, polyphosphoric acid, in 170～200 ℃ conditions polymerization can take place.This method has reduced the colourity of product poly aspartic acid owing in polymerization below 200 ℃, but owing to organic solvent need be separated from product, technology is very loaded down with trivial details, and cost also improves greatly.U.S. Pat P5,756,595 have proposed to carry out polyreaction in the organic solvent propylene carbonate, the problem that same existence will separate organic solvent.Chinese patent application 95192645.4 is carried out polycondensation with the aspartic acid monomer under the effect of mixed solution that contains two kinds of aprotic polar solvents formations at least and an acidic catalyst, obtain polysuccinimide and make its its be hydrolyzed to poly aspartic acid, the problem that same existence will separate organic solvent and catalyzer.But toxilic acid, generate the amine salt of toxilic acid then with the ammoniacal liquor reaction, the amine salt of toxilic acid is carried out thermal polycondensation at a certain temperature obtain poly-succinic diamide, separate drying and go out poly-succinic diamide, cyclodehydration generates polysuccinimide at a certain temperature again, at last the sodium salt of hydrolysis poly aspartic acid under the effect of aqueous sodium hydroxide solution.
Along with poly aspartic acid application as plant growth promoter in agricultural increases day by day, produce low-cost, as to be easy to carry out large-scale industrial production Technology effectively and become more and more important.Therefore need a kind of more convenient catalyzer, this catalyzer not only can shorten the reaction times and improve color, and in reaction, do not lump, it is convenient to handle, be easy to realize suitability for industrialized production, and need not to remove catalyzer from product, can be directly used in fertilizer additive, catalyst themselves also can be used as the nutritive ingredient of chemical fertilizer.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application that is used for the poly-aspartic potassium of plant growth promoter.This catalyzer not only can reduce polymeric reaction temperature, shortens the reaction times and improve the product color, and in reaction, do not lump and be easy to realize suitability for industrialized production, with overcome polymerization temperature height in the existing method, the time is long, colourity is dark, the polymerization process that is easy to lump.
For achieving the above object, the inventor finds that by further investigation boric acid, sulfuric acid (hydrogen) have the advantage that reduces polymerization temperature, shortening reaction times, improves the product color though potassium is done separately when catalyzer uses, but its advantage is not obvious, but when boric acid and vitriolate of tartar are used, the temperature and time of polyreaction can be reduced, the colourity of reaction product can be improved again.
The preparation method of the poly-aspartic potassium that is used for plant growth promoter that the present invention proposes, concrete steps are as follows:
With catalyzer boric acid, catalyst sulfuric acid potassium or sal enixum and raw material aspartic acid thorough mixing, make mixture in kneader or reactor, carry out heat polymerization then, obtain polysuccinimide, cooling is a poly-aspartic potassium with hydrolysis of polysuccinimide under the effect of potassium hydroxide; Wherein, the adding total amount of catalyzer boric acid and catalyst sulfuric acid potassium or sal enixum and the mol ratio of aspartic acid are 0.05:1～1:1, and the mol ratio of catalyzer boric acid and catalyst sulfuric acid potassium or sal enixum is 0.1:1～1:1.
Among the present invention, described blending means can be with catalyzer boric acid, catalyst sulfuric acid potassium or sal enixum and aspartic acid dissolving in the aqueous solution, then mixing solutions is carried out drying, boric acid wherein and sulfuric acid (hydrogen) potassium is distributed in the aspartic acid equably; Perhaps catalyzer boric acid, catalyst sulfuric acid potassium or sal enixum and aspartic acid directly can be mixed, fully grind, make in catalyzer boric acid and sulfuric acid (hydrogen) potassium and the aspartic acid mixed in together equably.
The inventor is through discovering that the adding total amount of the catalyzer that associating is used and the mol ratio of aspartic acid are 0.05:1～1:1.When containing relatively large boron, potassium, sulphur in the expectation end product, can use relatively large catalyzer.If need, the integral molar quantity of catalyzer boric acid and sulfuric acid (hydrogen) potassium can reach 1:1 with the ratio of the molar weight of aspartic acid.
Used boric acid is commercially available technical grade product among the present invention, and its molecular formula is H
3BO
3
Used vitriolate of tartar is commercially available product among the present invention, and its molecular formula is K
2SO
4
Used sal enixum is commercially available product among the present invention, and its molecular formula is KHSO
4
Boric acid used among the present invention uses as the boracic trace element fertilizer on agricultural, and many farm crop are had fertilizer efficiency, can promote crops quality and improve output.The used vitriolate of tartar of the present invention is a kind of widely used chemical fertilizer.The used sal enixum of the present invention changes vitriolate of tartar in hydrolytic process.Boric acid, vitriolate of tartar itself not because in above-mentioned reaction as catalyzer but its application suffer damage.Therefore when being used for fertilizer additive as plant growth promoter with present method synthetic poly aspartic acid, needn't remove catalyzer boric acid and vitriolate of tartar, because boric acid and vitriolate of tartar can play optimization function and balanced plant nutrient ingredient effect with aspartic acid.
The poly-aspartic potassium of boracic of the present invention and sulphur can directly be added in the chemical fertilizer as nitrogenous fertilizer (volatile salt, urea) and potash fertilizer (vitriolate of tartar), and adding part by weight is 0.1～10%, and the add-on of poly-aspartic potassium is 0.1g-10g in promptly every 100g chemical fertilizer.The mode of adding can be the chemical fertilizer thorough mixing under poly aspartic acid solution and aqueous solution state or the molten state, carries out granulation then.
The present invention has following advantage: (1) poly-aspartic potassium proposed by the invention is to carry out under the associating katalysis of boric acid and sulfuric acid (hydrogen) potassium, compare with traditional poly aspartic acid thermopolymerization, have that temperature of reaction is low, the time is short, colourity is low, molecular weight is issued uniform advantage; (2) used boric acid uses as the boracic trace element fertilizer on agricultural among the present invention, the used vitriolate of tartar of the present invention is a kind of widely used chemical fertilizer, and the used sal enixum of the present invention can change vitriolate of tartar in hydrolytic process, therefore when removing catalyzer with present method synthetic poly aspartic acid, can directly be added in the chemical fertilizer and use, nutritive ingredient that can balanced chemical fertilizer; (3) poly-aspartic potassium proposed by the invention belongs to amino acids, Biodegradable polymeric, is used for plant growth promoter, has effect safe, nontoxic, environmental protection; (4) poly-aspartic potassium proposed by the invention contains the required elements of plant-growth such as potassium, boron, sulphur, can improve the seed germination rate and the rate of being unearthed; (5) poly-aspartic potassium of the present invention's proposition can directly make an addition in the chemical fertilizer, can improve the utilization ratio of plant to chemical fertilizer, has the saving chemical fertilizer, reduces the peasant and drops into, and purifies the function of edatope.
Embodiment
Further describe positively effect of the present invention below by a series of embodiment and application examples.
Following Comparative Examples and the percentage ratio among the embodiment are weight percentage.Molecular weight is weight-average molecular weight.
In the Comparative Examples and embodiment of following poly aspartic acid preparation, the transformation efficiency of its aspartic acid in reaction is calculated as follows by weight-loss method:
If: the amount of monomer poly aspartic acid is a (g) before the polyreaction, and the catalyzer total amount is b (g), and the weight of polyreaction afterreaction mixture is x (g), and the weight of minimizing is the water that polycondensation loses:
The amount of the monomer aspartic acid that has then reacted is
Comparative Examples 1: the preparation of poly-aspartic potassium
The 133.00g aspartic acid is put into four-hole boiling flask be heated to about 220 ℃ in oil bath, after 9 hours, obtain the filemot polysuccinimide of 94.58g, according to weight-loss method, its transformation efficiency is 97.51%.The polysuccinimide of gained is added 133g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% dark brown red sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 8,600.
Embodiment 1: the preparation of poly-aspartic potassium
133.00g aspartic acid (1mol), 1.24g boric acid (0.02mol) and 5.22g vitriolate of tartar (0.03mol) are added in the 139.46g water, in rotatory evaporator, remove moisture after the dissolving again.Dried mixture is put into four-hole boiling flask and is heated to about 190 ℃ in oil bath, after 8.0 hours, obtains the lurid polysuccinimide of 104.11g, and according to weight-loss method, its transformation efficiency is 98.19%.The polysuccinimide of gained is added 133.00g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% yellow sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 8,750.
Embodiment 2: the preparation of poly-aspartic potassium
133.00g aspartic acid (1mol), 3.1g boric acid (0.05mol) and 8.70g vitriolate of tartar (0.05mol) are added in the 144.80g water, in rotatory evaporator, remove moisture then.Dried mixture is put into four-hole boiling flask and is heated to about 180 ℃ in oil bath, after 4.5 hours, obtains the lurid polysuccinimide of 109.02g, and according to weight-loss method, its transformation efficiency is 99.4%.The polysuccinimide of gained is added 133g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% yellow sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 8,600.
Embodiment 3: the preparation of poly-aspartic potassium
133.0g aspartic acid (1mol), 3.1g boric acid (0.05mol) and 8.7g vitriolate of tartar (0.05mol) are added in the 144.8g water, in rotatory evaporator, remove moisture then.Dried mixture is put into four-hole boiling flask and is heated to about 180 ℃ in oil bath, after 4.5 hours, obtains the lurid polysuccinimide of 109.0g, and according to weight-loss method, its transformation efficiency is 98.4%.The polysuccinimide of gained is added 133g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% yellow sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 8,600.
Embodiment 4: the preparation of poly-aspartic potassium
133.0g aspartic acid (1mol), 3.1g boric acid (0.05mol) and 8.7g vitriolate of tartar (0.05mol) are ground in mortar, the reaction mixture that will fully grind is put into four-hole boiling flask and is heated to about 180 ℃ in oil bath then, 4.5 after hour, obtain the lurid polysuccinimide of 109.2g, according to weight-loss method, its transformation efficiency is 98.9%.The polysuccinimide of gained is added 133g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% yellow sticking shape liquid, both poly aspartic acid potassium solution, wherein containing the molecular weight test is 8,900.
Embodiment 5: the preparation of poly-aspartic potassium
133.0g aspartic acid (1mol), 3.1g boric acid (0.05mol) and 6.8g sal enixum (0.05mol) are ground in mortar, the reaction mixture that will fully grind is put into four-hole boiling flask and is heated to about 180 ℃ in oil bath then, 3.5 after hour, obtain the polysuccinimide of 107.10g white, according to weight-loss method, its transformation efficiency is 99.4%.The polysuccinimide of gained is added 133.0g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% light yellow sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 9,100.
Embodiment 6: the preparation of poly-aspartic potassium
133.0g aspartic acid (1mol), 3.1g boric acid (0.05mol) and 17.4g vitriolate of tartar (0.10mol) are ground in mortar, the reaction mixture that will fully grind is put into four-hole boiling flask and is heated to about 180 ℃ in oil bath then, 3.5 after hour, obtain the polysuccinimide of 107.10g white, according to weight-loss method, its transformation efficiency is 99.4%.The polysuccinimide of gained is added 133.0g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% light yellow sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 9,100.
Embodiment 7: the preparation of poly-aspartic potassium
133.0g aspartic acid (1mol), 6.2g boric acid (0.10mol) and 26.1g vitriolate of tartar (0.15mol) are ground in mortar, the reaction mixture that will fully grind is put into four-hole boiling flask and is heated to about 180 ℃ in oil bath then, 3.5 after hour, obtain the polysuccinimide of 107.10g white, according to weight-loss method, its transformation efficiency is 99.4%.The polysuccinimide of gained is added 133.0g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% light yellow sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 9,100.
Embodiment 8: the preparation of poly-aspartic potassium
133.0g aspartic acid (1mol), 6.2g boric acid (0.10mol) and 26.1g vitriolate of tartar (0.15mol) are ground in mortar, the reaction mixture that will fully grind is put into four-hole boiling flask and is heated to about 180 ℃ in oil bath then, 3.5 after hour, obtain the polysuccinimide of 107.10g white, according to weight-loss method, its transformation efficiency is 99.4%.The polysuccinimide of gained is added 133.0g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% light yellow sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 9,100.
Embodiment 9: the preparation of poly-aspartic potassium
133.0g aspartic acid (1mol), 6.2g boric acid (0.10mol) and 26.1g vitriolate of tartar (0.15mol) are ground in mortar, the reaction mixture that will fully grind is put into four-hole boiling flask and is heated to about 180 ℃ in oil bath then, 3.5 after hour, obtain the polysuccinimide of 107.10g white, according to weight-loss method, its transformation efficiency is 99.4%.The polysuccinimide of gained is added 133.0g water and is heated to 70 ℃, and under this temperature, slowly add 25% potassium hydroxide aqueous solution 224g and be hydrolyzed, solid content be not less than 35% light yellow sticking shape liquid, both poly aspartic acid potassium solution, the molecular weight test is 9,100.
Embodiment 10: use the influence of poly-aspartic potassium of the present invention to pea seedlings percentage of germination and growth
Experiment is carried out in the round plastic basin of the band mesh that 3 diameters are 20cm, high 4cm, and every plastic tub can be cultivated the Semen Pisi sativi of dry weight 250g.Seed adopts commercially available preservation period to be no more than the Semen Pisi sativi in 1 year, tests used Semen Pisi sativi and all derives from same lot number.At first should choose seeds, reject and break seed and impurity residual, that damage by worms.Clean 2～3 times with clear water then, wash the dust on the seed off.Soak seed, with the aqueous solution soaking that contains poly-aspartic potassium that surpasses 2～3 times of seed volumes 20～24 hours, be dipped into seed and fully expand, wrinkle disappears, and visible through the seed coat can see that radicle is suitable.Soaked pea drop is gone excessive solution, and uniformly the shop is sprinkled upon in the plastic tub (plastic tub is earlier with the potassium permanganate sterilization, and spread toilet paper at the bottom of basin be matrix) then, takes off flat with hand.Spray every day the aqueous solution 2～3 times contain poly-aspartic potassium (spray with in the seedling dish not water for suitable).Observe and germinate and growing state.Experiment repeats 3 times, gets its mean value, the results are shown in Table 1.
Table 1 poly-aspartic potassium of the present invention is to the influence of pea seedlings percentage of germination and growth
As can be seen from Table 1, poly aspartic acid all has promoter action to the percentage of germination of pea seedlings and growth, and poly-aspartic potassium especially of the present invention is owing to contain elements such as potassium, boron, sulphur, and the germination and the growth of pea seedlings all had bigger promoter action.
Embodiment 11: use the influence of poly-aspartic potassium of the present invention to potted plant wheat growth
Present embodiment adopts the potted plant culture method of soil, uses the plastic tub of 16cm suitable for reading, end opening 12cm, dark 14cm, and every basin is adorned native 2kg, establishes 5 processing altogether, and each is handled and repeats 3 times, adopts the little wheat seeds of same packing bag.This test is handled as follows:
The processing of soaking seed earlier, the poly aspartic acid of wherein handle 1, handling the embodiment of the invention 2 of 2 usefulness 0.1mg/L soaks, and handles 3, handles 4, handles the immersion of 5 clear water.The immersion of wheat kind was implanted in the plastic tub after germinateing in about 15 days, every potted plant 20 strain rice shoots.In growth test, handle all equivalent fertilising 2 times for 5, wherein handle 1, handle the poly aspartic acid each 2 times that adds present embodiment 1 in 4, handle 3 and add commercially available poly aspartic acid each 2 times, handle 2 and do not add poly aspartic acid, handling 5 is the blank sample.Detailed process is as follows:
Handle 1: the rice shoot that germinates with the poly aspartic acid seed soaking of present embodiment 1 was implanted in the basin the 15th day, added the urea 50ml of mass concentration 1%, and the poly aspartic acid 50ml of 0.05mol/L present embodiment 2; Rice seedlings were implanted in the basin the 40th day, added the urea 50ml of mass concentration 1%, and the poly aspartic acid 50ml of 0.05mol/L present embodiment 2.
Handle 2: the rice shoot that germinates with the poly aspartic acid seed soaking of present embodiment 1 was implanted in the basin the 15th day, added the urea 50ml of mass concentration 1%, and clear water 50ml; Rice seedlings were implanted in the basin the 40th day, added the urea 50ml of mass concentration 1%, and clear water 50ml.
Handle 3: the rice shoot that germinates with the clear water seed soaking was implanted in the basin the 15th day, added the urea 50ml of mass concentration 1%, and the poly aspartic acid 50ml of 0.05mol/L present embodiment 2; Rice seedlings were implanted in the basin the 40th day, added the urea 50ml of mass concentration 1%, and the poly aspartic acid 50ml of 0.05mol/L present embodiment 2.
Handle 4: the rice shoot that germinates with the clear water seed soaking was implanted in the basin the 15th day, added the urea 50ml of mass concentration 1%, and the commercially available poly aspartic acid 50ml of 0.05mol/L; Rice seedlings were implanted in the basin the 40th day, added the urea 50ml of mass concentration 1%, and the commercially available poly aspartic acid 50ml of 0.05mol/L.
Handle 5 (blanks): the rice shoot that germinates with the clear water seed soaking was implanted in the basin the 15th day, added the urea 50ml of mass concentration 1%, and clear water 50ml; Rice seedlings were implanted in the basin the 40th day, added the urea 50ml of mass concentration 1%, and clear water 50ml.
Growing state after 60 days is shown in Table 2.
60 days growing state of table 2 wheat (cm) contrast
| Handle 1 | Handle 2 | Handle 3 | Handle 4 | Handle 5 | |
| Repeat 1 | 67 | 48 | 61 | 56 | 45 |
| Repeat 2 | 68 | 52 | 64 | 59 | 47 |
| Repeat 3 | 66 | 48 | 62 | 57 | 43 |
| Mean number | 67 | 49 | 62 | 57 | 45 |
From table 2 contrast as can be seen, processing 1, processing 3, processing 4 obviously are better than handling 5, illustrate that the effect that adds poly aspartic acid in the growth is better than what do not add.It should be noted that handling 2 only is to handle 2 seed to soak with poly aspartic acid with the difference of handling 5, other conditions are all with to handle 5 blank samples identical, but handle 2 advantage obviously as seen.Handle in addition 3 with handle to handle 4 and compare, illustrate that poly aspartic acid of the present invention is better than commercially available poly aspartic acid to the influence of plant-growth.
Embodiment 12: use the influence of the synergistic urea of poly-aspartic potassium preparation of the present invention to the field corn growth
The preparation of poly aspartic acid synergistic urea of the present invention: in the urea plant of certain fertilizer plant, before granulation, after the urea under poly-aspartic potassium and the molten state mixed, granulation again was the poly-aspartic potassium synergistic urea.The add-on of poly-aspartic potassium is 0.1% in the synergistic urea in the present embodiment.The urea that the common urea that blank in the present embodiment uses derives from same fertilizer plant carries out granulation.
Test is carried out in the Dongying corn field, and the experimental plot physical features is smooth, and soil fertility is even, and it is good that water waters condition.The corn seeding time is on June 8th, 2007, and on September 24th, 2007, results were planted the control measures unanimity.District's group arrangement is at random adopted in test, establishes three processing, and each handles triplicate.Fertilising is disposable applying of corn litmus mouth phase (July 6).The rate of fertilizer application of three processing is respectively handles 1: 30 kilograms/mu of synergistic ureas (poly-aspartic potassium that contains 1% present embodiment 1); Handle 2: 24 kilograms/mu of synergistic ureas (poly-aspartic potassium that contains 1% present embodiment 1); Handle 3: blank, promptly common urea is 30 kilograms/mu.
Test-results shows: use the experimental plot of synergistic urea to present obvious effects, show: the leaf look dark green, it is fast to grow, and blade is roomy, the plant height comparison is according to exceeding 10～20 centimeters, and heading was weaved silk early 2～3 days, and mealie is grown to the top, later stage is not taken off fertilizer, and is better ripe.The thousand seed weight of the corn of the corn of use synergistic urea and common urea contrasts and sees Table 3 after the harvesting, calculates as can be known if apply the urea (processing 1 and processing 3) of equivalent from table 3, and the synergistic urea corn thousand seed weight that then contains 1% poly aspartic acid increases by 10.36%; And, can obtain same effect when the synergistic urea of 1% poly aspartic acid during (handle 2 and handle 3) than blank Shaoshi 20%.
Table 4 is the output contrast of surveying statistics according to the experimental plot, and the result shows that handling 1 uses synergistic urea than 90 kilograms of use common urea check plot mu volume increase, amount of increase in production 18.95%, and through the check of F value, otherness is remarkable.It is suitable with check plot output to handle (2) poly-peptide organized enzyme urea amount of application minimizing 20%, and slightly volume increase, shows effect of increasing production preferably.Poly-peptide organized enzyme urea decrement 20% uses that to use output suitable with the capacity common urea, and input cost obviously reduces, thereby has improved input-output ratio, has increased economic benefit.
Therefore poly-aspartic potassium of the present invention has the effect of obvious promotion corn growth.
Table 3 corn is used poly-peptide organized enzyme urea and common urea thousand seed weight (g) contrast
| Handle 1 | Handle 2 | Handle 3 | |
| Repeat 1 | 298 | 272 | 259 |
| Repeat 2 | 312 | 290 | 289 |
| Repeat 3 | 318 | 298 | 292 |
| Mean number | 309 | 287 | 280 |
Table 4 corn is used poly-peptide organized enzyme urea and common urea output (Kg) contrast
| Handle 1 | Handle 2 | Handle 3 | |
| Repeat 1 | 581 | 493 | 458 |
| Repeat 2 | 550 | 503 | 466 |
| Repeat 3 | 564 | 480 | 500 |
| Mean number | 565 | 492 | 475 |
Claims (4)
1. preparation method who is used for the poly-aspartic potassium of plant growth promoter is characterized in that concrete steps are as follows:
With catalyzer boric acid, catalyst sulfuric acid potassium or sal enixum and raw material aspartic acid thorough mixing, make mixture in kneader or reactor, carry out heat polymerization then, obtain polysuccinimide, cooling, catalyzer need not separate, and is poly-aspartic potassium with hydrolysis of polysuccinimide under the effect of potassium hydroxide directly; Wherein, the adding total amount of catalyzer boric acid and catalyst sulfuric acid potassium or sal enixum and the mol ratio of aspartic acid are 0.05: 1～1: 1, and the mol ratio of catalyzer boric acid and catalyst sulfuric acid potassium or sal enixum is 0.1: 1～1: 1.
2. the preparation method who is used for the poly-aspartic potassium of plant growth promoter according to claim 1, it is characterized in that described blending means is in the aqueous solution catalyzer boric acid, catalyst sulfuric acid potassium or sal enixum and aspartic acid to be dissolved, and carries out mixing solutions drying then; Perhaps catalyzer boric acid, catalyst sulfuric acid potassium or sal enixum and aspartic acid are directly mixed, fully grind.
3. the application of poly-aspartic potassium in chemical fertilizer of obtaining of preparation method according to claim 1.
4. the application of poly-aspartic potassium according to claim 3 in chemical fertilizer, it is characterized in that described being applied as directly is added on poly-aspartic potassium in the chemical fertilizer, adding part by weight is 0.1～10%, and the add-on of poly-aspartic potassium is 0.1g-10g in promptly every 100g chemical fertilizer.
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| CN103059299B (en) * | 2013-01-22 | 2014-01-15 | 石家庄开发区德赛化工有限公司 | Compound type MSOD (Models of Superoxide Dismutase) and production process thereof |
| CN104446875B (en) * | 2014-10-22 | 2017-02-01 | 成都新柯力化工科技有限公司 | Macromolecular potash fertilizer and preparation method |
| CN106220846B (en) * | 2016-07-26 | 2018-05-04 | 史丹利化肥丰城有限公司 | A kind of poly-aspartate for fertilizer synergist and its preparation method and application |
| CN107879824A (en) * | 2017-12-25 | 2018-04-06 | 中国科学院化学研究所 | A kind of multi-Functional Fertilizers synergistic compound and preparation method thereof |
| CN112649518B (en) * | 2020-09-23 | 2022-09-30 | 贵州省产品质量检验检测院 | Method for determining content of potassium polyaspartate in wine by high performance liquid chromatography-fluorescence detection method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6300105B1 (en) * | 1998-07-23 | 2001-10-09 | Nippon Shokubai Co., Ltd. | Methods for producing a succinimide polymer, an aspartic acid polymer and L-aspartic acid |
| CN1498911A (en) * | 2002-11-05 | 2004-05-26 | 中国石化上海石油化工股份有限公司 | Method for preparing poly aspartic acid |
| CN1760311A (en) * | 2005-10-27 | 2006-04-19 | 常茂生物化学工程股份有限公司 | Method of application of poly asparagic acid in lowering viscidity in oil field |
| CN101215205A (en) * | 2007-12-29 | 2008-07-09 | 石家庄开发区德赛化工有限公司 | Synergistic foliage fertilizer and application method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6300105B1 (en) * | 1998-07-23 | 2001-10-09 | Nippon Shokubai Co., Ltd. | Methods for producing a succinimide polymer, an aspartic acid polymer and L-aspartic acid |
| CN1498911A (en) * | 2002-11-05 | 2004-05-26 | 中国石化上海石油化工股份有限公司 | Method for preparing poly aspartic acid |
| CN1760311A (en) * | 2005-10-27 | 2006-04-19 | 常茂生物化学工程股份有限公司 | Method of application of poly asparagic acid in lowering viscidity in oil field |
| CN101215205A (en) * | 2007-12-29 | 2008-07-09 | 石家庄开发区德赛化工有限公司 | Synergistic foliage fertilizer and application method thereof |
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