CN114805808A - Preparation method of polyaspartic acid potassium and application of polyaspartic acid potassium in plant growth promoter - Google Patents
Preparation method of polyaspartic acid potassium and application of polyaspartic acid potassium in plant growth promoter Download PDFInfo
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- CN114805808A CN114805808A CN202210610098.7A CN202210610098A CN114805808A CN 114805808 A CN114805808 A CN 114805808A CN 202210610098 A CN202210610098 A CN 202210610098A CN 114805808 A CN114805808 A CN 114805808A
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- 108010064470 polyaspartate Proteins 0.000 title claims abstract description 73
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 70
- 239000011591 potassium Substances 0.000 title claims abstract description 70
- 229920000805 Polyaspartic acid Polymers 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 230000008635 plant growth Effects 0.000 title claims abstract description 19
- 239000007952 growth promoter Substances 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 101
- 238000003756 stirring Methods 0.000 claims abstract description 84
- 239000000463 material Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 47
- 238000012546 transfer Methods 0.000 claims description 44
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 42
- 238000001035 drying Methods 0.000 claims description 40
- 239000007787 solid Substances 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 150000003863 ammonium salts Chemical class 0.000 claims description 26
- 238000005086 pumping Methods 0.000 claims description 25
- 230000007246 mechanism Effects 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000002347 injection Methods 0.000 claims description 17
- 239000007924 injection Substances 0.000 claims description 17
- 238000001556 precipitation Methods 0.000 claims description 17
- 238000007599 discharging Methods 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000006116 polymerization reaction Methods 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000002808 molecular sieve Substances 0.000 claims description 11
- 238000007790 scraping Methods 0.000 claims description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 9
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 9
- CKKXWJDFFQPBQL-UAIGNFCESA-N diazanium;(z)-but-2-enedioate Chemical compound [NH4+].[NH4+].[O-]C(=O)\C=C/C([O-])=O CKKXWJDFFQPBQL-UAIGNFCESA-N 0.000 claims description 9
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 9
- 239000011976 maleic acid Substances 0.000 claims description 9
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims description 8
- 239000013067 intermediate product Substances 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000007792 addition Methods 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000002689 soil Substances 0.000 claims description 3
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 5
- 125000004122 cyclic group Chemical group 0.000 abstract description 4
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000012295 chemical reaction liquid Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 11
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 10
- 239000003337 fertilizer Substances 0.000 description 9
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 8
- 229960005261 aspartic acid Drugs 0.000 description 8
- CKLJMWTZIZZHCS-UHFFFAOYSA-N D-OH-Asp Natural products OC(=O)C(N)CC(O)=O CKLJMWTZIZZHCS-UHFFFAOYSA-N 0.000 description 7
- CKLJMWTZIZZHCS-UWTATZPHSA-N L-Aspartic acid Natural products OC(=O)[C@H](N)CC(O)=O CKLJMWTZIZZHCS-UWTATZPHSA-N 0.000 description 7
- 230000012010 growth Effects 0.000 description 6
- 238000012643 polycondensation polymerization Methods 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
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- 238000010586 diagram Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
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- 239000002904 solvent Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
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- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
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- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
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- 239000011701 zinc Substances 0.000 description 1
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-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1092—Polysuccinimides
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyamides (AREA)
Abstract
The invention provides a preparation method of polyaspartic acid potassium and application of the polyaspartic acid potassium in a plant growth promoter, belongs to the technical field of plant growth promoters, and solves the problems of low preparation efficiency, high cost, poor purity, poor plant growth promoting effect and the like of the existing polyaspartic acid potassium. The preparation method of the potassium polyaspartate can realize the process cooperation of a plurality of steps on the quantity function of a plurality of devices, form flow line production, cannot stay on a certain process, and can work together after all parts are opened through time difference without frequently starting and stopping for waiting. The invention can realize the reaction temperature control of the stirring tank and the stirring barrel, and ensure the temperature stability; the collection and cyclic utilization of materials which do not react in the middle are realized, the energy is saved, the emission is reduced, and the cost is reduced; the purification of polysuccinimide can be repeatedly carried out, so that the purity of the potassium polyaspartate solution is high.
Description
Technical Field
The invention belongs to the technical field of plant growth promoters, relates to a preparation method of polyaspartic acid potassium, and particularly relates to an application of polyaspartic acid potassium in a plant growth promoter.
Background
The molecular formula of the polyaspartic acid potassium is [ [ C4H4O3N ] n ] -, the polyaspartic acid potassium is mainly applied to the field of green agriculture development in agriculture, and has the advantages of long-chain protein property, anionic surfactant and the like.
The fertilizer can promote the absorption of nutrient elements by crops, promote the growth of root systems, increase the yield, strengthen plants, enhance the stress resistance, achieve deep and luxuriant roots and leaves, improve the quality, improve the utilization rate of the fertilizer by 30 to 50 percent by applying the polyaspartic acid potassium, and reduce the fertilizer dosage by more than 20 percent. The polyaspartic acid potassium has the characteristics of no toxicity, no residue and the like. The first year of the United states was obtained in 96 as the "green chemical war of President".
The plant nutrient absorption enhancer is a novel crop nutrient absorption enhancer developed and researched by adopting a bionic synthesis technology (different from general crop hormones, has the characteristics of small dosage and high efficiency, can save one third of the dosage of a chemical fertilizer per mu, can enhance the drug effect and improve the disease-resistant and stress-resistant capabilities of crops), has comprehensive nutrition for the crops, stimulates the activity of biological enzymes, strengthens the absorption effect of nitrogen, phosphorus, potassium and trace elements, and is particularly obvious for three elements of zinc, manganese and iron of the crops, so the potassium polyaspartate is an attractive new-generation fertilizer synergistic granule.
The research on the synthesis process of polyaspartic acid mainly comprises 4 routes in summary: solid-phase thermal condensation polymerization of L-aspartic acid, liquid-phase thermal condensation polymerization of L-aspartic acid, chemical reaction of maleic anhydride and derivatives thereof and nitrogen-containing compounds, thermal condensation polymerization, and liquid-phase direct polymerization of maleic anhydride and derivatives thereof and nitrogen-containing compounds.
However, the 4 routes all have certain defects, the L-aspartic acid is used as a raw material, the cost is higher, the limitation is larger, the solid-phase reaction is heated unevenly, the mass and heat transfer effects are poor, the reaction is insufficient, the purity is low, the time of the latter two processes is longer (frequent start and stop is needed, the waiting period is long), and the molecular weight of the obtained polymerization product is not high; meanwhile, the intermediate solvent cannot be recycled, and the purity is low.
Based on the above, the preparation method of the polyaspartic acid potassium and the application of the polyaspartic acid potassium in the plant growth promoter are provided; the preparation method of the potassium polyaspartate can form flow line production by the process cooperation of a plurality of steps on the quantity function of a plurality of devices, does not stop on a certain process, works together after all parts are started with time difference, does not need frequent start-stop waiting, and has high automation degree, higher efficiency and low energy consumption;
the reaction temperature of the stirring tank and the stirring barrel is controlled by matching the drying mechanism, the fan, the stirring tank heat-preserving cylinder and the stirring barrel heat-preserving cylinder, and the temperature is ensured to be stable;
through the matching of the collecting box, the air pump and the molecular sieve, the collection and cyclic utilization of materials which do not react in the middle, such as absolute ethyl alcohol, N-dimethyl formamide and the like, are realized, the energy is saved, the emission is reduced, and the cost is reduced;
through the matching of the stirring tank, the precipitation tank and the vacuum dryer, the purification of the polysuccinimide can be repeatedly carried out, the polysuccinimide with high purity is obtained, and the purity of the polyaspartic acid potassium solution is high.
The application of the potassium polyaspartate in the plant growth promoter has good fertilizing effect and can promote effective growth, the fertilizing amount is 10g of the potassium polyaspartate solution in per 100g of clear water, the effect is optimal, and meanwhile, the preparation method has lower cost and higher efficiency and can be industrially produced in the application of the plant growth promoter.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method of polyaspartic acid potassium and application of polyaspartic acid potassium in a plant growth promoter, and the invention aims to solve the technical problems that: how to realize the process coordination of a plurality of steps on the quantity function of a plurality of devices to form the flow line production, the stop on a certain process is avoided, all parts work together after being started by time difference, frequent start-stop waiting is not needed, the automation degree is high, the efficiency is higher, and the energy consumption is low; the application of the potassium polyaspartate in the plant growth promoter is realized, the fertilizer application effect is good, and the effective growth can be promoted.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of polyaspartic acid potassium comprises the following steps:
step one, injecting a certain amount of maleic anhydride and a certain amount of water into a reaction kettle, heating the reaction kettle to raise the temperature, and performing hydrolysis reaction at the temperature of 60 +/-2 ℃ for 30 +/-5 min to obtain a maleic acid solution, wherein the chemical equation of hydrolysis is C 4 H 2 O 3 +H 2 O＝C 4 H 4 O 4 ；
Injecting a certain amount of liquid ammonia into a reaction kettle (the amount of the liquid ammonia is 1.2 +/-0.1 times of that of the maleic anhydride), heating the reaction kettle, carrying out mixing reaction at the temperature of 80 +/-5 ℃ for 2 +/-0.1 h to obtain a maleic acid ammonium salt solution mixture;
step three, stopping heating the reaction kettle, introducing cooling water, and opening the reaction kettle to discharge the reaction solution when the temperature is reduced to 50 +/-1 ℃;
step four, guiding the reaction solution into a drying mechanism with the temperature of 80 +/-5 ℃ for drying to obtain white solid ammonium salt;
putting the solid ammonium salt into a high-temperature reaction furnace, introducing nitrogen, heating the high-temperature reaction furnace, and carrying out thermal shrinkage polymerization reaction at the temperature of 210 +/-5 ℃ for 4 +/-0.1 h to obtain an intermediate product polysuccinimide;
step six, introducing polysuccinimide into a stirring tank filled with N, N-dimethyl formamide which is 10 +/-0.1 times of the mass of the polysuccinimide, purifying and dissolving the polysuccinimide, namely dissolving the polysuccinimide into the N, N-dimethyl formamide, insolubilizing maleic anhydride and ammonium maleate, and continuously stirring for 4 +/-0.1 h in a water bath at the temperature of 40 +/-1 ℃ to obtain a mixed solution;
step seven, injecting the mixed solution into a precipitation tank, simultaneously injecting absolute ethyl alcohol, mixing, precipitating, filtering, and washing with absolute ethyl alcohol to obtain a washing filtrate;
step eight, injecting the washing filtrate obtained in the step seven into a vacuum drier for vacuum drying to obtain polysuccinimide with higher purity, and repeating the step six to the step eight for 1 to 3 times to obtain polysuccinimide with high purity;
and step nine, taking out the polysuccinimide solid, adding the polysuccinimide solid into a stirring barrel filled with deionized water, stirring to form a suspension, injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0 +/-0.5, and hydrolyzing at the temperature of 40 +/-2 ℃ for 30 +/-5 min to obtain the potassium polyaspartate solution.
A preparation method of polyaspartic acid potassium comprises a plurality of reaction kettles, a drying mechanism, a lifter, a plurality of high-temperature reaction furnaces, a plurality of stirring tanks, a collecting box, a settling tank, a vacuum drier and a stirring barrel which are arranged in sequence, the drying mechanism is provided with a plurality of first material pumping pumps, the number and the position of the first material pumping pumps correspond to those of the reaction kettle, the feed end of the first material pumping pump is connected with the reaction kettle corresponding to the position, the discharge end of the elevator is provided with a flexible discharge pipe, an electric sliding seat is arranged above the feed end of a plurality of high-temperature reaction furnaces, the discharge end of the flexible discharge pipe is connected onto the electric sliding seat, a second material pumping pump is connected between the high-temperature reaction furnaces and the corresponding stirring tank, a third material pumping pump is arranged between the settling tank and the vacuum dryer, an air suction pump is arranged between the collecting tank and the vacuum dryer, the rear side of the settling tank is provided with a transfer box, and the transfer box is connected with the stirring tank and the settling tank through pipelines respectively.
By adopting the structure, a certain amount of maleic anhydride and a certain amount of water are injected into the reaction kettle, the reaction kettle is heated to increase the temperature to obtain a maleic acid solution, one reaction kettle is started every 0.5h, and the six reaction kettles are matched with the drying mechanism to form assembly line operation; injecting a certain amount of liquid ammonia into the reaction kettle, heating the reaction kettle to raise the temperature, and carrying out mixing reaction for 2 +/-0.1 h to obtain a maleic acid ammonium salt solution mixture; stopping heating the reaction kettle, introducing cooling water, cooling, and opening the reaction kettle to release reaction liquid when the reaction kettle is hot; introducing reaction liquid of the corresponding reaction kettle into a drying mechanism for drying every 0.5h by a first material pumping pump in sequence to obtain white solid ammonium salt; lifting solid ammonium salt by a lifter, sequentially introducing the solid ammonium salt into eight high-temperature reaction furnaces through the matching of a flexible discharge pipe and an electric sliding seat, introducing nitrogen, heating the high-temperature reaction furnaces, and carrying out thermal shrinkage polymerization reaction to obtain an intermediate product polysuccinimide; introducing polysuccinimide into a stirring tank filled with N, N-dimethyl formamide through a second material pumping pump, purifying and dissolving the polysuccinimide, namely dissolving the polysuccinimide into the N, N-dimethyl formamide, and insolubilizing maleic anhydride and ammonium salt of maleic acid to obtain a mixed solution, injecting the mixed solution into a settling tank through a transfer box, simultaneously injecting absolute ethyl alcohol, performing mixed settling, filtering, and washing with the absolute ethyl alcohol to obtain a washing filtrate; injecting the washing filtrate into a vacuum drier by a third material pumping pump for vacuum drying to obtain polysuccinimide with higher purity, sequentially injecting the polysuccinimide into the stirring tank, and repeating the steps for one time to obtain the polysuccinimide with high purity; adding the polysuccinimide solid into a stirring barrel filled with deionized water, stirring to form a suspension, injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0 +/-0.5, and hydrolyzing at the temperature of 40 +/-2 ℃ for 30 +/-5 min to obtain the potassium polyaspartate solution.
The stoving mechanism includes the stoving case, and stoving incasement portion is equipped with the conveyer, and the stoving case is stretched out at the both ends of conveyer, and the discharge end of first suction pump is located the top of the feed end of conveyer, and the discharge end of conveyer is equipped with scrapes the flitch, and the upper end of scraping the flitch is contradicted on the track of conveyer, scrapes the lower extreme of flitch and is located the feeder hopper top of lifting machine, and stoving case top is equipped with the drainage case, and the drainage case top is equipped with the fan.
Structure more than adopting, every 0.5h through first pump, the top of the leading-in conveyer's of the reaction liquid that will correspond reation kettle feed end is in proper order, and the stoving case is dried the reaction liquid, obtains white solid ammonium salt, scrapes white solid ammonium salt from the track of conveyer down with the scraping plate, falls into inside the feeder hopper of lifting machine, and the lifting machine promotes white solid ammonium salt inside the high temperature reaction stove in proper order, and the inside steam suction of stoving mechanism is gone up to the fan, obtains dry steam through the straining box filtration.
The external portion of agitator tank is equipped with agitator tank heat-preserving container, is connected with the second steam pipe between the air-out end of agitator tank heat-preserving container and fan, and the external portion of agitator tank is equipped with agitator heat-preserving container, is connected with first steam pipe between agitator heat-preserving container and the agitator tank heat-preserving container, is connected with the back flow between vacuum drying machine and the air pump of bleeding.
Structure more than adopting, inside the fan blew in dry steam through the second steam pipe in the agitator tank heat-preserving container, kept the constancy of temperature of agitator tank, inside the rethread first steam pipe got into the agitator heat-preserving container, kept the constancy of temperature of agitator, steam molecular sieve such as ethanol that the air pump produced when drying vacuum drying machine sieves and forms anhydrous alcohol and N, N two dimethyl formamide, through the back flow suction, collects the collection incasement, carries out the condensation.
Be equipped with the control valve pipe that leads to between transfer case and the agitator tank, the valve body that leads to the control valve pipe that leads to is connected with the agitator tank that corresponds, is connected through the inlet pipe between transfer case and the control valve pipe that leads to, is equipped with between transfer case and the settling tank and annotates the material pipe, and transfer incasement portion is equipped with feeding transfer pump and ejection of compact transfer pump, and the inlet pipe is connected with feeding transfer pump, annotates the material pipe and is connected with ejection of compact transfer pump.
Structure more than adopting, transit case and the cooperation of leading to the control valve pipe that leads to, the feeding transfer pump will with the inside mixed solution of agitator tank that the valve body of leading to the control valve pipe corresponds, through inlet pipe suction transit incasement portion, then will mixed solution through the ejection of compact transfer pump pour into the settling tank inside through annotating the material pipe, carry out the settling out.
The collecting box comprises collection liquid case and play liquid tank, and the collection liquid case is located a liquid tank top, and the air pump that bleeds is located collection liquid case top, and the collection liquid case is connected with the play liquid end of air pump that bleeds, goes out the inside liquid pump that is equipped with of liquid tank, goes out the liquid end of liquid pump and annotates the liquid union coupling, annotates the liquid union coupling on the setting-out tank, and collection liquid incasement portion is equipped with the molecular sieve.
Structure more than adopting, the steam that produces when air exhaust pump is with vacuum drying machine stoving, the condensation of suction collecting liquid case, via inside molecular sieve again, the screening forms anhydrous alcohol and N, N two methyl formamide, and anhydrous alcohol stores in the liquid tank insidely, and the liquid pump is taken out the inside anhydrous alcohol liquid of liquid tank, pours into the settling tank into through annotating the liquid pipe inside, carries out settling out, washing, and N, N two methyl formamide can collect the back purification and recycle.
The inside of settling out jar is equipped with the settling out filter plate, and the end that annotates the material pipe and annotate the liquid pipe is located the settling out filter plate, and the setting of settling out filter plate slope is equipped with the bin gate on the lateral part of settling out jar, and the bin gate is located the terminal downside of settling out filter plate slope, and vacuum drying machine is equipped with a plurality of hoppers, and one of them hopper is connected with the agitator.
By adopting the structure, the high-purity polysuccinimide is injected into a precipitation tank through a liquid injection pipe to perform precipitation, precipitated solids are collected on a precipitation filter plate, can be discharged by opening a discharge door, a washing solution obtained by washing is a polysuccinimide solution, polysuccinimide with high purity is obtained by a vacuum drier, is discharged through a certain discharge hopper, is sequentially injected into a stirring tank after being collected, can be cyclically repeated for one time to obtain high-purity polysuccinimide, and the high-purity polysuccinimide is introduced into the stirring tank from one discharge hopper to be mixed and hydrolyzed to obtain the high-purity potassium polyaspartate solution.
The application of the polyaspartic acid potassium in the plant growth promoter is that the polyaspartic acid potassium solution is added with water and then sprayed on the soil where crops grow, the adding weight proportion is 0.1 to 10 percent, namely, the adding amount of the polyaspartic acid potassium solution in every 100g of clear water is 0.1 to 10g
Compared with the prior art, the preparation method of the polyaspartic acid potassium has the following advantages:
the invention can form flow line production by the cooperation of a plurality of steps of technologies on the quantity function of a plurality of devices, can not stay on a certain process, and all parts work together after being started by time difference without frequent start-stop waiting, and has high automation degree, higher efficiency and low energy consumption;
the reaction temperature control of the stirring tank and the stirring barrel is realized through the matching of the drying mechanism, the fan, the stirring tank heat-preserving cylinder and the stirring barrel heat-preserving cylinder, and the temperature stability is ensured;
through the matching of the collecting box, the air pump and the molecular sieve, the collection and cyclic utilization of materials which do not react in the middle, such as absolute ethyl alcohol, N-dimethyl formamide and the like, are realized, the energy is saved, the emission is reduced, and the cost is reduced;
through the matching of the stirring tank, the precipitation tank and the vacuum dryer, the polysuccinimide can be purified repeatedly to obtain high-purity polysuccinimide, so that the purity of the polyaspartic acid potassium solution is high.
The application of the potassium polyaspartate in the plant growth promoter has good fertilizing effect, the fertilizing amount is 10g of the potassium polyaspartate solution in per 100g of clear water, the effect is optimal, and meanwhile, the preparation method has lower cost and higher efficiency and can be industrially produced in the application of the plant growth promoter.
Drawings
FIG. 1 is a block diagram of the process flow of the present invention.
FIG. 2 is a process timing diagram of the present invention.
FIG. 3 is a block diagram of the number of process equipment of the present invention.
Fig. 4 is a partial structural schematic diagram of the present invention.
Fig. 5 is a perspective view of a part of the components of the present invention.
FIG. 6 is a table of experiments on average growth height of corn plants from 0 to 28 days in corn fields.
In the figure, 1, a reaction kettle; 2. a first pump; 3. a drying mechanism; 4. a fan; 5. a scraping plate; 6. a hoist; 7. a high-temperature reaction furnace; 8. a second pump; 9. a stirring tank; 10. a stirring tank heat-preserving cylinder; 11. an air pump; 12. a collection box; 13. a third material pumping pump; 14. a vacuum drier; 15. a stirring barrel; 16. a mixing drum heat-preserving cylinder; 17. a first hot air pipe; 18. a return pipe; 19. a settling tank; 20. a second hot air pipe; 21. a feed pipe; 22. a material injection pipe; 23. a discharge gate; 24. a transfer box; 25. a liquid injection pipe; 26. an electric sliding seat; 27. and (4) a flexible discharge pipe.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
As shown in the figures 1-3, the preparation method of the potassium polyaspartate comprises the following steps:
step one, injecting a certain amount of maleic anhydride and a certain amount of water into a reaction kettle, heating the reaction kettle to raise the temperature, and performing hydrolysis reaction at the temperature of 60 +/-2 ℃ for 30 +/-5 min to obtain a maleic acid solution, wherein the chemical equation of hydrolysis is C 4 H 2 O 3 +H 2 O＝C 4 H 4 O 4 ；
Injecting a certain amount of liquid ammonia into a reaction kettle (the amount of the liquid ammonia is 1.2 +/-0.1 times of that of maleic anhydride), heating the reaction kettle, carrying out mixing reaction at the temperature of 80 +/-5 ℃, and reacting for 2 +/-0.1 h to obtain a maleic acid ammonium salt solution mixture;
step three, stopping heating the reaction kettle, introducing cooling water, and opening the reaction kettle to discharge the reaction solution when the temperature is reduced to 50 +/-1 ℃;
step four, guiding the reaction solution into a drying mechanism with the temperature of 80 +/-5 ℃ for drying to obtain white solid ammonium salt;
putting the solid ammonium salt into a high-temperature reaction furnace, introducing nitrogen, heating the high-temperature reaction furnace, and carrying out thermal shrinkage polymerization reaction at the temperature of 210 +/-5 ℃ for 4 +/-0.1 h to obtain an intermediate product polysuccinimide;
step six, introducing polysuccinimide into a stirring tank filled with N, N-dimethyl formamide which is 10 +/-0.1 times of the mass of the polysuccinimide, purifying and dissolving the polysuccinimide, namely dissolving the polysuccinimide into the N, N-dimethyl formamide, insolubilizing maleic anhydride and ammonium maleate, and continuously stirring for 4 +/-0.1 h in a water bath at the temperature of 40 +/-1 ℃ to obtain a mixed solution;
step seven, injecting the mixed solution into a precipitation tank, simultaneously injecting absolute ethyl alcohol, mixing, precipitating, filtering, and washing with absolute ethyl alcohol to obtain a washing filtrate;
step eight, injecting the washing filtrate obtained in the step seven into a vacuum drier for vacuum drying to obtain polysuccinimide with higher purity, and repeating the step six to the step eight for 1 to 3 times to obtain polysuccinimide with high purity;
and step nine, taking out the polysuccinimide solid, adding the polysuccinimide solid into a stirring barrel filled with deionized water, stirring to form a suspension, injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0 +/-0.5, and hydrolyzing at the temperature of 40 +/-2 ℃ for 30 +/-5 min to obtain the potassium polyaspartate solution.
As shown in figures 4-5, the preparation method of the polyaspartic acid potassium comprises a plurality of reaction kettles 1, a drying mechanism 3, a lifter 6, a plurality of high-temperature reaction furnaces 7, a plurality of stirring tanks 9, a collecting tank 12, a settling tank 19, a vacuum dryer 14 and a stirring barrel 15 which are arranged in sequence, wherein the drying mechanism 3 is provided with a plurality of first pumping pumps 2, the number and the position of the first pumping pumps 2 correspond to the reaction kettles 1, the feeding end of the first pumping pump 2 is connected with the reaction kettles 1 at the corresponding positions, the discharging end of the lifter 6 is provided with a flexible discharging pipe 27, an electric sliding seat 26 is arranged above the feeding end of the high-temperature reaction furnaces 7, the discharging end of the flexible discharging pipe is connected on the electric sliding seat 26, a second pumping pump 8 is connected between the high-temperature reaction furnaces 7 and the corresponding stirring tank 9, a third pumping pump 13 is arranged between the settling tank 19 and the vacuum dryer 14, an air pump 11 is arranged between the collecting tank 12 and the vacuum dryer 14, a transfer tank 24 is arranged at the rear side of the settling tank 19, and the transfer tank 24 is respectively connected with the stirring tank 9 and the settling tank 19 through pipelines;
a certain amount of maleic anhydride and a certain amount of water are injected into the reaction kettle 1, the reaction kettle is heated to raise the temperature to obtain a maleic acid solution, one reaction kettle 1 is started after every 0.5 hour, and six reaction kettles 1 are matched with a drying mechanism to form assembly line operation; injecting a certain amount of liquid ammonia into the reaction kettle 1, heating the reaction kettle 1 to raise the temperature, and carrying out mixing reaction for 2 +/-0.1 h to obtain a maleic acid ammonium salt solution mixture; stopping heating the reaction kettle, introducing cooling water, cooling, opening the reaction kettle 1 and discharging the reaction liquid while the reaction kettle is hot; introducing reaction liquid corresponding to the reaction kettle 1 into a drying mechanism 3 for drying by a first material pumping pump 2 every 0.5h in sequence to obtain white solid ammonium salt; the hoister 6 lifts the solid ammonium salt, the solid ammonium salt is guided into the eight high-temperature reaction furnaces 7 in sequence through the matching of the flexible discharge pipe and the electric sliding seat 26, nitrogen is introduced, the high-temperature reaction furnaces 7 are heated, and thermal shrinkage polymerization reaction is carried out to obtain an intermediate product polysuccinimide; introducing polysuccinimide into a stirring tank 9 filled with N, N-dimethyl formamide through a second material pumping pump 8, purifying and dissolving the polysuccinimide, namely dissolving the polysuccinimide into the N, N-dimethyl formamide, and insolubilizing maleic anhydride and ammonium salt of maleic acid to obtain a mixed solution, injecting the mixed solution into a settling tank 19 through a transfer box 24, simultaneously injecting absolute ethyl alcohol, carrying out mixed settling, filtering, and washing with the absolute ethyl alcohol to obtain a washing filtrate; injecting the washing filtrate into a vacuum drier by a third material pumping pump 13 for vacuum drying to obtain polysuccinimide with higher purity, sequentially injecting the polysuccinimide into the stirring tank 9, and repeating for 1-3 times to obtain the polysuccinimide with high purity; adding the polysuccinimide solid into a stirring barrel 15 filled with deionized water, stirring to form a suspension, injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0 +/-0.5, and hydrolyzing at the temperature of 40 +/-2 ℃ for 30 +/-5 min to obtain the potassium polyaspartate solution.
The drying mechanism 3 comprises a drying box, a conveyor is arranged in the drying box, two ends of the conveyor extend out of the drying box, the discharge end of the first material pumping pump 2 is positioned above the feed end of the conveyor, a scraping plate 5 is arranged at the discharge end of the conveyor, the discharge end of the conveyor is provided with the scraping plate 5, the upper end of the scraping plate 5 is abutted against a track of the conveyor, the lower end of the scraping plate 5 is positioned above a feed hopper of a lifting machine 6, a water filtering box is arranged above the drying box, and a fan 4 is arranged above the water filtering box; every 0.5h through first material pump 2 will correspond reation kettle 1's the leading-in conveyer's of reaction liquid top in proper order, the stoving case is dried the reaction liquid, obtain white solid ammonium salt, scraping flitch 5 scrapes white solid ammonium salt from the track of conveyer, fall into inside the feeder hopper of lifting machine 6, lifting machine 6 promotes white solid ammonium salt to inside high temperature reaction stove 7 in proper order, fan 4 is with the inside steam suction of stoving mechanism 3, obtain dry steam through the straining box filtration.
A stirring tank heat-preserving cylinder 10 is arranged outside the stirring tank 9, a second hot air pipe 20 is connected between the stirring tank heat-preserving cylinder 10 and the air outlet end of the fan 4, a stirring barrel heat-preserving cylinder 16 is arranged outside the stirring barrel 15, a first hot air pipe 17 is connected between the stirring barrel heat-preserving cylinder 16 and the stirring tank heat-preserving cylinder 10, and a return pipe 18 is connected between the vacuum drier 14 and the air exhaust pump 11; inside fan 4 insufflates agitator tank heat-preserving container 10 with dry steam through second hot-air pipe 20, keep the constancy of temperature of agitator tank 9, inside rethread first hot-air pipe 17 got into agitator heat-preserving container 16, keep the constancy of temperature of agitator 15, steam molecular sieve such as the ethanol that produces when air pump 11 will vacuum drying machine 14 dry sieves and forms anhydrous alcohol and N, N two methyl formamide, through the suction of back flow 18, collect inside collection box 12, condense.
A multi-way control valve pipe is arranged between the transfer box 24 and the stirring tank 9, a valve body of the multi-way control valve pipe is connected with the corresponding stirring tank 9, the transfer box 24 is connected with the multi-way control valve pipe through a feeding pipe 21, a material injection pipe 22 is arranged between the transfer box 24 and the settling tank 19, a feeding transfer pump and a discharging transfer pump are arranged inside the transfer box 24, the feeding pipe 21 is connected with the feeding transfer pump, and the material injection pipe 22 is connected with the discharging transfer pump; transfer case 24 and the cooperation of multi-ported control valve pipe, the feeding transfer pump will with the inside mixed solution of agitator tank 9 that the valve body of multi-ported control valve pipe corresponds, through inlet pipe 21 suction transfer case 24 inside, then inside pouring into the settling tank 19 with mixed solution via notes material pipe 22 through ejection of compact transfer pump, carry out the settling.
The collecting box 12 consists of a collecting box and a liquid outlet box, the collecting box is positioned above the liquid outlet box, the air exhaust pump 11 is positioned above the collecting box, the collecting box is connected with the liquid outlet end of the air exhaust pump 11, the liquid outlet box is internally provided with a liquid outlet pump, the liquid outlet end of the liquid outlet pump is connected with a liquid injection pipe 25, the liquid injection pipe 25 is connected to the precipitation tank 19, and the collecting box is internally provided with a molecular sieve; steam that produces when air pump 11 dries vacuum drying machine 14, the condensation of suction collection liquid case, again via inside molecular sieve, the screening forms anhydrous alcohol and N, N two-methyl formamide, anhydrous alcohol stores inside the liquid outlet box, and the liquid outlet pump is taken out the inside anhydrous alcohol liquid of liquid outlet box, through annotating inside liquid pipe 25 injection settling tank 19, carry out the settling, wash, N, N two-methyl formamide can collect the back purification and recycle.
A settling filter plate is arranged in the settling tank 19, the tail ends of the material injection pipe 22 and the liquid injection pipe 25 are positioned on the settling filter plate, the settling filter plate is arranged in an inclined mode, a discharge door 23 is arranged on the side portion of the settling tank 19, the discharge door 23 is positioned on the lower side of the inclined tail end of the settling filter plate, the vacuum dryer 14 is provided with a plurality of discharge hoppers, and one of the discharge hoppers is connected with the stirring barrel 15; the high-purity polysuccinimide is injected into the settling tank 19 through the liquid injection pipe 25 for settling, settled solids are collected on a settling filter plate, can be discharged by opening the discharge door 23, the washing solution obtained by washing is polysuccinimide solution, the polysuccinimide with high purity is obtained by the vacuum drier 14, is discharged through a certain discharge hopper, is sequentially injected into the stirring tank 9 after being collected, can be circularly repeated for 1-3 times to obtain high-purity polysuccinimide, and the high-purity polysuccinimide is introduced into the stirring barrel 15 from one discharge hopper for mixing and hydrolysis to obtain high-purity potassium polyaspartate solution.
Example 1
A certain amount of maleic anhydride and a certain amount of water are injected into the reaction kettle 1, the reaction kettle is heated to raise the temperature to obtain a maleic acid solution, one reaction kettle 1 is started after every 0.5 hour, and six reaction kettles 1 are matched with a drying mechanism to form assembly line operation; injecting a certain amount of liquid ammonia into the reaction kettle 1, heating the reaction kettle 1 to raise the temperature, and carrying out mixing reaction for 2 +/-0.1 h to obtain a maleic acid ammonium salt solution mixture; stopping heating the reaction kettle, introducing cooling water, cooling, opening the reaction kettle 1 and discharging the reaction liquid while the reaction kettle is hot;
the reaction liquid corresponding to the reaction kettle 1 is sequentially led into the upper part of the feed end of the conveyor every 0.5h through the first material pumping pump 2, the drying box dries the reaction liquid to obtain white solid ammonium salt, and the white solid ammonium salt is scraped off from the track of the conveyor by the scraper plate 5 and falls into the feed hopper of the elevator 6;
the hoister 6 lifts the solid ammonium salt, the solid ammonium salt is guided into the eight high-temperature reaction furnaces 7 in sequence through the matching of the flexible discharge pipe and the electric sliding seat 26, nitrogen is introduced, the high-temperature reaction furnaces 7 are heated, and thermal shrinkage polymerization reaction is carried out to obtain an intermediate product polysuccinimide;
introducing the polysuccinimide into a stirring tank 9 filled with N, N-dimethyl formamide through a second material pumping pump 8, and purifying and dissolving the polysuccinimide, namely dissolving the polysuccinimide into the N, N-dimethyl formamide, and insolubilizing maleic anhydride and ammonium salt of maleic anhydride to obtain a mixed solution;
the feeding transfer pump sucks the mixed solution in the stirring tank 9 corresponding to the valve body of the multi-way control valve pipe into the transfer box 24 through the feeding pipe 21, then the mixed solution is injected into the interior of the settling tank 19 through the discharging transfer pump via the material injection pipe 22, meanwhile, the liquid outlet pump pumps the absolute ethyl alcohol liquid in the interior of the liquid outlet box, the absolute ethyl alcohol liquid is injected into the interior of the settling tank 19 through the material injection pipe 25 for settling and washing, settled solids are collected on a settling filter plate, and the settled solids can be discharged by opening the discharge door 23 to obtain a polysuccinimide solution as a washing solution;
injecting the washing filtrate into a vacuum drier by a third material pumping pump 13 for vacuum drying to obtain polysuccinimide with higher purity, sequentially injecting the polysuccinimide into the stirring tank 9, and repeating for 1-3 times to obtain the polysuccinimide with high purity;
adding the high-purity polysuccinimide solid into a stirring barrel 15 filled with deionized water, stirring to form a suspension, injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0 +/-0.5, and hydrolyzing at the temperature of 40 +/-2 ℃ for 30 +/-5 min to obtain a high-purity potassium polyaspartate solution;
the fan 4 sucks out hot air in the drying mechanism 3, the hot air is filtered by the water filtering box to obtain dry hot air, the fan 4 blows the dry hot air into the stirring tank heat-preserving cylinder 10 through the second hot air pipe 20 to keep the temperature of the stirring tank 9 constant, and then the dry hot air enters the stirring barrel heat-preserving cylinder 16 through the first hot air pipe 17 to keep the temperature of the stirring barrel 15 constant;
steam that produces when air exhaust pump 11 dries vacuum drying machine 14, the condensation of suction collection liquid case, via inside molecular sieve again, the screening forms anhydrous alcohol and N, N two methyl formamide, and anhydrous alcohol stores inside the liquid outlet box, and the liquid outlet pump is taken out the inside anhydrous alcohol liquid of liquid outlet box, pours into the settling tank 19 through annotating liquid pipe 25 inside, carries out settling out, washing, and N, N two methyl formamide can collect the back purification and recycle.
In conclusion, the invention can form flow line production by the process cooperation of a plurality of steps on the quantity function of a plurality of devices, can not stop on a certain process, can work together after all parts are started through time difference, does not need to be started and stopped frequently, and has high automation degree, higher efficiency and low energy consumption;
the drying mechanism 3, the fan 4, the stirring tank heat-preserving cylinder 10 and the stirring barrel heat-preserving cylinder 16 are matched, so that the reaction temperature of the stirring tank 9 and the stirring barrel 15 is controlled, and the temperature is ensured to be stable;
through the matching of the collection box 12, the air extraction air pump 11 and the molecular sieve, the collection and cyclic utilization of materials which do not react in the middle, such as absolute ethyl alcohol, N-dimethyl formamide and the like, are realized, the energy is saved, the emission is reduced, and the cost is reduced;
through the matching of the stirring tank 9, the precipitation tank 19 and the vacuum dryer 14, the polysuccinimide can be purified repeatedly to obtain high-purity polysuccinimide, so that the purity of the polyaspartic acid potassium solution is high.
In the embodiment, the polyaspartic acid potassium solution can be dried to obtain brown yellow polyaspartic acid potassium salt, and the drying mode is that a conveyor is additionally arranged inside the drying box, and the polyaspartic acid potassium solution is injected into the drying box for drying.
Example 2
Solid-phase thermal condensation polymerization of L-aspartic acid: synthesizing an intermediate product polysuccinimide by using L-aspartic acid as a raw material, and hydrolyzing with KOH to obtain polyaspartic acid potassium;
example 3
Liquid phase thermal condensation polymerization of aspartic acid: raising the temperature of L-aspartic acid in a solvent to the temperature required by the reaction for polymerization reaction, and then separating, purifying and hydrolyzing to obtain a product of potassium polyaspartate;
the disadvantages of examples 2 and 3 are that L-aspartic acid is used as raw material, the cost is high, the limitation is large, the solid phase reaction is heated unevenly, the mass and heat transfer effects are poor, and the reaction is insufficient and the purity is low.
Example 4
The indirect polymerization of maleic anhydride and derivatives thereof and nitrogen-containing compounds is to take maleic anhydride and derivatives thereof and nitrogen-containing compounds as raw materials, stir and react for a certain time in aqueous solution, then dry in an oven to obtain ammonium salt mixture of maleic acid, continue to raise the temperature to the polymerization temperature, along with the temperature rise, water evaporates rapidly, reactants become viscous liquid, the color deepens gradually, then polymerization reaction occurs in a molten state, the reactants become solid gradually at the later stage of the polymerization reaction, the fluidity is poor, and then the polyaspartic acid solution is obtained by hydrolysis;
example 4 is a simple way of example 1, i.e. there is no quantitative cooperation between the components, the whole process flow is long (frequent start and stop is required, the waiting period is long), and the molecular weight of the obtained polymer product is not high; meanwhile, the intermediate solvent cannot be recycled, and the purity is low.
The application of the polyaspartic acid potassium prepared by the preparation method of the polyaspartic acid potassium in the plant growth accelerant is that the polyaspartic acid potassium solution is sprayed on soil where crops grow after water is added, the adding weight proportion is 0.1-10%, namely the adding amount of the polyaspartic acid potassium solution in every 100g of clear water is 0.1-10 g.
Meanwhile, a certain amount of the potassium polyaspartate prepared in the example 2-4 is taken for application in the plant growth promoter,
in the same corn field, A, B, C, D, E, F, G, H and I were divided on the average of plants, 9 experimental zones, zone A as a blank, zone B, C, D as fertilizer with potassium polyaspartate prepared according to the method of example 1, zone E, F, G as fertilizer with potassium polyaspartate prepared according to examples 2-4, and zone H, I as fertilizer with commercially available potassium polyaspartate. The test plants naturally grow for an average growth height (cm) of 0-28 days.
The experimental table is as follows (table 1):
TABLE 1
Therefore, the potassium polyaspartate prepared by the preparation method has good fertilizing effect and can promote effective growth, the fertilizing amount is 10g of the potassium polyaspartate solution in per 100g of clear water, the effect is optimal, and meanwhile, the preparation method is lower in cost and higher in efficiency and can be applied to industrial production in plant growth promoters.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (8)
1. A preparation method of polyaspartic acid potassium comprises the following steps:
step one, injecting a certain amount of maleic anhydride and a certain amount of water into a reaction kettle, heating the reaction kettle to raise the temperature, and performing hydrolysis reaction at the temperature of 60 +/-2 ℃ for 30 +/-5 min to obtain a maleic acid solution, wherein the chemical equation of hydrolysis is C 4 H 2 O 3 +H 2 O＝C 4 H 4 O 4 ；
Injecting a certain amount of liquid ammonia into a reaction kettle (the amount of the liquid ammonia is 1.2 +/-0.1 times of that of the maleic anhydride), heating the reaction kettle, carrying out mixing reaction at the temperature of 80 +/-5 ℃ for 2 +/-0.1 h to obtain a maleic acid ammonium salt solution mixture;
step three, stopping heating the reaction kettle, introducing cooling water, and opening the reaction kettle to discharge the reaction solution when the temperature is reduced to 50 +/-1 ℃;
step four, guiding the reaction solution into a drying mechanism with the temperature of 80 +/-5 ℃ for drying to obtain white solid ammonium salt;
putting the solid ammonium salt into a high-temperature reaction furnace, introducing nitrogen, heating the high-temperature reaction furnace, and carrying out thermal shrinkage polymerization reaction at the temperature of 210 +/-5 ℃ for 4 +/-0.1 h to obtain an intermediate product polysuccinimide;
step six, introducing polysuccinimide into a stirring tank filled with N, N-dimethyl formamide which is 10 +/-0.1 times of the mass of the polysuccinimide, purifying and dissolving the polysuccinimide, namely dissolving the polysuccinimide into the N, N-dimethyl formamide, insolubilizing maleic anhydride and ammonium maleate, and continuously stirring for 4 +/-0.1 h in a water bath at the temperature of 40 +/-1 ℃ to obtain a mixed solution;
step seven, injecting the mixed solution into a precipitation tank, simultaneously injecting absolute ethyl alcohol, mixing, precipitating, filtering, and washing with absolute ethyl alcohol to obtain a washing filtrate;
step eight, injecting the washing filtrate obtained in the step seven into a vacuum drier for vacuum drying to obtain polysuccinimide with higher purity, and repeating the step six to the step eight for 1 to 3 times to obtain polysuccinimide with high purity;
and step nine, taking out the polysuccinimide solid, adding the polysuccinimide solid into a stirring barrel filled with deionized water, stirring to form a suspension, injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0 +/-0.5, and hydrolyzing at the temperature of 40 +/-2 ℃ for 30 +/-5 min to obtain the potassium polyaspartate solution.
2. The preparation method of the potassium polyaspartate according to claim 1, characterized by comprising a plurality of reaction kettles (1), a drying mechanism (3), a lifter (6), a plurality of high temperature reaction furnaces (7), a plurality of stirring tanks (9), a collection box (12), a precipitation tank (19), a vacuum dryer (14) and a stirring barrel (15) which are arranged in sequence, wherein the drying mechanism (3) is provided with a plurality of first pumping pumps (2), the number and the positions of the first pumping pumps (2) correspond to those of the reaction kettles (1), the feeding end of each first pumping pump (2) is connected with the reaction kettle (1) at the corresponding position, the discharging end of the lifter (6) is provided with a flexible discharging pipe (27), an electric sliding seat (26) is arranged above the feeding end of the plurality of high temperature reaction furnaces (7), and the discharging end of the flexible discharging pipe is connected with the electric sliding seat (26), be connected with second pump material pump (8) between high temperature reacting furnace (7) and agitator tank (9) that correspond, be equipped with third pump material pump (13) between settling tank (19) and vacuum drying machine (14), be equipped with between collecting box (12) and vacuum drying machine (14) air exhaust pump (11), the rear side of settling tank (19) is equipped with transfer case (24), transfer case (24) are connected with agitator tank (9) and settling tank (19) through the pipeline respectively.
3. The preparation method of the potassium polyaspartate according to claim 2, wherein the drying mechanism (3) comprises a drying box, a conveyor is arranged inside the drying box, two ends of the conveyor extend out of the drying box, the discharge end of the first material pumping pump (2) is positioned above the feed end of the conveyor, a scraping plate (5) is arranged at the discharge end of the conveyor, the upper end of the scraping plate (5) is abutted against a track of the conveyor, the lower end of the scraping plate (5) is positioned above a feed hopper of a lifting machine (6), a water filtering box is arranged above the drying box, and a fan (4) is arranged above the water filtering box.
4. The preparation method of the polyaspartic acid potassium salt according to claim 3, characterized in that a stirring tank heat-preserving cylinder (10) is arranged outside the stirring tank (9), a second hot air pipe (20) is connected between the stirring tank heat-preserving cylinder (10) and the air outlet end of the fan (4), a stirring barrel heat-preserving cylinder (16) is arranged outside the stirring barrel (15), a first hot air pipe (17) is connected between the stirring barrel heat-preserving cylinder (16) and the stirring tank heat-preserving cylinder (10), and a return pipe (18) is connected between the vacuum drier (14) and the air exhaust pump (11).
5. The preparation method of the potassium polyaspartate according to claim 4, wherein a multi-way control valve pipe is arranged between the transfer box (24) and the stirring tank (9), a valve body of the multi-way control valve pipe is connected with the corresponding stirring tank (9), the transfer box (24) is connected with the multi-way control valve pipe through a feeding pipe (21), a feeding pipe (22) is arranged between the transfer box (24) and the settling tank (19), a feeding transfer pump and a discharging transfer pump are arranged inside the transfer box (24), the feeding pipe (21) is connected with the feeding transfer pump, and the feeding pipe (22) is connected with the discharging transfer pump.
6. The preparation method of the potassium polyaspartate according to claim 5, wherein the collection box (12) is composed of a collection box and a liquid outlet box, the collection box is located above the liquid outlet box, the air-exhaust air pump (11) is located above the collection box, the collection box is connected with the liquid outlet end of the air-exhaust air pump (11), the liquid outlet box is internally provided with the liquid outlet pump, the liquid outlet end of the liquid outlet pump is connected with the liquid injection pipe (25), the liquid injection pipe (25) is connected to the settling tank (19), and the collection box is internally provided with the molecular sieve.
7. The method for preparing the potassium polyaspartate according to claim 6, wherein a precipitation filter plate is arranged inside the precipitation tank (19), the tail ends of the injection pipe (22) and the injection pipe (25) are positioned on the precipitation filter plate, the precipitation filter plate is arranged in an inclined manner, a discharge gate (23) is arranged on the side part of the precipitation tank (19), the discharge gate (23) is positioned on the lower side of the inclined tail end of the precipitation filter plate, the vacuum dryer (14) is provided with a plurality of discharge hoppers, and one discharge hopper is connected with the stirring barrel (15).
8. The application of the polyaspartic acid potassium prepared by the preparation method of the polyaspartic acid potassium in the plant growth promoter is characterized in that the polyaspartic acid potassium solution is added with water and then sprayed on soil where crops grow, and the addition proportion by weight is 0.1-10%, namely the addition amount of the polyaspartic acid potassium solution in every 100g of clear water is 0.1-10 g.
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