CN114805808B - Preparation method of potassium polyaspartate and application of potassium polyaspartate in plant growth promoter - Google Patents
Preparation method of potassium polyaspartate and application of potassium polyaspartate in plant growth promoter Download PDFInfo
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- CN114805808B CN114805808B CN202210610098.7A CN202210610098A CN114805808B CN 114805808 B CN114805808 B CN 114805808B CN 202210610098 A CN202210610098 A CN 202210610098A CN 114805808 B CN114805808 B CN 114805808B
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 108010064470 polyaspartate Proteins 0.000 title claims abstract description 68
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 68
- 239000011591 potassium Substances 0.000 title claims abstract description 68
- 230000008635 plant growth Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000007952 growth promoter Substances 0.000 title claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 101
- 238000006243 chemical reaction Methods 0.000 claims abstract description 100
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims description 81
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 80
- 238000001035 drying Methods 0.000 claims description 55
- 239000000243 solution Substances 0.000 claims description 49
- 238000012546 transfer Methods 0.000 claims description 47
- 239000007787 solid Substances 0.000 claims description 42
- 238000001556 precipitation Methods 0.000 claims description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 150000003863 ammonium salts Chemical class 0.000 claims description 27
- 230000007246 mechanism Effects 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- 238000007599 discharging Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 23
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 23
- 238000006116 polymerization reaction Methods 0.000 claims description 19
- 229920000805 Polyaspartic acid Polymers 0.000 claims description 18
- 239000012295 chemical reaction liquid Substances 0.000 claims description 16
- 238000002347 injection Methods 0.000 claims description 16
- 239000007924 injection Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 238000005086 pumping Methods 0.000 claims description 14
- 238000007790 scraping Methods 0.000 claims description 14
- 239000002808 molecular sieve Substances 0.000 claims description 12
- 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 12
- 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 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 9
- 230000003301 hydrolyzing effect Effects 0.000 claims description 8
- 239000013067 intermediate product Substances 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 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
- 239000012266 salt solution Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000002689 soil Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 18
- 230000000694 effects Effects 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 12
- 230000004720 fertilization Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000012010 growth Effects 0.000 abstract description 7
- 238000000746 purification Methods 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000003337 fertilizer Substances 0.000 description 13
- 238000004321 preservation Methods 0.000 description 11
- 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
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 5
- 235000017491 Bambusa tulda Nutrition 0.000 description 5
- 241001330002 Bambuseae Species 0.000 description 5
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 5
- 239000011425 bamboo Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 3
- 239000011976 maleic acid Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 235000016709 nutrition Nutrition 0.000 description 3
- 230000035764 nutrition Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 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
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- -1 nitrogen-containing compound Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 208000035240 Disease Resistance Diseases 0.000 description 1
- 241001057636 Dracaena deremensis Species 0.000 description 1
- 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
- 239000003655 absorption accelerator Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000003945 anionic surfactant 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
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 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
- 230000000361 pesticidal effect 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
- 238000011160 research Methods 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
Landscapes
- 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 potassium polyaspartate and application of the potassium polyaspartate 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 effect of promoting plant growth and the like of the existing potassium polyaspartate. The preparation method of the potassium polyaspartate can be matched through a plurality of steps of processes in the number function of a plurality of devices to form production line production, can not stay on a certain procedure, works together after all parts are opened through time difference, does not need to be frequently started and stopped for waiting, has high automation degree, higher efficiency and small energy consumption, has good fertilization effect as a plant growth promoter, and can promote effective growth. The invention can realize the control of the reaction temperature of the stirring tank and the stirring barrel, and ensure the temperature stability; the material collection and recycling of the material which does 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 potassium polyaspartate solution has high purity.
Description
Technical Field
The invention belongs to the technical field of plant growth promoters, and relates to a preparation method of potassium polyaspartate, in particular to application of potassium polyaspartate in a plant growth promoter.
Background
The molecular formula of the potassium polyaspartate- (C4H 4O 3N) N- (is mainly applied to the field of green agricultural development in agriculture, has the advantages of long-chain protein property, anionic surfactant and the like, and can be used as a carrier to prepare fertilizers with different formulations, and can be used as a base fertilizer, an additional fertilizer and an external root fertilizer, and the nutrition enrichment effect of the potassium polyaspartate on the fertilizer is realized.
Promote the absorption of crop to nutrient elements, promote the growth of root system, increase yield, strengthen plant, strengthen stress resistance, reach deep leaf, improve quality, and use potassium polyaspartate, and can raise fertilizer utilization by 30-50% and reduce fertilizer consumption by more than 20%. The potassium polyaspartate has the characteristics of no toxicity, no residue and the like. The first U.S. gazette "president green chemical warfare will" was obtained in 96 years.
The novel crop nutrition absorption accelerator developed by adopting the bionic synthesis technology (which is different from common crop hormone, has the characteristics of small consumption and high efficiency, can save one third of the consumption of chemical fertilizers per mu, can enhance the pesticide effect, improve the disease resistance and stress resistance of crops), has comprehensive nutrition for crops, stimulates the activity of biological enzymes, strengthens the absorption effect of nitrogen, phosphorus, potassium and trace elements, and is particularly obvious for the three elements of zinc, manganese and iron of crops, so that the polyaspartic acid potassium is an attractive new-generation fertilizer synergistic granule.
The synthesis process research of polyaspartic acid mainly comprises 4 routes: solid-phase thermal shrinkage polymerization of L-aspartic acid, liquid-phase thermal shrinkage polymerization of L-aspartic acid, advanced chemical reaction of maleic anhydride and derivatives thereof and nitrogen-containing compounds, and then thermal shrinkage polymerization, direct liquid-phase polymerization of maleic anhydride and derivatives thereof and nitrogen-containing compounds.
However, the 4 routes have certain defects, namely, the L-aspartic acid is used as a raw material, the cost is high, the limitation is high, the solid phase reaction is heated unevenly, the mass and heat transfer effect is poor, the reaction is insufficient, the purity is low, the time of the two latter processes is long (frequent start and stop are needed, the waiting period is long), and the molecular weight of the obtained polymerization product is not high; meanwhile, the intermediate solvent can not be recycled, and the purity is low.
Based on the above, we propose a preparation method of potassium polyaspartate and application thereof in plant growth promoters; the preparation method of the potassium polyaspartate can be matched through a plurality of steps of processes in the number function of a plurality of devices, so that the production line is formed, the potassium polyaspartate can not stay in a certain procedure, all parts work together after being opened through time difference, the potassium polyaspartate does not need to be frequently started and stopped for waiting, the automation degree is high, the efficiency is higher, and the energy consumption is low;
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 barrel and the stirring barrel heat-preserving barrel, so that the temperature stability is ensured;
the collection box, the air suction pump and the molecular sieve are matched to realize the collection and recycling of materials which do not react in the middle of absolute ethyl alcohol, N-dimethylformamide and the like, so that the energy is saved, the emission is reduced, and the cost is reduced;
through the cooperation of the stirring tank, the precipitation tank and the vacuum dryer, the purification of the polysuccinimide can be repeatedly carried out, and the polysuccinimide with high purity is obtained, so that the potassium polyaspartate solution has high purity.
The application of the polyaspartic acid potassium in the plant growth promoter has good fertilization effect, can promote effective growth, has the best effect of 10g of fertilization amount of polyaspartic acid potassium solution in per 100g of clear water, 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 at solving the problems in the prior art, and provides a preparation method of potassium polyaspartate and application of the potassium polyaspartate in a plant growth promoter, wherein the technical problems to be solved by the invention are as follows: how to realize the process cooperation of a plurality of steps in the number of a plurality of devices, so that the production line is formed, the devices cannot stay in a certain process, all the components work together after being opened by time difference, the devices do not need to be frequently started and stopped for waiting, 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 has good fertilization effect, and the effective growth can be promoted.
The aim of the invention can be achieved by the following technical scheme:
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, and carrying out hydrolysis reaction at 60+/-2 ℃ for 30+/-5 min to obtain maleic anhydride solution, wherein the hydrolysis chemical equation 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, and carrying out mixed reaction at the temperature of 80+/-5 ℃ for 2+/-0.1 h to obtain a maleic acid ammonium salt solution mixture;
stopping heating the reaction kettle, introducing cooling water, and opening the reaction kettle to release the reaction liquid when the temperature is reduced to 50+/-1 ℃;
step four, the reaction solution is led into a drying mechanism with the temperature of 80+/-5 ℃ for drying, so that white solid ammonium salt is obtained;
putting the solid ammonium salt into a high-temperature reaction furnace, introducing nitrogen, heating the high-temperature reaction furnace, and performing thermal shrinkage polymerization reaction at the temperature of 210+/-5 ℃ for 4+/-0.1 h to obtain an intermediate product polysuccinimide;
step six, the polysuccinimide is led into a stirring tank filled with N, N-dimethylformamide, wherein the mass of the N, N-dimethylformamide is 10+/-0.1 times that of the polysuccinimide, the polysuccinimide is purified and dissolved, namely the polysuccinimide is dissolved in the N, N-dimethylformamide, maleic anhydride and maleic acid ammonium salt are insoluble, and the mixture is continuously stirred for 4+/-0.1 h in a water bath with 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 washing filtrate;
step eight, injecting the washing filtrate obtained in the step seven into a vacuum dryer for vacuum drying to obtain polysuccinimide with higher purity, and repeating the steps six-eight for 1-3 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, then injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0+/-0.5, hydrolyzing at the temperature of 40+/-2 ℃ for 30+/-5 min, and obtaining the potassium polyaspartate solution.
The utility model provides a preparation method of potassium polyaspartate, includes a plurality of reation kettle, stoving mechanism, lifting machine, a plurality of high temperature reaction furnaces, a plurality of agitator tanks, collecting box, precipitation jar, vacuum dryer and agitator tank that set gradually, be equipped with a plurality of first pump on the stoving mechanism, the quantity and the position of first pump correspond with reation kettle, the reation kettle of corresponding position is connected to first pump feed end, the discharge end of lifting machine is equipped with flexible discharging pipe, the top of the feed end of a plurality of high temperature reaction furnaces is equipped with electronic sliding seat, the discharge end of flexible discharging pipe is connected on electronic sliding seat, be connected with the second pump between high temperature reaction furnace and the corresponding agitator tank, be equipped with the third pump between precipitation jar and the vacuum dryer, be equipped with the air pump between collecting box and the vacuum dryer, the rear side of precipitation jar is equipped with the transfer box, the transfer box is connected with agitator tank and precipitation jar through the pipeline 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 raise the temperature to obtain maleic anhydride solution, one reaction kettle is started after every 0.5h, and six reaction kettles are matched with the drying mechanism to form assembly line operation; injecting a certain amount of liquid ammonia into a reaction kettle, heating the reaction kettle, and carrying out mixed 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, and discharging the reaction liquid when the reaction kettle is hot; sequentially introducing the reaction liquid of the corresponding reaction kettle into a drying mechanism for drying every 0.5h through a first material pumping pump to obtain white solid ammonium salt; lifting the solid ammonium salt by a lifting machine, sequentially introducing the solid ammonium salt into eight high-temperature reaction furnaces by matching a flexible discharging pipe with an electric sliding seat, introducing nitrogen, heating the high-temperature reaction furnaces, and performing thermal shrinkage polymerization reaction to obtain an intermediate product polysuccinimide; the polysuccinimide is led into a stirring tank filled with N, N-dimethylformamide through a second pumping pump, the polysuccinimide is purified and dissolved, namely the polysuccinimide is dissolved in the N, N-dimethylformamide, maleic anhydride and maleic ammonium salt to obtain a mixed solution, the mixed solution is injected into a precipitation tank through a transfer box, and meanwhile, absolute ethyl alcohol is injected into the precipitation tank for mixed precipitation and filtration, and washing is carried out by using absolute ethyl alcohol to obtain washing filtrate; the third pump is used for injecting the washing filtrate into a vacuum dryer for vacuum drying to obtain polysuccinimide with higher purity, and sequentially injecting the polysuccinimide into the stirring tank for repeating the steps for a plurality of times to obtain polysuccinimide with high purity; adding polysuccinimide solid into a stirring barrel filled with deionized water, stirring to form suspension, then injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0+/-0.5, hydrolyzing at 40+/-2 ℃ for 30+/-5 min, and obtaining the potassium polyaspartate solution.
The drying mechanism comprises a drying box, a conveyor is arranged inside the drying box, two ends of the conveyor extend out of the drying box, a discharge end of a first pumping pump is located above a feed end of the conveyor, a scraping plate is arranged at the discharge end of the conveyor, the upper end of the scraping plate is abutted to a crawler belt of the conveyor, the lower end of the scraping plate is located above a feed hopper of the elevator, a water filtering tank is arranged above the drying box, and a fan is arranged above the water filtering tank.
By adopting the structure, the reaction liquid corresponding to the reaction kettle is sequentially led into the upper part of the feeding end of the conveyor through the first pumping pump every 0.5h, the reaction liquid is dried by the drying box to obtain white solid ammonium salt, the scraping plate scrapes the white solid ammonium salt off the crawler belt of the conveyor and falls into the feeding hopper of the lifting machine, the lifting machine sequentially lifts the white solid ammonium salt into the high-temperature reaction furnace, the fan sucks out hot air in the drying mechanism, and the hot air is filtered by the water filtering box to obtain dry hot air.
The outside of agitator tank is equipped with agitator tank heat preservation section of thick bamboo, is connected with the second hot air pipe between agitator tank heat preservation section of thick bamboo and the air-out end of fan, and the outside of agitator tank is equipped with agitator tank heat preservation section of thick bamboo, is connected with first hot air pipe between agitator tank heat preservation section of thick bamboo and the agitator tank heat preservation section of thick bamboo, is connected with the back flow between vacuum dryer and the air-out pump.
By adopting the structure, the fan blows dry hot air into the stirring tank heat preservation barrel through the second hot air pipe, keeps the temperature of the stirring tank constant, and enters the stirring tank heat preservation barrel through the first hot air pipe, keeps the temperature of the stirring tank constant, and the air pump screens the steam molecular sieves such as ethanol generated during drying of the vacuum dryer to form anhydrous ethanol and N, N-dimethylformamide, and the anhydrous ethanol and N-dimethylformamide are sucked out through the return pipe and collected into the collecting box for condensation.
Be equipped with the multiway control valve pipe between transfer case and the agitator tank, the valve body of multiway control valve pipe is connected with the agitator tank that corresponds, is connected through the inlet pipe between transfer case and the multiway control valve pipe, is equipped with the notes material pipe between transfer case and the settling tank, 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, and notes material pipe is connected with ejection of compact transfer pump.
By adopting the structure, the transfer box is matched with the multi-way control valve pipe, the feeding transfer pump pumps the mixed solution in the stirring tank corresponding to the valve body of the multi-way control valve pipe into the transfer box through the feeding pipe, and then the mixed solution is injected into the precipitation tank through the feeding pipe by the discharging transfer pump for precipitation.
The collecting box comprises collecting liquid box and play liquid case, and collecting liquid box is located out liquid case top, and the air pump that bleeds is located collecting liquid box top, and collecting liquid case is connected with the play liquid end of air pump, goes out liquid incasement portion and is equipped with out the liquid pump, goes out the liquid end of liquid pump and annotates liquid union coupling, annotates liquid union coupling on settling tank, and collecting liquid incasement portion is equipped with the molecular sieve.
By adopting the structure, the air pump pumps the steam generated during the drying of the vacuum dryer into the collecting tank for condensation, then the steam is screened by the internal molecular sieve to form absolute ethyl alcohol and N, N-dimethylformamide, the absolute ethyl alcohol is stored in the liquid outlet tank, the liquid outlet pump pumps the absolute ethyl alcohol liquid in the liquid outlet tank, the absolute ethyl alcohol liquid is injected into the settling tank through the liquid injection pipe for settling and washing, and the N, N-dimethylformamide can be purified and reused after being collected.
The inside of settling tank is equipped with the settling filter plate, and the end of notes material pipe and notes liquid pipe is located the settling filter plate, and the settling filter plate slope sets up, and the lateral part of settling tank is equipped with the discharge door, and the discharge door is located the downside at the settling filter plate slope end, and the vacuum dryer is equipped with a plurality of hopper, and one of them hopper is connected with the agitator.
By adopting the structure, the solid precipitated is collected on a precipitation filter plate, the discharge gate is opened to discharge, the washing solution is polysuccinimide solution, the polysuccinimide with higher purity is obtained by a vacuum dryer, the polysuccinimide is discharged through a certain discharge hopper, the polysuccinimide is sequentially injected into the stirring tank after being collected, the polysuccinimide with high purity can be circularly repeated for a plurality of times, and the polysuccinimide with high purity is obtained by mixing and hydrolyzing the polysuccinimide with one discharge hopper and then is guided into the stirring tank to obtain the potassium polyaspartate solution with high purity.
The application of the polyaspartic acid potassium in the plant growth promoter comprises the steps of adding water into a polyaspartic acid potassium solution, spraying the solution onto the soil where crops grow, wherein the adding weight ratio is 0.1-10%, namely the adding amount of the polyaspartic acid potassium solution in per 100g of clear water is 0.1-10 g
Compared with the prior art, the preparation method of the potassium polyaspartate has the following advantages:
the invention can be matched through a plurality of steps of processes in the number function of a plurality of devices to form production line production, can not stay on a certain procedure, can work together after all parts are opened by time difference, and can not be frequently started and stopped for waiting, thereby having high automation degree, higher efficiency and small 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 barrel and the stirring barrel heat-preserving barrel, so that the temperature stability is ensured;
the collection box, the air suction pump and the molecular sieve are matched to realize the collection and recycling of materials which do not react in the middle of absolute ethyl alcohol, N-dimethylformamide and the like, so that the energy is saved, the emission is reduced, and the cost is reduced;
through the cooperation of the stirring tank, the precipitation tank and the vacuum dryer, the purification of the polysuccinimide can be repeatedly carried out, and the polysuccinimide with high purity is obtained, so that the potassium polyaspartate solution has high purity.
The application of the polyaspartic acid potassium in the plant growth promoter has good fertilization effect, the fertilization amount is 10g of the polyaspartic acid potassium 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 the plant growth promoter.
Drawings
FIG. 1 is a process flow diagram 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 schematic perspective view of a part of the components of the present invention.
FIG. 6 is a table of average growth height experiments for corn plants from 0 to 28 days in the corn test field.
In the figure, 1, a reaction kettle; 2. a first material pumping pump; 3. a drying mechanism; 4. a blower; 5. a scraping plate; 6. a hoist; 7. a high temperature reaction furnace; 8. a second material pumping pump; 9. a stirring tank; 10. a stirring tank heat preservation cylinder; 11. an air pump; 12. a collection box; 13. a third material pumping pump; 14. a vacuum dryer; 15. a stirring barrel; 16. a stirring barrel heat preservation barrel; 17. a first hot air pipe; 18. a return pipe; 19. a precipitation 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. a flexible discharge pipe.
Detailed Description
The following are specific embodiments of the present invention and the technical solutions of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
As shown in 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, and carrying out hydrolysis reaction at 60+/-2 ℃ for 30+/-5 min to obtain maleic anhydride solution, wherein the hydrolysis chemical equation 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, and carrying out mixed reaction at the temperature of 80+/-5 ℃ for 2+/-0.1 h to obtain a maleic acid ammonium salt solution mixture;
stopping heating the reaction kettle, introducing cooling water, and opening the reaction kettle to release the reaction liquid when the temperature is reduced to 50+/-1 ℃;
step four, the reaction solution is led into a drying mechanism with the temperature of 80+/-5 ℃ for drying, so that white solid ammonium salt is obtained;
putting the solid ammonium salt into a high-temperature reaction furnace, introducing nitrogen, heating the high-temperature reaction furnace, and performing thermal shrinkage polymerization reaction at the temperature of 210+/-5 ℃ for 4+/-0.1 h to obtain an intermediate product polysuccinimide;
step six, the polysuccinimide is led into a stirring tank filled with N, N-dimethylformamide, wherein the mass of the N, N-dimethylformamide is 10+/-0.1 times that of the polysuccinimide, the polysuccinimide is purified and dissolved, namely the polysuccinimide is dissolved in the N, N-dimethylformamide, maleic anhydride and maleic acid ammonium salt are insoluble, and the mixture is continuously stirred for 4+/-0.1 h in a water bath with 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 washing filtrate;
step eight, injecting the washing filtrate obtained in the step seven into a vacuum dryer for vacuum drying to obtain polysuccinimide with higher purity, and repeating the steps six-eight for 1-3 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, then injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0+/-0.5, hydrolyzing at the temperature of 40+/-2 ℃ for 30+/-5 min, and obtaining the potassium polyaspartate solution.
As shown in fig. 4-5, the preparation method of the potassium polyaspartate comprises a plurality of reaction kettles 1, a drying mechanism 3, a lifting machine 6, a plurality of high-temperature reaction kettles 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 sequentially arranged, wherein the drying mechanism 3 is provided with a plurality of first material suction pumps 2, the number and positions of the first material suction pumps 2 correspond to those of the reaction kettles 1, the feeding ends of the first material suction pumps 2 are connected with the reaction kettles 1 at the corresponding positions, the discharging ends of the lifting machine 6 are provided with flexible discharging pipes 27, electric sliding seats 26 are arranged above the feeding ends of the plurality of high-temperature reaction kettles 7, the discharging ends of the flexible discharging pipes are connected to the electric sliding seats 26, a second material suction pump 8 is connected between the high-temperature reaction kettles 7 and the corresponding stirring tanks 9, a third material suction pump 13 is arranged between the precipitation tank 19 and the vacuum dryer 14, an air suction pump 11 is arranged between the collection box 12 and the vacuum dryer 14, and the rear side of the precipitation tank 19 is provided with a transfer box 24, and the transfer box 24 is respectively connected with the stirring tanks 9 and the stirring tank 19 through pipelines;
injecting a certain amount of maleic anhydride and a certain amount of water into the reaction kettle 1, heating the reaction kettle to raise the temperature to obtain maleic acid solution, starting one reaction kettle 1 after every 0.5h, and matching the six reaction kettles 1 with a drying mechanism to form pipelining operation; injecting a certain amount of liquid ammonia into the reaction kettle 1, heating the reaction kettle 1, and carrying out mixed 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 1 to discharge the reaction liquid when the reaction kettle is hot; the reaction liquid corresponding to the reaction kettle 1 is sequentially led into a drying mechanism 3 for drying every 0.5h through a first material pumping pump 2, so that white solid ammonium salt is obtained; lifting the solid ammonium salt by a lifting machine 6, sequentially introducing the solid ammonium salt into eight high-temperature reaction furnaces 7 through the cooperation of a flexible discharging pipe and an electric sliding seat 26, introducing nitrogen, heating the high-temperature reaction furnaces 7, and performing thermal shrinkage polymerization reaction to obtain an intermediate product polysuccinimide; the polysuccinimide is led into a stirring tank 9 filled with N, N-dimethylformamide through a second pumping pump 8, the polysuccinimide is purified and dissolved, namely the polysuccinimide is dissolved in the N, N-dimethylformamide, maleic anhydride and ammonium maleate salt to obtain a mixed solution, the mixed solution is injected into a precipitation tank 19 through a transfer box 24, and meanwhile, absolute ethyl alcohol is injected into the precipitation tank for mixed precipitation and filtration, and the washing filtrate is obtained after washing with the absolute ethyl alcohol; the third pumping pump 13 injects the washing filtrate into a vacuum dryer for vacuum drying to obtain polysuccinimide with higher purity, sequentially injects the polysuccinimide into the stirring tank 9, and repeats for 1-3 times to obtain polysuccinimide with high purity; adding polysuccinimide solid into a stirring barrel 15 filled with deionized water, stirring to form suspension, then injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0+/-0.5, hydrolyzing at 40+/-2 ℃ for 30+/-5 min, and obtaining 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, a discharge end of the first suction pump 2 is positioned above a 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 crawler belt of the conveyor, the lower end of the scraping plate 5 is positioned above a feed hopper of the hoister 6, a water filtering tank is arranged above the drying box, and a fan 4 is arranged above the water filtering tank; the reaction liquid corresponding to the reaction kettle 1 is guided into the upper part of the feeding end of the conveyor through the first pumping pump 2 every 0.5h in sequence, the reaction liquid is dried by the drying box to obtain white solid ammonium salt, the scraping plate 5 scrapes the white solid ammonium salt off the crawler belt of the conveyor and falls into the feeding hopper of the lifting machine 6, the lifting machine 6 sequentially lifts the white solid ammonium salt into the high-temperature reaction furnace 7, the fan 4 sucks out hot air in the drying mechanism 3, and the hot air is filtered by the water filtering box to obtain dry hot air.
The outside of the stirring tank 9 is provided with a stirring tank heat-preserving cylinder 10, 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 tank heat-preserving cylinder 16 is arranged outside the stirring tank 15, a first hot air pipe 17 is connected between the stirring tank heat-preserving cylinder 16 and the stirring tank heat-preserving cylinder 10, and a return pipe 18 is connected between the vacuum dryer 14 and the air suction air pump 11; the fan 4 blows dry hot air into the stirring tank heat-preserving cylinder 10 through the second hot air pipe 20, keeps the temperature of the stirring tank 9 constant, and then enters the stirring tank heat-preserving cylinder 16 through the first hot air pipe 17, keeps the temperature of the stirring tank 15 constant, and the air pump 11 screens the steam molecular sieves such as ethanol and the like generated when the vacuum dryer 14 dries to form anhydrous ethanol and N, N-dimethylformamide, and the anhydrous ethanol and the N-dimethylformamide are sucked out through the return pipe 18 and collected into the collecting box 12 for condensation.
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 feed pipe 21, a feed 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 in the transfer box 24, the feed pipe 21 is connected with the feeding transfer pump, and the feed pipe 22 is connected with the discharging transfer pump; the transfer box 24 is matched with the multi-way control valve pipe, the feeding transfer pump pumps 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, and then the mixed solution is injected into the sedimentation tank 19 through the feeding pipe 22 by the discharging transfer pump for sedimentation.
The collecting box 12 consists of a collecting liquid box and a liquid outlet box, the collecting liquid box is positioned above the liquid outlet box, the air suction pump 11 is positioned above the collecting liquid box, the collecting liquid box is connected with the liquid outlet end of the air suction pump 11, a liquid outlet pump is arranged in the liquid outlet box, 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 a molecular sieve is arranged in the collecting liquid box; the air pump 11 pumps the steam generated during the drying of the vacuum drier 14 into the collecting tank for condensation, then the anhydrous ethanol and N, N-dimethylformamide are formed by screening through the internal molecular sieve, the anhydrous ethanol is stored in the liquid outlet tank, the liquid outlet pump pumps the anhydrous ethanol liquid in the liquid outlet tank, the liquid is injected into the precipitation tank 19 through the liquid injection pipe 25 for precipitation and washing, and the N, N-dimethylformamide can be collected for purification and reuse.
The inside of the settling tank 19 is provided with a settling filter plate, 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 obliquely arranged, the side part of the settling tank 19 is provided with a discharge door 23, the discharge door 23 is positioned at 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 discharge hopper is connected with the stirring barrel 15; the solid precipitated is collected on a precipitation filter plate, a discharge gate 23 is opened to discharge the solid, the washing solution is polysuccinimide solution, the polysuccinimide with higher purity is obtained by a vacuum drier 14, the solid is discharged through a discharge hopper, the solid is sequentially injected into a stirring tank 9 after being collected, the solid can be circularly repeated for 1-3 times to obtain polysuccinimide with high purity, and the polysuccinimide with high purity is introduced into the stirring tank 15 for mixed hydrolysis from one of the discharge hoppers to obtain potassium polyaspartate solution with high purity.
Example 1
Injecting a certain amount of maleic anhydride and a certain amount of water into the reaction kettle 1, heating the reaction kettle to raise the temperature to obtain maleic acid solution, starting one reaction kettle 1 after every 0.5h, and matching the six reaction kettles 1 with a drying mechanism to form pipelining operation; injecting a certain amount of liquid ammonia into the reaction kettle 1, heating the reaction kettle 1, and carrying out mixed 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 1 to discharge the reaction liquid when the reaction kettle is hot;
the reaction liquid corresponding to the reaction kettle 1 is sequentially led into the upper part of the feeding end of the conveyor every 0.5h through the first pumping pump 2, the reaction liquid is dried by the drying box to obtain white solid ammonium salt, and the white solid ammonium salt is scraped from the crawler belt of the conveyor by the scraping plate 5 and falls into the feed hopper of the lifting machine 6;
lifting the solid ammonium salt by a lifting machine 6, sequentially introducing the solid ammonium salt into eight high-temperature reaction furnaces 7 through the cooperation of a flexible discharging pipe and an electric sliding seat 26, introducing nitrogen, heating the high-temperature reaction furnaces 7, and performing thermal shrinkage polymerization reaction to obtain an intermediate product polysuccinimide;
the polysuccinimide is led into a stirring tank 9 filled with N, N-dimethylformamide through a second pump 8, and is purified and dissolved, namely, the polysuccinimide is dissolved in the N, N-dimethylformamide, maleic anhydride and maleic ammonium salt are insoluble, so as to obtain a mixed solution;
the feeding transfer pump pumps the mixed solution in the stirring tank 9 corresponding to the valve body of the multi-way control valve pipe into the transfer tank 24 through the feeding pipe 21, then the mixed solution is injected into the precipitation tank 19 through the feeding pipe 22 by the discharging transfer pump, meanwhile, the liquid outlet pump pumps the absolute ethyl alcohol liquid in the liquid outlet tank, the absolute ethyl alcohol liquid is injected into the precipitation tank 19 through the liquid injection pipe 25, precipitation and washing are carried out, precipitated solids are collected on a precipitation filter plate, a discharge gate 23 is opened for discharge, and the obtained washing solution is polysuccinimide solution;
the third pumping pump 13 injects the washing filtrate into a vacuum dryer for vacuum drying to obtain polysuccinimide with higher purity, sequentially injects the polysuccinimide into the stirring tank 9, and repeats for 1-3 times to obtain polysuccinimide with high purity;
adding the high-purity polysuccinimide solid into a stirring barrel 15 filled with deionized water, stirring to form a suspension, then injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0+/-0.5, hydrolyzing at 40+/-2 ℃ for 30+/-5 min to obtain high-purity potassium polyaspartate solution;
the fan 4 sucks out the hot air in the drying mechanism 3, the hot air is filtered by the water filtering tank to obtain dry hot air, the fan 4 blows the dry hot air into the stirring tank heat preservation cylinder 10 through the second hot air pipe 20, the temperature of the stirring tank 9 is kept constant, and the hot air enters the stirring tank heat preservation cylinder 16 through the first hot air pipe 17, so that the temperature of the stirring tank 15 is kept constant;
the air pump 11 pumps the steam generated during the drying of the vacuum drier 14 into the collecting tank for condensation, then the anhydrous ethanol and N, N-dimethylformamide are formed by screening through the internal molecular sieve, the anhydrous ethanol is stored in the liquid outlet tank, the liquid outlet pump pumps the anhydrous ethanol liquid in the liquid outlet tank, the liquid is injected into the precipitation tank 19 through the liquid injection pipe 25 for precipitation and washing, and the N, N-dimethylformamide can be collected for purification and reuse.
In conclusion, the invention can be matched through a plurality of steps of processes in the number function of a plurality of devices to form the production line, the production line can not stay on a certain procedure, all parts can work together after being opened through time difference, and the equipment does not need to be frequently started and stopped for waiting, so that the automation degree is high, the efficiency is higher, and the energy consumption is low;
the reaction temperature of the stirring tank 9 and the stirring tank 15 is controlled by matching the drying mechanism 3, the fan 4, the stirring tank heat-preserving cylinder 10 and the stirring tank heat-preserving cylinder 16, so that the temperature stability is ensured;
the collection box 12 and the air suction pump 11 are matched with the molecular sieve, so that the materials which do not react in the middle of the anhydrous ethanol, the N, N-dimethylformamide and the like are collected and recycled, the energy is saved, the emission is reduced, and the cost is reduced;
the stirring tank 9, the precipitation tank 19 and the vacuum dryer 14 are matched, so that the purification of polysuccinimide can be repeatedly performed, and the polysuccinimide with high purity can be obtained, so that the potassium polyaspartate solution with high purity can be obtained.
In this embodiment, the potassium polyaspartate solution may be further dried to obtain brown potassium polyaspartate, and the drying mode is to add a conveyer inside the drying box to inject the potassium polyaspartate solution for drying.
Example 2
Solid phase thermal shrinkage polymerization of L-aspartic acid: synthesizing an intermediate product polysuccinimide by taking L-aspartic acid as a raw material, and then hydrolyzing with KOH to obtain potassium polyaspartate;
example 3
Liquid phase thermal shrinkage polymerization of aspartic acid: the L-aspartic acid is raised to the temperature required by the reaction in a solvent to carry out polymerization reaction, and then the product potassium polyaspartate is obtained through separation, purification and hydrolysis;
the disadvantages of examples 2 and 3 are that L-aspartic acid is used as a raw material, the cost is high, the limitation is large, the solid phase reaction is heated unevenly, the mass and heat transfer effect is poor, the reaction is insufficient, and the purity is low.
Example 4
The indirect polymerization of maleic anhydride and its derivative and nitrogen-containing compound is to stir maleic anhydride and its derivative and nitrogen-containing compound in water solution for reacting for a certain period of time, then dry in oven to obtain ammonium salt mixture of maleic acid, continuously raise temperature to polymerization temperature, quickly evaporate water with the rise of temperature, make reactant become viscous liquid, gradually deepen color, then make polymerization reaction in molten state, make reactant become solid gradually in later stage of polymerization reaction, mobility is worse, then hydrolyze to obtain polyaspartic acid solution;
example 4 is a simple way of example 1, i.e. no quantitative coordination between the parts, longer overall process flow, (frequent start-up and shut-down, long waiting period) and low molecular weight of the resulting polymer; meanwhile, the intermediate solvent can not be recycled, and the purity is low.
The application of the polyaspartic acid potassium prepared by the preparation method in the plant growth promoter is that the polyaspartic acid potassium solution is sprayed on the soil where crops grow after being added with water, the adding weight ratio is 0.1-10%, namely, the adding amount of the polyaspartic acid potassium solution in per 100g of clear water is 0.1-10 g.
Simultaneously taking a certain amount of the potassium polyaspartate prepared in the examples 2-4 for application in plant growth promoters,
in the same corn test field, the plant was divided into A, B, C, D, E, F, G, H and I,9 test areas, area A was used as a blank, area B, C, D was used as fertilizer by potassium polyaspartate prepared according to the method of example 1, area E, F, G was used as fertilizer by potassium polyaspartate prepared according to the method of examples 2-4, and area H, I was used as fertilizer by potassium polyaspartate. The plants tested grew naturally for an average growth height (cm) of 0-28 days.
The experimental table is as follows (table 1):
TABLE 1
The preparation method has the advantages of good fertilization effect, promotion of effective growth, optimal fertilization effect of 10g of potassium polyaspartate solution added into 100g of clear water, lower cost and higher efficiency, and can be applied to industrial production in plant growth promoters.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
Claims (2)
1. A preparation method of potassium polyaspartate is characterized by comprising the following steps:
the device for preparing the polyaspartic acid potassium comprises a plurality of reaction kettles (1), a drying mechanism (3), a lifting machine (6), a plurality of high-temperature reaction furnaces (7), a plurality of stirring tanks (9), a collecting box (12), a precipitation tank (19), a vacuum dryer (14) and stirring tanks (15) which are sequentially arranged, wherein a plurality of first material suction pumps (2) are arranged on the drying mechanism (3), the number and the positions of the first material suction pumps (2) are corresponding to those of the reaction kettles (1), the feeding ends of the first material suction pumps (2) are connected with the reaction kettles (1) at the corresponding positions, the discharging ends of the lifting machine (6) are provided with flexible discharging pipes (27), the upper parts of the feeding ends of the plurality of high-temperature reaction furnaces (7) are provided with electric sliding seats (26), the discharging ends of the flexible discharging pipes are connected to the electric sliding seats (26), a second material suction pump (8) is connected between the high-temperature reaction furnaces (7) and the corresponding stirring tanks (9), a third material suction pump (13) is arranged between the precipitation tank (19) and the vacuum dryer (14), the collecting box (12) and the vacuum dryer (14) are provided with feeding ends connected with the stirring tanks (24), and the stirring tanks (19) are respectively connected with the stirring tanks (24);
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, a discharge end of the first suction pump (2) is located above a 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 crawler of the conveyor, the lower end of the scraping plate (5) is located above a feed hopper of the hoister (6), a water filtering tank is arranged above the drying box, and a fan (4) is arranged above the water filtering tank;
the stirring tank is 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 tank heat-preserving cylinder (16) is arranged outside the stirring tank (15), a first hot air pipe (17) is connected between the stirring tank heat-preserving cylinder (16) and the stirring tank heat-preserving cylinder (10), and a return pipe (18) is connected between the vacuum dryer (14) and the air suction air pump (11);
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 in 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;
the collecting box (12) consists of a collecting liquid box and a liquid outlet box, the collecting liquid box is positioned above the liquid outlet box, the air suction pump (11) is positioned above the collecting liquid box, the collecting liquid box is connected with the liquid outlet end of the air suction pump (11), a liquid outlet pump is arranged in the liquid outlet box, 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 a molecular sieve is arranged in the collecting liquid box;
the inside of the settling tank (19) is provided with a settling filter plate, 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 obliquely arranged, the side part of the settling tank (19) is provided with a discharge door (23), the discharge door (23) is positioned at 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 discharge hopper is connected with the stirring barrel (15);
the preparation method comprises the following steps:
firstly, injecting a certain amount of maleic anhydride and a certain amount of water into one reaction kettle (1), heating the reaction kettle (1), carrying out hydrolysis reaction at the temperature of 60+/-2 ℃ for 30+/-5 min to obtain maleic anhydride solution, starting one reaction kettle (1) after every 0.5h, and matching the six reaction kettles (1) with a drying mechanism (3) to form pipelining operation;
injecting a certain amount of liquid ammonia into a reaction kettle (1), wherein the amount of the liquid ammonia is 1.2+/-0.1 times of that of maleic anhydride, heating the reaction kettle (1), and carrying out mixed reaction at the temperature of 80+/-5 ℃ for 2+/-0.1 h to obtain a maleic acid ammonium salt solution mixture;
stopping heating the reaction kettle, introducing cooling water, and opening the reaction kettle (1) to discharge the reaction liquid when the temperature is reduced to 50+/-1 ℃;
step four, the reaction liquid corresponding to the reaction kettle 1 is sequentially led into the upper part of the feeding end of the conveyor every 0.5h through a first material pumping pump (2), the reaction liquid is dried through a drying box with the temperature of 80+/-5 ℃ to obtain white solid ammonium salt, and the white solid ammonium salt is scraped from the crawler belt of the conveyor by a scraping plate 5 and falls into the feed hopper of a lifting machine (6);
step five, lifting solid ammonium salt by a lifting machine (6), sequentially introducing the solid ammonium salt into eight high-temperature reaction furnaces (7) through the cooperation of a flexible discharging pipe and an electric sliding seat 26, introducing nitrogen, heating the high-temperature reaction furnaces (7), performing thermal shrinkage polymerization reaction, and performing thermal shrinkage polymerization reaction at 210+/-5 ℃ for 4+/-0.1 h to obtain an intermediate product polysuccinimide, and obtaining the intermediate product polysuccinimide;
step six, the polysuccinimide is led into a stirring tank (9) filled with N, N-dimethylformamide by a second pump (8), the mass of the N, N-dimethylformamide is 10+/-0.1 times that of the polysuccinimide, the polysuccinimide is purified and dissolved, namely the polysuccinimide is dissolved in the N, N-dimethylformamide, maleic anhydride and maleic acid ammonium salt are insoluble, and the mixture is continuously stirred in a water bath at 40+/-1 ℃ for 4+/-0.1 h to obtain a mixed solution;
step seven, the feeding transfer pump pumps the mixed solution in the stirring tank (9) corresponding to the valve body of the multi-way control valve pipe into the transfer tank (24) through the feeding pipe (21), then the mixed solution is injected into the precipitation tank (19) through the feeding pipe (22) by the discharging transfer pump, meanwhile, the liquid pump pumps the absolute ethyl alcohol liquid in the liquid outlet tank, the absolute ethyl alcohol liquid is injected into the precipitation tank (19) through the liquid injection pipe (25) for precipitation and washing, the precipitated solid is collected on a precipitation filter plate, and a discharge gate (23) is opened for discharge, so that the washing solution is polysuccinimide solution;
step eight, injecting the washing filtrate obtained in the step seven into a vacuum dryer (14) through a third material sucking pump 13 for vacuum drying to obtain polysuccinimide with higher purity, sequentially injecting the polysuccinimide into a stirring tank 9 to obtain polysuccinimide with higher purity, and repeating the steps six-eight for 1-3 times to obtain polysuccinimide with high purity;
step nine, taking out polysuccinimide solid, adding the polysuccinimide solid into a stirring barrel (15) filled with deionized water, stirring to form suspension, then injecting 30% KOH solution, adjusting the pH value of the mixed solution to 9.0+/-0.5, hydrolyzing at the temperature of 40+/-2 ℃ for 30+/-5 min, and obtaining high-purity potassium polyaspartate solution;
the fan (4) sucks out hot air in the drying mechanism (3) and filters the hot air through the water filtering tank 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), the temperature of the stirring tank (9) is kept constant, the hot air in the stirring tank (9) enters the stirring tank heat-preserving cylinder (16) through the first hot air pipe (17), and the temperature of the stirring tank (15) is kept constant;
the air pump (11) pumps the steam generated during the drying of the vacuum dryer (14) into the collecting tank for condensation, then the steam is screened by the internal molecular sieve to form absolute ethyl alcohol and N, N-dimethylformamide, the absolute ethyl alcohol is stored in the liquid outlet tank, the liquid outlet pump pumps the absolute ethyl alcohol liquid in the liquid outlet tank, the absolute ethyl alcohol liquid is injected into the precipitating tank (19) through the liquid injection pipe (25) for precipitation and washing, and the N, N-dimethylformamide can be collected and purified for reuse;
and a conveyor is additionally arranged in the drying box, and the potassium polyaspartate solution is injected into the drying box for drying, so that the brown yellow potassium polyaspartate is obtained after the drying.
2. The application of the polyaspartic acid potassium prepared by the preparation method of the polyaspartic acid potassium in the plant growth promoter, which is characterized in that the polyaspartic acid potassium solution is sprayed on the soil where crops grow after being added with water, wherein the adding weight ratio is 0.1-10%, namely, the adding amount of the polyaspartic acid potassium solution in per 100g of clear water is 0.1-10 g.
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