CN101941709A - Microwave preparation process of poly-potassium borate - Google Patents

Microwave preparation process of poly-potassium borate Download PDF

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Publication number
CN101941709A
CN101941709A CN 201010222780 CN201010222780A CN101941709A CN 101941709 A CN101941709 A CN 101941709A CN 201010222780 CN201010222780 CN 201010222780 CN 201010222780 A CN201010222780 A CN 201010222780A CN 101941709 A CN101941709 A CN 101941709A
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China
Prior art keywords
poly
microwave
potassium borate
boric acid
potassium
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Pending
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CN 201010222780
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Chinese (zh)
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汪鹤亭
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JIANGXI LVYUE BIOENGINEERING CO Ltd
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JIANGXI LVYUE BIOENGINEERING CO Ltd
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Priority to CN 201010222780 priority Critical patent/CN101941709A/en
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Abstract

The invention discloses a microwave preparation process of poly-potassium borate, comprising the following three steps: adding water to dissolve the raw material boric acid and potassium hydroxide into mixed liquor; carrying out microwave polymerization and simultaneously carrying out dehydration; and immediately carrying out microwave treatment or storing and cooling on the mixture formed by first-step reaction to form a solid material and then carrying out microwave treatment on the solid material. The frequency adopted during microwave treatment is 2450MHz. During first-step reaction, the water is firstly heated to 40-60 DEG C, then specific parts of KOH by weight is thrown according to the requirement of the final product and finally specific parts of boric acid by weight is slowly added after stirring and dissolving. The heating temperature ranges from 40 DEG C to 116 DEG C during first-step dissolution reaction. The process saves energy, can greatly lower the cost and make contributions to energy saving and emission reduction and environmental protection, is simple, has controllable and easily-controlled main parameters and ensures yield and quality. The process can adjust the formula according to the requirement of the crops for K2O or B and ensure the product to have wider adaptability.

Description

The microwave preparation technology of poly-potassium borate
Technical field
The present invention relates to a kind of technology of preparing of chemical fertilizer, particularly relate to a kind of microwave preparation new technology of poly-potassium borate.
Background technology
Knop in 1859 and Sachs adopt the water culture plant to confirm that potassium is one of essential element of plant-growth.To the analytical test of plant ashes, find K 2It is very high that O accounts for ash rate, proves that potassium is the required main macroelement of plant.Modern study shows, K +Can activate the activity of plurality of enzymes, can promote photosynthesis, can accelerate carbohydrate running and starch and accumulate, can help protein synthesis, can help crop resistance of adverse circumstance (drought, disease and pest, cold etc.) or the like.
Boron is found laterly to the effect of growth and development of plants, is that nineteen thirty-nine Arnon and Stout confirm by experiment.They are classified as boron one of essential trace element of plant.A large amount of field tests had been carried out to boron fertilizer in beginning China various places in 1980, after the crop on the boron deficient soil (cotton, rape, barley and wheat, paddy rice, corn, soybean etc.) is used boron fertilizer, obtained very significantly volume increase (stimulation ratio is generally 20~60%) effect.Wherein the rape on farm, Lishui of Zhejiang county is executed boron (B) back even is increased production 584.6~1044.1%, and it is important to illustrate that boron fertilizer acts on agricultural.
Existing boron fertilizer mainly is boric acid, borax, boron magnesium-phosphorus fertilizer, poly-Sodium Tetraborate etc.What wherein have is poorly soluble, and what have contains sodium, and sodium is plant does not need, also deleterious element when concentration is high.The poly-potassium borate of recent development is then different, and its master contains potassium and boron, all be that plant is necessary, and its solvability is very good.Abroad potassium borate supply the markets gather in (U.S.) existing eight.The publication number that China Gazette of Patent for Invention 2009.07.29 announces is that a kind of potassium decaborate fertilizer and preparation method thereof has been reported in the application for a patent for invention of CN101492311, this method main technique had two steps: the first step, boric acid and potassium hydroxide or other sylvite (adding water) dissolving and high temperature polymerization.Second step, the spray-dried crystalline product that granulates of polymers soln.Need the energy (heating) by above-mentioned technology the first step material dissolution and high temperature polymerization, estimate product power consumption 200 kilowatt-hours per ton, be roughly equal to 150 yuan of Renminbi by the market electricity price.In second step, spraying drying product per ton adopts oil hot air furnace by removing 1.6 tons of calculating of moisture total amount, needs to consume about diesel oil 470kg, is roughly equal to 3200 yuan of Renminbi, about 3350 yuan of total energy consumption expense by existing market price.Energy consumption is greatly the weak point of above-mentioned patent technology.
Summary of the invention
The objective of the invention is to: propose to adopt the also poly-potassium borate of the technological line of dehydration preparation simultaneously of microwave polymerization, to reduce the energy consumption in the poly-potassium borate production.
The microwave preparation technology of the poly-potassium borate that the present invention proposes comprises following three steps:
The first step: raw material boric acid is dissolved in water into mixed solution with potassium hydroxide.This step also need heat, and electric energy consumption is amounted to about 113 yuan of Renminbi with about 150 kilowatt-hours of product per ton.
Second step: microwave polymerization and dehydration simultaneously.Product per ton about 560kg that need dewater consumes about 934 kilowatt-hours of electric energy, amounts to about 700 yuan of Renminbi.
The 3rd step: product is pulverized, and product power consumption 15 kilowatt-hours per ton are roughly equal to 11.3 yuan of Renminbi.More than about 825 yuan of three step total energy consumption expenses.
The mixture that the first step reaction of the present invention forms enters microwave treatment immediately or deposits and carry out microwave treatment again after cooling forms solids.
The frequency that adopts during microwave treatment of the present invention is 2450MHZ.
Water was heated to 40-60 ℃ earlier when the first step of the present invention was reacted, and pressed the weight part of the required input of the finished product KOH regulation again, after the stirring and dissolving, slowly added the weight part of boric acid regulation again.The Heating temperature scope is 40 ℃ to 116 ℃ during the first step solubilizing reaction.
Raw material is by weight boric acid in the first step of the present invention: potassium hydroxide is 1: 0.56 or 1: 0.28 or 1: 0.374.
Technology of the present invention has characteristics:
1, energy-conservation, can reduce cost greatly, also can be energy-saving and emission-reduction, protect environment to make contributions.Poly-potassium borate is that high energy carries product, and energy consumption cost accounts for the cost large percentage, so energy efficient is the main path that reduces production costs.The present invention compares with 200910116215.9 patents, can save energy consumption cost about 75%.
2, K 2O and the B component proportions in product is adjustable.Therefore can be according to farm crop to K 2The demand of O or B is regulated prescription, makes product have adaptability widely.
3, technology of the present invention is simple, controlled, the easy control of main technologic parameters, and output and quality is guaranteed.
Embodiment
The present invention is described in detail below in conjunction with implementing.
The microwave preparation of 1: four poly-potassium borate of embodiment:
2KOH+4H 3BO 3→K 2B 4O 7+7H 2O
Add water 16 weight parts in the reactor, be heated to 50 ℃, drop into KOH 14 weight parts, after the stirring and dissolving, slowly add boric acid 25 weight parts again, stir, heat 50-116 ℃ until dissolving fully.About 0.5 hour of this process, evaporable moisture need not to replenish therebetween.
The bigger mixture of viscosity that reaction forms can enter microwave treatment immediately, also can deposit cooling formation solids and enter microwave treatment again.Microwave treatment adopts 2450MHz, and high firepower was finished in 6 minutes.Handicraft product cooling pulverizing.
Product is about 65% to the raw material yield, is anhydrous K 2B 4O 7, wherein contain K 2O 〉=45%, B 〉=17%, moisture content≤3%.
The microwave preparation of 2: eight poly-potassium borates of embodiment:
2KOH+8H 3BO 3→K 2B 8O 13+13H 2O
Add water 26 weight parts in the reactor, be heated to 40 ℃, drop into the KOH14 weight part, after the stirring and dissolving, slowly add boric acid 50 weight parts again, stir, continue to heat 40-110 ℃ until dissolving fully.About 1.2 hours of this process, evaporable moisture need not to replenish therebetween.
The bigger mixture of viscosity that reaction forms can enter microwave treatment immediately, also can deposit cooling formation solids and enter microwave treatment again.Microwave treatment adopts 2450MHz, and high firepower was finished in 6 minutes.Handicraft product cooling pulverizing.
Product is about 66.3% to the raw material yield, is anhydrous K 2B 8O 13, wherein contain K 2O 〉=26%, B 〉=20%, moisture content≤3%.
Embodiment: the microwave preparation of mixing poly-potassium borate
Add water 20 weight parts in the reactor, be heated to 60 ℃, drop into the KOH18.7 weight part, after the stirring and dissolving, slowly add boric acid 50 weight parts again, stir, continue to be heated to 40-110 ℃ of directly dissolving fully.About 1 hour of this process, evaporable moisture need not to replenish therebetween.
Press the polymerization of mode microwave, dehydration, cooling, the pulverizing of embodiment 1, embodiment 2, get approximately each mixture of 50% of four poly-potassium borates and eight poly-potassium borates.
Product is about 66% to the raw material yield, is anhydrous K 2B 4O 7And K 2B 8O 13Mixture wherein contains K 2O 〉=31%, B 〉=18%, moisture content≤3%.
Above-mentioned three example products, the result of use on agricultural (physiologic effect of K and B) all is similar, just K 2O content difference is bigger, can need K to need the situation decision of B to adopt which kind of product to be advisable according to crop.
Energy consumption cost of the present invention only be patent 200910116215.9 the spraying drying energy consumption cost about 25%, saved 75% energy consumption.It is as follows that we analyze the reason that energy consumption significantly reduces: the first step in the poly-potassium borate preparation, after being mixing and water adding dissolving boric acid and potassium hydroxide, when the higher solution surface of formation viscosity is heated dehydration, easily form the film that compacts, this film can stop that internal moisture distributes, and causes hot dewatering efficiency to descend.Therefore need consume more heat energy during spraying drying.
And microwave drying is different with the thermal conduction of traditional heating exsiccant, and microwave is a kind of higher frequency electromagnetic field, the tool penetrance.When microwave action during in reaction mixture, can make whole mixture, the molecular polarization that comprises mixture inside, and make polar molecule do commutation campaign, friction, the collision of per second 24.5 hundred million times, promoted the polymerization ofathe reactants reaction so on the one hand, produce high heat on the other hand, make the rapid loss of moisture (moisture that comprises reactant inside) in the reactant.

Claims (6)

1. the microwave preparation technology of a poly-potassium borate is characterized in that: may further comprise the steps:
The first step: raw material boric acid is dissolved in water into mixed solution with potassium hydroxide;
Second step: microwave polymerization and dehydration simultaneously;
The 3rd step: product is pulverized.
2. the microwave preparation technology of poly-potassium borate according to claim 1 is characterized in that: the mixture that the first step reaction forms enters microwave treatment immediately or deposits and carry out microwave treatment again after cooling forms solids.
3. the microwave preparation technology of poly-potassium borate according to claim 2, it is characterized in that: the frequency that adopts during microwave treatment is 2450MHZ.
4. the microwave preparation technology of poly-potassium borate according to claim 1 and 2, it is characterized in that: water is heated to 40-60 ℃ earlier during the first step reaction, press the weight part of the required input of the finished product KOH regulation again, after the stirring and dissolving, slowly add the weight part of boric acid regulation again.
5. the microwave preparation technology of poly-potassium borate according to claim 1 and 2, it is characterized in that: the Heating temperature scope is 40 ℃ to 116 ℃ during the first step solubilizing reaction.
6. the microwave preparation technology of poly-potassium borate according to claim 1 and 2 is characterized in that: raw material is by weight boric acid in the first step: potassium hydroxide is 1: 0.56 or 1: 0.28 or 1: 0.374.
CN 201010222780 2010-07-09 2010-07-09 Microwave preparation process of poly-potassium borate Pending CN101941709A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102153375A (en) * 2011-04-22 2011-08-17 淮阴师范学院 Boron-potassium binary foliar fertilizer
WO2017030978A1 (en) * 2015-08-14 2017-02-23 U.S. Borax Inc. Potassium magnesium borate use for delayed release of borate and methods of manufacturing the same
CN111747776A (en) * 2020-06-04 2020-10-09 普罗丰禾(武汉)科技有限公司 Polymeric full-water-soluble fertilizer, preparation method and application thereof, and preparation method of boron potassium polyphosphate compound
CN112457095A (en) * 2020-10-09 2021-03-09 王平 Slow-release organic fertilizer and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2094881A (en) * 1935-10-18 1937-10-05 American Potash & Chem Corp Method of preparing potassium pentaborate
CN101020690A (en) * 2007-03-21 2007-08-22 北京科技大学 Microwave process of synthesizing lithium dioxalate borate
CN101054180A (en) * 2007-04-09 2007-10-17 沈阳化工学院 Method of coproducing anhydrous potassium pentaborate by boric acid factory self-producing boric acid
CN101492311A (en) * 2009-02-19 2009-07-29 安徽省农望农业科技开发有限公司 Potassium decaborate fertilizer and method for producing the same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2094881A (en) * 1935-10-18 1937-10-05 American Potash & Chem Corp Method of preparing potassium pentaborate
CN101020690A (en) * 2007-03-21 2007-08-22 北京科技大学 Microwave process of synthesizing lithium dioxalate borate
CN101054180A (en) * 2007-04-09 2007-10-17 沈阳化工学院 Method of coproducing anhydrous potassium pentaborate by boric acid factory self-producing boric acid
CN101492311A (en) * 2009-02-19 2009-07-29 安徽省农望农业科技开发有限公司 Potassium decaborate fertilizer and method for producing the same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《农机化研究》 20070131 杨旭等 微波干燥设备的性能特点及其市场前景分析 41-42 1-6 , 第1期 2 *
《化工进展》 20051231 杨刚等 五硼酸钾制备方法的对比 1011-1014 1-6 第24卷, 第9期 2 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102153375A (en) * 2011-04-22 2011-08-17 淮阴师范学院 Boron-potassium binary foliar fertilizer
CN102153375B (en) * 2011-04-22 2013-05-22 淮阴师范学院 Boron-potassium binary foliar fertilizer
WO2017030978A1 (en) * 2015-08-14 2017-02-23 U.S. Borax Inc. Potassium magnesium borate use for delayed release of borate and methods of manufacturing the same
CN111747776A (en) * 2020-06-04 2020-10-09 普罗丰禾(武汉)科技有限公司 Polymeric full-water-soluble fertilizer, preparation method and application thereof, and preparation method of boron potassium polyphosphate compound
CN112457095A (en) * 2020-10-09 2021-03-09 王平 Slow-release organic fertilizer and preparation method thereof

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Application publication date: 20110112