CN104446795B - A kind of adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat - Google Patents

A kind of adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat Download PDF

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CN104446795B
CN104446795B CN201410713163.4A CN201410713163A CN104446795B CN 104446795 B CN104446795 B CN 104446795B CN 201410713163 A CN201410713163 A CN 201410713163A CN 104446795 B CN104446795 B CN 104446795B
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potassium
reaction
compound fertilizer
sulfate compound
consumption
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CN104446795A (en
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魏鑫
吴晓疆
焦志达
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JIANGSU GEOLOGY & MINERAL COMPOUND FERTILIZER FACTORY
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JIANGSU GEOLOGY & MINERAL COMPOUND FERTILIZER FACTORY
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B7/00Fertilisers based essentially on alkali or ammonium orthophosphates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/01Chlorine; Hydrogen chloride
    • C01B7/03Preparation from chlorides
    • C01B7/035Preparation of hydrogen chloride from chlorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/02Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Fertilizers (AREA)

Abstract

A kind of adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat, with potassium chloride and concentrated sulphuric acid direct reaction, extracting sulfuric acid hydrogen potassium, then dissolve and solution is sent to nitration mixture groove, mix with the MAP for dissolving, then the serosity for mixing and gas ammonia are carried out chemical reaction in the tubular reactor with the special charging aperture of ammonium bicarbonate soln, the ammonium bicarbonate soln for having prepared is injected into tubular reactor simultaneously, by adjusting the consumption of ammonium bicarbonate soln, to adjust the excessive heat of course of reaction generation to avoid because of overheated caused all technological problemses, through adding appropriate carbamide after reaction, drum granulating, dry, finally obtain nitrogenous, phosphorus, the potassium sulfate compound fertilizer of three element of potassium.Present invention process flow process advantages of simple, is avoided that the problems of excessive heat of tubular reactor, prevent because react overheated caused scab, pant and the technological problemses such as reactor vibration are had undesirable effect to normal production, reduce fault rate, improve production efficiency.

Description

A kind of adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat
Technical field
The present invention relates to a kind of composite heat transfer technology, the adjustable potassium sulfate compound fertilizer ammonification of particularly a kind of reaction heat Production technology.
Background technology
The ammonification production technology of current country's potassium sulfate compound fertilizer, capital equipment used is propylhomoserin tubular reactor, Reaction pressure and mixed effect, spray feed material, evaporation moisture are improved using the heat release of reaction, but reaction heat is excessively acutely easily produced Raw localized hyperthermia and violent turbulence, cause to scab, pant and the problems such as reactor vibrates.
Content of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, it is proposed that a kind of adjustable sulphuric acid of reaction heat Jia Xing compound fertilizer ammonification production technology.
The technical problem to be solved in the present invention is achieved through the following technical solutions, and a kind of proportioning is easy to adjust, produces Product shape and the adjustable potassium sulfate compound fertilizer ammonification production technology of superior in quality reaction heat, are characterized in:
(One)With potassium chloride and concentrated sulphuric acid direct reaction, both mol ratios are 1:1.01 ~ 1.20, reaction temperature be 90 ~ 120 DEG C, extracting sulfuric acid hydrogen potassium, while by desulfurization, cooling, absorbing and producing by-product hydrochloric acid;(Two)By step(One)Obtained sulfur Potassium hydrogen phthalate temperature is 40 ~ 100 DEG C of hot water dissolving, and the consumption of hot water is(One)1.6 ~ 2.0 times of middle potassium chloride, and by solution It is sent to nitration mixture groove;(Three)By the hot water dissolving that MAP temperature is 40 ~ 100 DEG C, the consumption of MAP is according to difference Adjusting, the consumption of hot water is 1.7 ~ 2.3 times of MAP to the needs of the composition of type products, is then delivered to nitration mixture groove, with (Two)In dissolved potassium hydrogen sulfate solution mixing;(Four)By step(Three)The serosity for mixing is with gas ammonia in tubular reactor Chemical reaction is inside carried out, while injecting the bicarbonate for having prepared into tubular reactor by the special charging aperture of ammonium bicarbonate soln Ammonium salt solution, according to the consumption that reaction condition controls ammonium bicarbonate soln immediately, adjusts the excessive heat of course of reaction generation, right The control method of ammonium bicarbonate soln consumption is that the initial flow of solution injection is set to step(Three)Gained mixed serum flow 0.1 times, monitoring tubular reactor temperature has simultaneously been noticed that whether asthma and improper vibration, if nothing, solution injection flow is subtracted For the 75% of initial value, still without then repeating to reduce until there is just above-mentioned bad phenomenon, if having asthma and improper vibration, will Solution injection flow increases to 1.25 times of initial value, still has, repeats to be increased up eliminating just above-mentioned bad phenomenon;(Five)Will Step(Four)Obtained product imports dashpot, then carries out drum granulating, drying, screening, finally obtains nitrogenous, phosphorus, potassium three The potassium sulfate compound fertilizer of element.
The technical problem to be solved in the present invention can also come further to realize by the following technical programs, step(Four)Described Ammonium bicarbonate soln of the ammonium bicarbonate soln for concentration saturation, it is room temperature ~ 80 DEG C which prepares temperature.
The technical problem to be solved in the present invention can also come further to realize by the following technical programs, step(Four)Described The consumption of gas ammonia is defined for 5 ~ 6 by final product pH value.
The technical problem to be solved in the present invention can also come further to realize by the following technical programs, step(Five)Middle general Step(Four)After obtained product imports dashpot, add carbamide carries out drum granulating, drying, sieve to supplement nitrogen component, then Point, finally obtain nitrogenous, phosphorus, the potassium sulfate compound fertilizer of three element of potassium.
Then present invention potassium chloride and concentrated sulphuric acid direct reaction, extracting sulfuric acid hydrogen potassium dissolve and solution are sent to nitration mixture Groove, is mixed with the MAP for dissolving, then by the serosity for mixing and gas ammonia with the special charging of ammonium bicarbonate soln Chemical reaction is carried out in the tubular reactor of mouth, while the ammonium bicarbonate soln for having prepared is injected into tubular reactor, is passed through The consumption of adjustment ammonium bicarbonate soln, adjusts the excessive heat of course of reaction generation avoiding asking because of overheated caused all technique Topic, through adding appropriate carbamide, drum granulating, drying after reaction, finally obtains nitrogenous, phosphorus, the potassium sulfate type of three element of potassium is combined Fertilizer.Present invention process flow process advantages of simple, is avoided that the problems of excessive heat of tubular reactor, prevents because reacting overheated caused knot The technological problemses such as scar, asthma and reactor vibration are had undesirable effect to normal production, reduce fault rate, improve production efficiency. With the potassium sulphate type ternary of this technique productions element compound fertilizer, nitrogen, phosphorus, the proportioning of three element of potassium are easy to adjust, shape of product and matter Amount is excellent, and by-product hydrochloric acid, good in economic efficiency.
Specific embodiment
A kind of adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat,(One)Directly anti-with concentrated sulphuric acid with potassium chloride Should, both mol ratios are 1:1.01 ~ 1.20, reaction temperature be 90 ~ 120 DEG C, extracting sulfuric acid hydrogen potassium, at the same by desulfurization, cooling, By-product hydrochloric acid is produced in absorption;(Two)By step(One)Obtained potassium acid sulfate temperature is 40 ~ 100 DEG C of hot water dissolving, hot The consumption of water is(One)1.6 ~ 2.0 times of middle potassium chloride, and solution is sent to nitration mixture groove;(Three)It is 40 by MAP temperature ~ 100 DEG C of hot water dissolving, the consumption of MAP be the needs of the composition according to dissimilar product adjusting, the use of hot water 1.7 ~ 2.3 times for MAP are measured, nitration mixture groove is then delivered to, with(Two)In dissolved potassium hydrogen sulfate solution mixing; (Four)By step(Three)The serosity for mixing carries out chemical reaction with gas ammonia in tubular reactor, while molten by ammonium hydrogen carbonate The special charging aperture of liquid injects the ammonium bicarbonate soln for having prepared into tubular reactor, controls immediately bicarbonate according to reaction condition The consumption of ammonium salt solution, adjusts the excessive heat of course of reaction generation, to the control method of ammonium bicarbonate soln consumption is The initial flow of solution injection is set to step(Three)0.1 times of gained mixed serum flow, monitoring tubular reactor temperature simultaneously note Whether have asthma and improper vibration, if nothing, by solution injection flow be kept to the 75% of initial value, still without then repeat reduce up to Just there is above-mentioned bad phenomenon, if having asthma and improper vibration, solution is injected flow and increases to 1.25 times of initial value, still Have, repeat to be increased up eliminating just above-mentioned bad phenomenon;(Five)By step(Four)Obtained product imports dashpot, then Drum granulating, drying, screening is carried out, nitrogenous, phosphorus, the potassium sulfate compound fertilizer of three element of potassium is finally obtained.
Principle is that ammonium hydrogen carbonate and acid serosity react and generate carbon dioxide and water, reaction heat release very little itself, And the carbon dioxide and water of generation is easy to remove in follow-up link, will not bring additional impurities into product, can play regulation ammonia Change the effect of exothermic heat of reaction, while not reducing the ammonium composition in product.
As the content of phosphorus composition in dissimilar product has different requirements, so step(Three)The consumption of middle MAP It is the needs of composition according to dissimilar product adjusting in good time.
Step(Four)Ammonium bicarbonate soln of the ammonium bicarbonate soln for concentration saturation, it is room temperature ~ 80 which prepares temperature ℃.It is advisable with room temperature, concentration is advisable with saturation, unsaturation also may be used.
Step(Four)The consumption of the gas ammonia is defined for 5 ~ 6 by final product pH value.
Step(Five)Middle by step(Four)After obtained product imports dashpot, add carbamide to supplement nitrogen component, then Drum granulating, drying, screening is carried out, nitrogenous, phosphorus, the potassium sulfate compound fertilizer of three element of potassium is finally obtained.According to dissimilar The component content of product is required, by the content for adding nitrogen component in actuator potassium sulfate compound fertilizer of carbamide.
The concrete technical scheme of the present invention described further below, further understands this in order to those skilled in the art Invention, but do not constitute the restriction to right of the present invention.
The first step:With potassium chloride and concentrated sulphuric acid direct reaction, 10 parts of potassium chloride, 13.4 parts of concentrated sulphuric acid, reaction temperature is 120 DEG C, extracting sulfuric acid hydrogen potassium, while by desulfurization, cooling, absorbing and producing by-product hydrochloric acid.
Second step:By 18 parts of dissolvings of hot water that potassium acid sulfate temperature obtained in the first step is 60 DEG C, and solution is sent to Nitration mixture groove.
3rd step:By 10.3 parts of MAP, 21 parts of dissolvings of the hot water that temperature is 60 DEG C, nitration mixture groove is then delivered to, with the The potassium hydrogen sulfate solution mixing that has been dissolved in two steps.
4th step:The serosity that 3rd step is mixed carries out chemical reaction with gas ammonia in tubular reactor, while passing through The special charging aperture of ammonium bicarbonate soln injects the ammonium bicarbonate soln for having prepared into tubular reactor, prepares ammonium bicarbonate soln Temperature be 30 DEG C, 10 parts of ammonium hydrogen carbonate, 45 parts of water, according to the consumption that reaction condition controls ammonium bicarbonate soln immediately, are adjusted The excessive heat that section course of reaction is produced, controls the consumption of gas ammonia to ensure the pH value of final product as 5 ~ 6, molten to ammonium hydrogen carbonate The control method of liquid consumption is 0.1 times that solution injects that initial flow is set to the 3rd step gained mixed serum flow, monitors Tubular reactor temperature has simultaneously been noticed that whether asthma and improper vibration, if nothing, solution injection flow is kept to initial value 75%, still without then repeating to reduce up to there is just above-mentioned bad phenomenon, if having asthma and improper vibration, by solution injection stream Amount increases to 1.25 times of initial value, still has, repeats to be increased up eliminating just above-mentioned bad phenomenon.
5th step:Product obtained in 4th step is imported dashpot, and adds 4.2 parts of carbamide to supplement nitrogen component, then Drum granulating, drying, screening is carried out, nitrogenous, phosphorus is finally obtained(In terms of phosphorus pentoxide), potassium(In terms of potassium oxide)Three elements are matched somebody with somebody Than for 17%:17%:17% potassium sulfate compound fertilizer.

Claims (4)

1. the adjustable potassium sulfate compound fertilizer ammonification production technology of a kind of reaction heat, it is characterised in that:
(One)With potassium chloride and concentrated sulphuric acid direct reaction, both mol ratios are 1:1.01 ~ 1.20, reaction temperature is 90 ~ 120 DEG C, extracting sulfuric acid hydrogen potassium, while by desulfurization, cooling, absorbing and producing by-product hydrochloric acid;
(Two)By step(One)Obtained potassium acid sulfate temperature is 40 ~ 100 DEG C of hot water dissolving, and the consumption of hot water is(One)In 1.6 ~ 2.0 times of potassium chloride, and solution is sent to nitration mixture groove;
(Three)By the hot water dissolving that MAP temperature is 40 ~ 100 DEG C, the consumption of MAP is according to dissimilar product Composition needs adjusting, the consumption of hot water is 1.7 ~ 2.3 times of MAP, is then delivered to nitration mixture groove, with(Two)In The potassium hydrogen sulfate solution mixing that has dissolved;
(Four)By step(Three)The serosity for mixing carries out chemical reaction with gas ammonia in tubular reactor, while passing through bicarbonate The special charging aperture of ammonium salt solution injects the ammonium bicarbonate soln for having prepared into tubular reactor, controls immediately carbon according to reaction condition The consumption of sour hydrogen ammonium salt solution, adjusts the excessive heat of course of reaction generation,
To the control method of ammonium bicarbonate soln consumption it is:The initial flow of solution injection is set to step(Three)Gained combined slurry flow 0.1 times of amount, monitoring tubular reactor temperature have simultaneously been noticed that whether asthma and improper vibration, if nothing, solution are injected flow The 75% of initial value is kept to, still without minimizing is then repeated until there is just above-mentioned bad phenomenon, if having asthma and improper vibration, Solution injection flow is increased to initial value 1.25 times, still have, repeat to be increased up eliminating just above-mentioned bad phenomenon;
(Five)By step(Four)Obtained product imports dashpot, then carries out drum granulating, drying, screening, is finally contained Nitrogen, phosphorus, the potassium sulfate compound fertilizer of three element of potassium.
2. the adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat according to claim 1, it is characterised in that:Step Suddenly(Four)Ammonium bicarbonate soln of the ammonium bicarbonate soln for concentration saturation, it is room temperature ~ 80 DEG C which prepares temperature.
3. the adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat according to claim 1, it is characterised in that:Step Suddenly(Four)The consumption of the gas ammonia is defined for 5 ~ 6 by final product pH value.
4. the adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat according to claim 1, it is characterised in that:Step Suddenly(Five)Middle by step(Four)After obtained product imports dashpot, interpolation carbamide carries out rotary drum to supplement nitrogen component, then and makes Grain, drying, screening, finally obtain nitrogenous, phosphorus, the potassium sulfate compound fertilizer of three element of potassium.
CN201410713163.4A 2014-12-02 2014-12-02 A kind of adjustable potassium sulfate compound fertilizer ammonification production technology of reaction heat Active CN104446795B (en)

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CN106673762A (en) * 2016-12-28 2017-05-17 郑州阿波罗肥业有限公司 Method for producing compound fertilizer from monoammonium phosphate hydrolysate
CN109608247A (en) * 2019-01-22 2019-04-12 盘锦冠桥复合肥科技服务有限公司 A kind of production method of novel ammonification S-based compound fertilizer

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JPH0684272B2 (en) * 1989-01-04 1994-10-26 多木化学株式会社 Tobacco fertilizer
CN1035725C (en) * 1993-04-19 1997-08-27 山东省临沂市化工总厂 Method for prodn. of potassium sulphate type ternary composite fertilizer
CN1180047A (en) * 1997-07-25 1998-04-29 樊彩梅 Preparation method of lemery salt and ternary compound fertilizer containing nitrogen, phosphorus and potassium
CN1280967A (en) * 2000-08-29 2001-01-24 陈爱中 Process for preparing powdered composite potassium sulfate fertilizer
CN100475744C (en) * 2007-05-22 2009-04-08 河北梅花味精集团有限公司 Method for producing agricultural fertilizer by using waste liquid of monosodium glutamate

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