CN104446795A - Process for ammoniation production of potassium sulfate type compound fertilizer with adjustable reaction heat - Google Patents
Process for ammoniation production of potassium sulfate type compound fertilizer with adjustable reaction heat Download PDFInfo
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- CN104446795A CN104446795A CN201410713163.4A CN201410713163A CN104446795A CN 104446795 A CN104446795 A CN 104446795A CN 201410713163 A CN201410713163 A CN 201410713163A CN 104446795 A CN104446795 A CN 104446795A
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- potassium
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- compound fertilizer
- potassium sulfate
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
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- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a process for ammoniation production of a potassium sulfate type compound fertilizer with adjustable reaction heat. The process comprises the following steps: taking potassium chloride to directly react with concentrated sulfuric acid so as to prepare potassium hydrogen sulfate; then dissolving potassium hydrogen sulfate, and delivering the solution to an acid mixing tank to mix with dissolved mono-ammonium phosphate; performing chemical reaction between mixed slurry and gas ammonia in a tubular reactor with a special feed opening of an ammonium hydrogen carbonate solution, injecting the prepared ammonium hydrogen carbonate solution into the tubular reactor at the same time, and adjusting excess heat generated in a reaction process by adjusting the used amount of the ammonium hydrogen carbonate solution so as to avoid process problems caused by overheating; adding an appropriate amount of urea after reaction, and performing drum granulation, and drying to finally obtain the potassium sulfate type compound fertilizer containing nitrogen, phosphorus and potassium. By adopting the process disclosed by the invention, the process flow is simple and reasonable, the overheating problem of the tubular reactor can be avoided, adverse effects of process problems including scabbing, breathing, reactor vibration and the like caused by overheating on regular production are prevented, the fault rate is reduced, and the production efficiency is improved.
Description
Technical field
The present invention relates to the potassium sulfate compound fertilizer ammonification production technique that a kind of composite heat transfer technology, particularly a kind of reaction heat are adjustable.
Background technology
The ammonification production technique of current domestic potassium sulfate compound fertilizer, major equipment used is propylhomoserin tubular reactor, the heat release of reaction is utilized to improve reaction pressure and mixed effect, spray feed material, transpiring moisture, but reaction heat is too violent easily produces localized hyperthermia and violent turbulence, cause scabbing, pant and the problem such as reactor vibration.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, proposes the potassium sulfate compound fertilizer ammonification production technique that a kind of reaction heat is adjustable.
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 the adjustable potassium sulfate compound fertilizer ammonification production technique of adjustment, shape of product and superior in quality reaction heat, is characterized in:
(1) with Repone K and vitriol oil direct reaction, both mol ratios are 1:1.01 ~ 1.20, and temperature of reaction is 90 ~ 120 DEG C, extracting sulfuric acid hydrogen potassium, produce by-product hydrochloric acid by desulfurization, cooling, absorption simultaneously, (2) by sal enixum temperature obtained for step () be the hot water dissolving of 40 ~ 100 DEG C, the consumption of hot water be 1.6 ~ 2.0 times of (one) middle Repone K, and solution is delivered to nitration mixture groove, (3) by monoammonium phosphate temperature be the hot water dissolving of 40 ~ 100 DEG C, the consumption of monoammonium phosphate adjusts according to the needs of the composition of dissimilar product, the consumption of hot water is 1.7 ~ 2.3 times of monoammonium phosphate, then delivers to nitration mixture groove, mixes with the potassium hydrogen sulfate solution dissolved in (two), (4) slurries step (three) mixed and gas ammonia carry out chemical reaction in tubular reactor, in tubular reactor, inject by the special opening for feed of ammonium bicarbonate soln the ammonium bicarbonate soln prepared simultaneously, immediately the consumption of ammonium bicarbonate soln is controlled according to reaction condition, the excessive heat regulating reaction process to produce, to the control method of ammonium bicarbonate soln consumption being---solution injects 0.1 times that initial flow is set to step (three) gained mixed serum flow, monitoring tubular type temperature of reactor also notes whether having asthma and improper vibration, if nothing, solution is injected flow is kept to initial value 75%, still without then repeating to reduce until just there is above-mentioned bad phenomenon, if have asthma and improper vibration, solution is injected 1.25 times that flow increases to initial value, still have, repeat to increase until just eliminate above-mentioned bad phenomenon, (5) product obtained for step (four) is imported dashpot, then carry out drum granulating, oven dry, screening, finally obtain nitrogenous, phosphorus, potassium element potassium sulfate compound fertilizer.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, and step (four) described ammonium bicarbonate soln is the ammonium bicarbonate soln that concentration is saturated, and its preparation temperature is room temperature ~ 80 DEG C.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, and the consumption of step (four) described gas ammonia is 5 ~ 6 to be as the criterion with final product pH value.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, after product obtained for step (four) being imported dashpot in step (five), add urea with supplementary nitrogen component, then carry out drum granulating, oven dry, screening, finally obtain nitrogenous, phosphorus, potassium element potassium sulfate compound fertilizer.
The present invention's Repone K and vitriol oil direct reaction, extracting sulfuric acid hydrogen potassium, then dissolve and solution is delivered to nitration mixture groove, mix with the monoammonium phosphate dissolved, then the slurries mixed and gas ammonia are carried out chemical reaction in the tubular reactor with the special opening for feed of ammonium bicarbonate soln, in tubular reactor, inject the ammonium bicarbonate soln prepared simultaneously, by adjusting the consumption of ammonium bicarbonate soln, the excessive heat regulating reaction process to produce is to avoid because of the overheated all technological problemses caused, through adding appropriate urea after reaction, drum granulating, dry, finally obtain nitrogenous, phosphorus, the potassium sulfate compound fertilizer of potassium element.Present invention process flow process advantages of simple, can avoid the problems of excessive heat of tubular reactor, and what prevent from causing because of reacted thermal conductance scabs, to pant and the technological problems such as reactor vibration causes detrimentally affect to normal production, reduces failure rate, enhances productivity.With the potassium sulphate type ternary of this explained hereafter element composite fertilizer, the proportioning of nitrogen, phosphorus, potassium element is easy to adjustment, shape of product and superior in quality, and by-product hydrochloric acid, good in economic efficiency.
Embodiment
The potassium sulfate compound fertilizer ammonification production technique that a kind of reaction heat is adjustable, (1) with Repone K and vitriol oil direct reaction, both mol ratios are 1:1.01 ~ 1.20, and temperature of reaction is 90 ~ 120 DEG C, extracting sulfuric acid hydrogen potassium, produces by-product hydrochloric acid by desulfurization, cooling, absorption simultaneously, (2) by sal enixum temperature obtained for step () be the hot water dissolving of 40 ~ 100 DEG C, the consumption of hot water be 1.6 ~ 2.0 times of (one) middle Repone K, and solution is delivered to nitration mixture groove, (3) by monoammonium phosphate temperature be the hot water dissolving of 40 ~ 100 DEG C, the consumption of monoammonium phosphate adjusts according to the needs of the composition of dissimilar product, the consumption of hot water is 1.7 ~ 2.3 times of monoammonium phosphate, then delivers to nitration mixture groove, mixes with the potassium hydrogen sulfate solution dissolved in (two), (4) slurries step (three) mixed and gas ammonia carry out chemical reaction in tubular reactor, in tubular reactor, inject by the special opening for feed of ammonium bicarbonate soln the ammonium bicarbonate soln prepared simultaneously, immediately the consumption of ammonium bicarbonate soln is controlled according to reaction condition, the excessive heat regulating reaction process to produce, to the control method of ammonium bicarbonate soln consumption being---solution injects 0.1 times that initial flow is set to step (three) gained mixed serum flow, monitoring tubular type temperature of reactor also notes whether having asthma and improper vibration, if nothing, solution is injected flow is kept to initial value 75%, still without then repeating to reduce until just there is above-mentioned bad phenomenon, if have asthma and improper vibration, solution is injected 1.25 times that flow increases to initial value, still have, repeat to increase until just eliminate above-mentioned bad phenomenon, (5) product obtained for step (four) is imported dashpot, then carry out drum granulating, oven dry, screening, finally obtain nitrogenous, phosphorus, potassium element potassium sulfate compound fertilizer.
Principle is that bicarbonate of ammonia and acid slurries react and generate carbonic acid gas and water, the heat release of this reaction own is very little, and the carbonic acid gas generated and water are easy to remove in follow-up link, additional impurities can not be brought into product, the effect regulating aminating reaction heat release can be played, do not reduce the ammonium composition in product simultaneously.
Because in dissimilar product, the content of phosphorus composition has different requirement, so the consumption of monoammonium phosphate adjusts according to the needs of the composition of dissimilar product in step (three) in good time.
Step (four) described ammonium bicarbonate soln is the ammonium bicarbonate soln that concentration is saturated, and its preparation temperature is room temperature ~ 80 DEG C.Be advisable with room temperature, concentration is advisable with saturated, unsaturatedly also can.
The consumption of step (four) described gas ammonia is 5 ~ 6 to be as the criterion with final product pH value.
After product obtained for step (four) being imported dashpot in step (five), add urea with supplementary nitrogen component, then carry out drum granulating, oven dry, screening, finally obtain nitrogenous, phosphorus, potassium element potassium sulfate compound fertilizer.According to the component content requirement of dissimilar product, by the content of nitrogen component in the interpolation setter potassium sulfate compound fertilizer of urea.
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, but do not form the restriction to right of the present invention.
The first step: with Repone K and vitriol oil direct reaction, 10 parts, Repone K, the vitriol oil 13.4 parts, temperature of reaction is 120 DEG C, extracting sulfuric acid hydrogen potassium, produces by-product hydrochloric acid by desulfurization, cooling, absorption simultaneously.
Second step: the sal enixum temperature the first step obtained is the hot water 18 parts dissolving of 60 DEG C, and solution is delivered to nitration mixture groove.
3rd step: the hot water 21 parts dissolving by monoammonium phosphate 10.3 parts by temperature being 60 DEG C, then delivers to nitration mixture groove, mixes with the potassium hydrogen sulfate solution dissolved in second step.
4th step: the slurries mix the 3rd step and gas ammonia carry out chemical reaction in tubular reactor, in tubular reactor, inject by the special opening for feed of ammonium bicarbonate soln the ammonium bicarbonate soln prepared simultaneously, the temperature of preparation ammonium bicarbonate soln is 30 DEG C, 10 parts, bicarbonate of ammonia, 45 parts, water, immediately the consumption of ammonium bicarbonate soln is controlled according to reaction condition, the excessive heat regulating reaction process to produce, control the consumption of gas ammonia to ensure that the pH value of final product is for 5 ~ 6, to the control method of ammonium bicarbonate soln consumption being---solution injects 0.1 times that initial flow is set to the 3rd step gained mixed serum flow, monitoring tubular type temperature of reactor also notes whether having asthma and improper vibration, if nothing, solution is injected flow is kept to initial value 75%, still without then repeating to reduce until just there is above-mentioned bad phenomenon, if have asthma and improper vibration, solution is injected 1.25 times that flow increases to initial value, still have, repeat to increase until just eliminate above-mentioned bad phenomenon.
5th step: product obtained for the 4th step is imported dashpot, and add 4.2 parts, urea with supplementary nitrogen component, then carry out drum granulating, oven dry, screening, finally obtaining nitrogenous, phosphorus (in Vanadium Pentoxide in FLAKES), potassium (in potassium oxide) element proportioning is the potassium sulfate compound fertilizer of 17%:17%:17%.
Claims (4)
1. the potassium sulfate compound fertilizer ammonification production technique that reaction heat is adjustable, is characterized in that:
(1) with Repone K and vitriol oil direct reaction, both mol ratios are 1:1.01 ~ 1.20, and temperature of reaction is 90 ~ 120 DEG C, extracting sulfuric acid hydrogen potassium, produce by-product hydrochloric acid by desulfurization, cooling, absorption simultaneously;
(2) by sal enixum temperature obtained for step () be the hot water dissolving of 40 ~ 100 DEG C, the consumption of hot water be 1.6 ~ 2.0 times of (one) middle Repone K, and solution is delivered to nitration mixture groove;
(3) by monoammonium phosphate temperature be the hot water dissolving of 40 ~ 100 DEG C, the consumption of monoammonium phosphate adjusts according to the needs of the composition of dissimilar product, the consumption of hot water is 1.7 ~ 2.3 times of monoammonium phosphate, then delivers to nitration mixture groove, mixes with the potassium hydrogen sulfate solution dissolved in (two);
(4) slurries step (three) mixed and gas ammonia carry out chemical reaction in tubular reactor, in tubular reactor, inject by the special opening for feed of ammonium bicarbonate soln the ammonium bicarbonate soln prepared simultaneously, immediately the consumption of ammonium bicarbonate soln is controlled according to reaction condition, the excessive heat regulating reaction process to produce
To the control method of ammonium bicarbonate soln consumption be: solution injects 0.1 times that initial flow is set to step (three) gained mixed serum flow, monitoring tubular type temperature of reactor also notes whether having asthma and improper vibration, if nothing, solution is injected flow is kept to initial value 75%, still without then repeating to reduce until just there is above-mentioned bad phenomenon, if have asthma and improper vibration, solution is injected 1.25 times that flow increases to initial value, still have, repeat to increase until just eliminate above-mentioned bad phenomenon;
(5) product obtained for step (four) is imported dashpot, then carry out drum granulating, oven dry, screening, finally obtain nitrogenous, phosphorus, potassium element potassium sulfate compound fertilizer.
2. the potassium sulfate compound fertilizer ammonification production technique that reaction heat according to claim 1 is adjustable, is characterized in that: step (four) described ammonium bicarbonate soln is the ammonium bicarbonate soln that concentration is saturated, and its preparation temperature is room temperature ~ 80 DEG C.
3. the potassium sulfate compound fertilizer ammonification production technique that reaction heat according to claim 1 is adjustable, is characterized in that: the consumption of step (four) described gas ammonia is 5 ~ 6 to be as the criterion with final product pH value.
4. the potassium sulfate compound fertilizer ammonification production technique that reaction heat according to claim 1 is adjustable, it is characterized in that: after product obtained for step (four) being imported dashpot in step (five), add urea with supplementary nitrogen component, then carry out drum granulating, oven dry, screening, finally obtain nitrogenous, phosphorus, potassium element potassium sulfate compound fertilizer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (5)
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| JPH02180781A (en) * | 1989-01-04 | 1990-07-13 | Taki Chem Co Ltd | Fertilizer for tobacco |
| CN1078226A (en) * | 1993-04-19 | 1993-11-10 | 山东省临沂市化工总厂 | The production method 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 |
| CN101037353A (en) * | 2007-05-22 | 2007-09-19 | 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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2014
- 2014-12-02 CN CN201410713163.4A patent/CN104446795B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02180781A (en) * | 1989-01-04 | 1990-07-13 | Taki Chem Co Ltd | Fertilizer for tobacco |
| CN1078226A (en) * | 1993-04-19 | 1993-11-10 | 山东省临沂市化工总厂 | The production method 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 |
| CN101037353A (en) * | 2007-05-22 | 2007-09-19 | 河北梅花味精集团有限公司 | Method for producing agricultural fertilizer by using waste liquid of monosodium glutamate |
Non-Patent Citations (1)
| Title |
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| 叶树滋: "碳酸氢铵稀酸法生产硫酸钾技术的回顾与设想", 《硫磷设计与粉体工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN104446795B (en) | 2017-03-15 |
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