CN101817706A - Production method for potassium sulfate compound fertilizer - Google Patents
Production method for potassium sulfate compound fertilizer Download PDFInfo
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- CN101817706A CN101817706A CN200910231262A CN200910231262A CN101817706A CN 101817706 A CN101817706 A CN 101817706A CN 200910231262 A CN200910231262 A CN 200910231262A CN 200910231262 A CN200910231262 A CN 200910231262A CN 101817706 A CN101817706 A CN 101817706A
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- production method
- nitration mixture
- potassium sulfate
- compound fertilizer
- ammonia
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Abstract
The invention relates to a production method for a potassium sulfate compound fertilizer, which comprises the steps of: performing neutralization reaction on 10 to 10 mass percent ammonia water first, ammonia then and phosphorus-containing mixed acid until the neutralization degree of the ammonia and phosphoric acid in the mixed acid is between 1.10 and 1.30; and then performing granulation. In the production method, the density of the neutralized slurry is easy to adjust, the appearance quality of the compound fertilizer is improved, and simultaneously, the production method has the advantage of simple process operation and great reduction of the cost.
Description
Technical field
The present invention relates to a kind of production method of composite fertilizer, belong to fertilizer manufacturing technology field.
Background technology
Well-known chemosynthesis spray granulating composite fertilizer traditional technology production method, be utilize nitration mixture and purified gas ammonia in neutralizing well or the tubular reactor internal reaction generate slip, further production composite fertilizer, and gas ammonia is owing to be not easy to transportation and storage, all transport and store in liquid mode, when changing into gas ammonia and nitration mixture reaction, liquefied ammonia need absorb a large amount of steam, and ammoniacal liquor not only transports and storage is convenient to liquefied ammonia, and fecund is born in the byproduct of some Production in Chemical Plant, with low cost, easily obtain.
Useful high density ammoniacal liquor replacement ammonia gas react of prior art or high density ammoniacal liquor and ammonia make simultaneously and are used for neutralizing, and regulate not too easily with the rare denseness of slip in this kind technology, cause and produce instability, influence quality product.
Summary of the invention
The production method that the objective of the invention is to overcome above-mentioned deficiency and a kind of potassium sulfate compound fertilizer is provided, this kind method adopt intermediate concentration ammoniacal liquor again with ammonia and the preparation of phosphorous nitration mixture neutralization reaction earlier, and technological operation is simple, cost is low.
The technical scheme that the present invention takes is:
A kind of production method of potassium sulfate compound fertilizer may further comprise the steps:
(1) vitriol oil and Repone K are generated the solution of sulfur-bearing potassium hydrogen phthalate and excess sulfuric acid at the conversion tank internal reaction, add again phosphoric acid mixed nitration mixture;
(2) ammoniacal liquor that adds mass concentration 10%-18% in nitration mixture carries out the pre-neutralization reaction;
(3) with nitration mixture after the pre-neutralization and the further neutralization reaction of gas ammonia, to the degree of neutralization of the phosphoric acid of ammonia and nitration mixture be 1.10～1.30;
(4) spray granulating.
Described vitriol oil mass concentration is 98%, and phosphoric acid quality concentration is 20%.
The material proportion 1t of described Repone K, the vitriol oil, phosphoric acid: 0.4-1.4m
3: 3.0-5.0m
3
The described former nitration mixture proportion that adds behind the mass concentration 10%-18% ammoniacal liquor: 1.38-1.45g/ml.
In order to improve the efficient of pre-neutralization reaction, make the alternative ammonia of ammoniacal liquor energy maximum, described ammoniacal liquor preferred mass concentration is 12%, the preferred 1t of the material proportion of Repone K, the vitriol oil, phosphoric acid: 0.9m
3: 3.5m
3Add the preferred 1.4g/ml of former nitration mixture proportion behind the ammoniacal liquor; After step (3) reaction, the degree of neutralization of ammonia and nitration mixture preferred 1.15.
Beneficial effect of the present invention:
(1) the present invention closes nitration mixture with intermediate concentration ammoniacal liquor in pre-earlier, again with gas ammonia further in and nitration mixture, can reach and use in the gas ammonia fully and the effect of nitration mixture, and in and the rare consistency ratio of slip be easier to regulate, composite fertilizer's output can not have any impact.
(2) improved the visual appearance of composite fertilizer, strengthened the homogeneity of material proportion, it is good to show compound fertilizer granules smooth finish, and granularity is round, and whiteness promotes to some extent, and inner quality is nitrogenous on the rise.
(3) in the nitration mixture jar, add ammoniacal liquor, avoided utilizing the drawback of gas ammonia and the volatile loss of nitration mixture reaction gas ammonia, reduced resource loss, improved resource utilization,, saved fund by replace liquefied ammonia production composite fertilizer with partial ammonia water, reduced cost, and technological operation is simple.
Embodiment
Embodiment 1
A kind of production method of potassium sulfate compound fertilizer may further comprise the steps:
(1) nitration mixture preparation
From sulfuric acid plant circulation groove H
2SO
4Mass concentration is 98% sulfuric acid, and temperature is controlled between 75 ℃-90 ℃, and the sulfuric acid pump is delivered to plate heater to sulfuric acid by after the under meter metering, enters conversion tank after reaching requirement by steam heating.
Repone K enters hopper by lift, through rotary disc feeder, spiral claim with worm conveyor enter conversion tank with the heating after sulfuric acid react first in conversion tank one district.
KCL and H
2SO
4Generate sal enixum and hydrogen chloride gas under the condition of heating, reaction equation is as follows:
KCL+H
2SO
4＝KHSO
4+HCL↑
The HCL volatilization that reaction generates is reclaimed production byproduct hydrochloric acid and is taken out the KHSO that reaction generates
4With excessive H
2SO
4Overflow to nitration mixture geosyncline phosphoric acid interior and after the metering of peroxophosphoric acid under meter and mix the generation nitration mixture.H in the phosphoric acid
3PO
4Mass concentration is 20%, and phosphoric acid proportion is 1.2g/ml, the material proportion 1t of Repone K, sulfuric acid, phosphoric acid: 0.5m
3: 3.5m
3
(2) in nitration mixture, add mass concentration 10%-18% ammoniacal liquor and carry out the pre-neutralization reaction
After the ammoniacal liquor of outsourcing is unloaded with aqua ammonia pump, be stored in the ammoniacal liquor storage tank, squeeze into the nitration mixture jar with pump then, the mass concentration of ammonia is 13% in the ammoniacal liquor, adds the nitration mixture proportion behind the ammoniacal liquor: 1.4g/ml.Nitration mixture after the neutralization finally is transported in the composite fertilizer and the post is used for production composite fertilizer.
The chemical equation that takes place:
2KHSO
4+2NH
3H
2O＝K
2SO
4+(NH
4)
2SO
4+2H
2O
H
3PO
4+NH
3H
2O＝NH
4H
2PO
4+H
2O
H
3PO
4+2NH
3H
2O＝(NH
4)
2HPO
4+2H
2O
Open aqua ammonia pump during driving and add ammoniacal liquor in the nitration mixture jar, attention will slowly add, regulated valve by a small margin, and control nitration mixture proportion then and exist: 1.4g/ml, the liquid level of grasping the ammoniacal liquor storage tank is between 50-90%.
In startup procedure, to pay close attention to ammoniacal liquor storage tank liquid level, nitration mixture proportion guarantees to be controlled at indication range, keep and multiple fertilizer in and the contact in post.
The operative employee measures the proportion of a nitration mixture and the liquid level of observing the ammoniacal liquor storage tank each hour, and carries out record.
The short period of time system shutdown can slowly be closed the aqua ammonia pump outlet valve earlier, stops aqua ammonia pump then and directly stops.
Long term stop after must earlier using up the ammoniacal liquor in the ammoniacal liquor storage tank, adds 0.5 meter water, and ammoniated water in the ammoniacal liquor storage tank is used up, and the dilute sulphuric acid of the 10-20% of topped up with water, and adding then neutralizes, and when pH value during at 7-9, replaces and can efflux after qualified.
(3) with nitration mixture after the pre-neutralization and the further neutralization reaction of gas ammonia, main monoammonium phosphate, diammonium phosphate, vitriolate of tartar, the ammonium sulfate mixture of generating of reaction.
Reaction equation:
H
3PO
4+NH
3＝NH
4H
2PO
4
H
3PO
4+2NH
3＝(NH
4)
2HPO
4
2KHSO
4+2NH
3＝(NH
4)
2SO
4+K
2SO
4
Nitration mixture enters ammonia reactor by the nitration mixture pump by the nitration mixture pipeline, gas ammonia is supplied with liquefied ammonia evaporation back by the ammonia station, control into ammonia, acid intake amount by valve, further neutralize, mix through stirring through entering neutralizing well after the ammonia reactor reaction, nitration mixture through with ammonia gas react after, the degree of neutralization of ammonia and phosphoric acid is 1.20.
(4) slip that is generated by step (3) enters feeding trough, in and tail gas discharge by feeding trough, add from feeding trough and regulate the auxiliary material that generates total nutrient, slip is sent into tablets press by spray pump and is carried out granulation then.
Embodiment 2
The difference of present embodiment and embodiment 1 is: adopting phosphoric acid proportion is 1.23g/ml, the material proportion 1t of Repone K, sulfuric acid, phosphoric acid: 0.9m
3: 3.5m
3The mass concentration of ammonia is 12% in the ammoniacal liquor, adds the former nitration mixture proportion behind the ammoniacal liquor: 1.4g/ml.Nitration mixture through with ammonia gas react after, the degree of neutralization of ammonia and phosphoric acid is 1.15.
Embodiment 3
The difference of present embodiment and embodiment 1 is: adopting phosphoric acid proportion is 1.27g/ml, the material proportion 1t of Repone K, sulfuric acid, phosphoric acid: 1.3m
3: 4m
3The mass concentration of ammonia is 18% in the ammoniacal liquor, adds the former nitration mixture proportion behind the ammoniacal liquor: 1.44g/ml.Nitration mixture through with ammonia gas react after, the degree of neutralization of ammonia and phosphoric acid is 1.24.
The degree of neutralization determination step is as follows among each embodiment of the present invention:
With in and in the one after another drop of triangular flask of going into 250mL of slip, add the about 50ml of distilled water, add one of 0.1% tetrabromo-mcresolsulfonphthalein indicator, if solution is the blue slip degree of neutralization of representing greater than 1.0; Show that its degree of neutralization is less than 1.0 if be yellow.
If degree of neutralization is greater than 1.0, with the H of 0.05mol/L
2SO
4Standard solution titration to yellow-green colour is first terminal point, writing down sulfuric acid consumption A (ml), add 10 of 1% phenolphthalein indicators again, is second terminal point with NaOH standard solution titration to the red-purple of 0.1mol/L, write down NaOH consumption B (ml), then be: degree of neutralization=1.0+A/B for degree of neutralization numerical value
If degree of neutralization is less than 1.0, then with the NaOH standardized solution of 0.1mol/L drip to grass green be first terminal point, write down consumption A ' (ml); Add 10 phenolphthalein indicators again, NaOH solution titration to the red-purple that continues with 0.1mol/L is second terminal point, writes down (mL) degree of neutralization numerical value: degree of neutralization=1.0-A '/B ' then of consumption B '.
Nitrogen (N) content is 11.5% in the embodiment 1 production compound potassium sulfate fertilizer, and phosphorus content is (with effective P
2O
5Meter) 19.0%, potassium (K
2O) 14.5%.
Nitrogen (N) content is 11.55% in the embodiment 2 production compound potassium sulfate fertilizers, and phosphorus content is (with effective P
2O
5Meter) 19.17%, potassium (K
2O) 14.71%.
Nitrogen (N) content is 11.82% in the embodiment 3 production compound potassium sulfate fertilizers, and phosphorus content is (with effective P
2O
5Meter) 18.14%, potassium (K
2O) 15.16%.
Claims (8)
1. the production method of a potassium sulfate compound fertilizer is characterized in that may further comprise the steps:
(1) vitriol oil and Repone K are generated the solution of sulfur-bearing potassium hydrogen phthalate and excess sulfuric acid at the conversion tank internal reaction, add again phosphoric acid mixed nitration mixture;
(2) ammoniacal liquor that adds mass concentration 10%-18% in nitration mixture carries out the pre-neutralization reaction;
(3) with nitration mixture after the pre-neutralization and the further neutralization reaction of gas ammonia, to the degree of neutralization of the phosphoric acid of ammonia and nitration mixture be 1.10～1.30;
(4) spray granulating.
2. according to the production method of the described a kind of potassium sulfate compound fertilizer of claim 1, it is characterized in that described vitriol oil mass concentration is 98%, phosphoric acid quality concentration is 20%.
3. according to the production method of claim 1 or 2 described a kind of potassium sulfate compound fertilizers, it is characterized in that the material proportion of described Repone K, the vitriol oil, phosphoric acid is 1t: 0.4-1.4m
3: 3.0-5.0m
3
4. according to the production method of the described a kind of potassium sulfate compound fertilizer of claim 3, it is characterized in that the material proportion of Repone K, the vitriol oil, phosphoric acid is 1t: 0.9m
3: 3.5m
3
5. according to the production method of the described a kind of potassium sulfate compound fertilizer of claim 1, it is characterized in that described ammoniacal liquor mass concentration is 12%
6. according to the production method of the described a kind of potassium sulfate compound fertilizer of claim 1, it is characterized in that the described former nitration mixture proportion that adds behind the mass concentration 10%-18% ammoniacal liquor: 1.38-1.45g/ml.
7. according to the production method of the described a kind of potassium sulfate compound fertilizer of claim 6, it is characterized in that the former nitration mixture proportion that adds behind the ammoniacal liquor is 1.4g/ml.
8. according to the production method of the described a kind of potassium sulfate compound fertilizer of claim 1, it is characterized in that the degree of neutralization of the phosphoric acid of step (3) reacting ammonia and nitration mixture is 1.15.
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|---|---|---|---|
| CN2009102312628A CN101817706B (en) | 2009-12-18 | 2009-12-18 | Production method for potassium sulfate compound fertilizer |
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|---|---|---|---|
| CN2009102312628A CN101817706B (en) | 2009-12-18 | 2009-12-18 | Production method for potassium sulfate compound fertilizer |
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| CN101817706A true CN101817706A (en) | 2010-09-01 |
| CN101817706B CN101817706B (en) | 2012-07-04 |
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ID=42653007
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153392A (en) * | 2011-04-08 | 2011-08-17 | 山东聊城鲁西化工第五化肥有限公司 | Production method of novel slow release urea-formaldehyde compound fertilizer |
| CN102249777A (en) * | 2011-04-28 | 2011-11-23 | 山东聊城鲁西化工第五化肥有限公司 | Production method for ammoniated sulfur-based compound fertilizer by chemical synthesis |
| CN102351588A (en) * | 2011-07-05 | 2012-02-15 | 山东聊城鲁西化工第五化肥有限公司 | Production method of novel chemically synthesized ammoniated sulfur-base composite fertilizer |
| CN104418626A (en) * | 2013-08-26 | 2015-03-18 | 山东聊城鲁西化工第五化肥有限公司 | Method for producing sulfur-based composite fertilizer by using monoammonium phosphate instead of phosphoric acid |
| CN106220278A (en) * | 2016-07-27 | 2016-12-14 | 中化化肥有限公司成都研发中心 | A kind of additive improving potassium sulfate compound fertilizer granule strength and the preparation method of high-strength complex Hefei granule |
| CN111943784A (en) * | 2020-09-17 | 2020-11-17 | 嘉施利（宜城）化肥有限公司 | Compound fertilizer production method |
-
2009
- 2009-12-18 CN CN2009102312628A patent/CN101817706B/en active Active
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153392A (en) * | 2011-04-08 | 2011-08-17 | 山东聊城鲁西化工第五化肥有限公司 | Production method of novel slow release urea-formaldehyde compound fertilizer |
| CN102153392B (en) * | 2011-04-08 | 2014-04-23 | 山东聊城鲁西化工第五化肥有限公司 | Production method of novel slow release urea-formaldehyde compound fertilizer |
| CN102249777A (en) * | 2011-04-28 | 2011-11-23 | 山东聊城鲁西化工第五化肥有限公司 | Production method for ammoniated sulfur-based compound fertilizer by chemical synthesis |
| CN102249777B (en) * | 2011-04-28 | 2013-07-17 | 山东聊城鲁西化工第五化肥有限公司 | Production method for ammoniated sulfur-based compound fertilizer by chemical synthesis |
| CN102351588A (en) * | 2011-07-05 | 2012-02-15 | 山东聊城鲁西化工第五化肥有限公司 | Production method of novel chemically synthesized ammoniated sulfur-base composite fertilizer |
| CN102351588B (en) * | 2011-07-05 | 2013-11-06 | 山东聊城鲁西化工第五化肥有限公司 | Production method of novel chemically synthesized ammoniated sulfur-base composite fertilizer |
| CN104418626A (en) * | 2013-08-26 | 2015-03-18 | 山东聊城鲁西化工第五化肥有限公司 | Method for producing sulfur-based composite fertilizer by using monoammonium phosphate instead of phosphoric acid |
| CN106220278A (en) * | 2016-07-27 | 2016-12-14 | 中化化肥有限公司成都研发中心 | A kind of additive improving potassium sulfate compound fertilizer granule strength and the preparation method of high-strength complex Hefei granule |
| CN111943784A (en) * | 2020-09-17 | 2020-11-17 | 嘉施利（宜城）化肥有限公司 | Compound fertilizer production method |
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| Publication number | Publication date |
|---|---|
| CN101817706B (en) | 2012-07-04 |
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Owner name: SHANDONG LIAOCHENG LUXI CHEMICAL FIFTH FERTILIZER Free format text: FORMER NAME: LIAOCHENG LUXI CHEMICAL NO.5 CHEMICAL FERTILIZER PLANT |
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Address after: 252300 No. 13 Han Qiao Road, Chengxi, Yanggu County, Shandong, Liaocheng Patentee after: Shandong Liaocheng Luxi Chemical Fifth Fertilizer Co.,Ltd. Address before: 252300 No. 13 Han Qiao Road, Chengxi, Yanggu County, Shandong, Liaocheng Patentee before: Liaocheng Luxi Chemical No.5 Chemical Fertilizer Plant |