CN1071408A - There is not chlorine composite fertilizer with Repone K as raw material production - Google Patents
There is not chlorine composite fertilizer with Repone K as raw material production Download PDFInfo
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- CN1071408A CN1071408A CN 91109650 CN91109650A CN1071408A CN 1071408 A CN1071408 A CN 1071408A CN 91109650 CN91109650 CN 91109650 CN 91109650 A CN91109650 A CN 91109650A CN 1071408 A CN1071408 A CN 1071408A
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- repone
- composite fertilizer
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- sulfuric acid
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Abstract
A kind of do not have the method for chlorine composite fertilizer with Repone K as raw material production, and it is that a certain proportion of Repone K and acid were made it to generate sal enixum in 0.5～2 hour 70～120 ℃ of reactions, and normal pressure feeds ammonia till pH reaches at 6.5～7 o'clock in this product.Above-mentioned acid can be sulfuric acid, also can be the nitration mixture of sulfuric acid and phosphoric acid, and they and Repone K are in Repone K: the ratio of sulfuric acid=1: 1.2～1.8 (mol ratio) is reacted.Method flow of the present invention is short, technology is simple, reaction conditions is gentle; The cost of saving the energy, product is low; The content of chlorine root meets no chlorine composite fertilizer standard in the product.
Description
The present invention relates to a kind of fertilizer, particularly a kind of inorganic composite fertilizer.
It is raw material production that no chlorine composite fertilizer generally is to use not chloride potash fertilizer, but such raw material source of goods is tight slightly, costs an arm and a leg, the difficult needs that satisfy agriculture production.But the source of goods of Repone K is comparatively abundant comparatively speaking, is that raw material production does not have chlorine composite fertilizer with Repone K so people have adopted many diverse ways.As reacting the typical method that makes vitriolate of tartar with sulfuric acid and Repone K is Mannheim proeess and extraction process, and the former flow process is brief but 700 ℃ of high temperature of need make industrial condition very harsh, and energy consumption is very high; The latter does not need high temperature, but reaction process is long, and technology is also complicated.Another kind is that vitriol and Klorvess Liquid carry out the method that replacement(metathesis)reaction makes vitriolate of tartar, as in＜chemical fertilizer industry〉(1987(1) 6-11) disclosed＜Repone K, ammonium sulfate transforms potassium sulfate making ammonium and ammonium chloride in its again one of association to abandoning the flow process that mother liquor is handled in a large number, so it is very long that whole flow process seems, make industrial production become loaded down with trivial details.
In view of above-mentioned weak point of the prior art the object of the present invention is to provide a kind of is the brief flow process of prepared using is produced the no chlorine composite fertilizer that need not to handle mother liquor under gentle reaction conditions method with Repone K.
Purpose of the present invention can realize by following measure: a kind of method of not having chlorine composite fertilizer with Repone K as raw material production, it is that a certain proportion of Repone K and acid were made it to generate sal enixum in 0.5～2 hour 60～120 ℃ of reactions, and it is characterized in that: normal pressure feeds ammonia till PH reaches at 6.5～7 o'clock in the product that makes under above-mentioned condition.The acid of reacting with Repone K can be sulfuric acid, also can be the nitration mixture of sulfuric acid and phosphoric acid.Repone K and sulfuric acid react in the ratio of 1: 1.2 above (mol ratio).The reaction that generates sal enixum is preferably in 80 ℃ of reactions 1 hour.
Method of the present invention mainly contains following reaction and carries out:
Its concrete brief description of the process is as follows:
What method of the present invention was at first carried out is Repone K and vitriolic reaction, and the consumption of its raw material is a Repone K: sulfuric acid=1: 1.2 above (mol ratio).If the transformation efficiency of Repone K was lower when the sulfuric acid consumption was lower than 1.2 moles; When if the sulfuric acid consumption is higher, the content of ammonium sulfate is higher in the product, and it can ratio according to actual needs adjust the vitriolic consumption.The raw material of aforementioned proportion is reacted under 70～120 ℃ temperature condition, and optimal reaction temperature is 80 ℃; Reaction times generally is 0.5～2 hour, and optimum reacting time is 1 hour.This reaction is preferably under the condition of negative pressure to be carried out, so that the hydrogen chloride gas that produces is in time got rid of, can be used as commodity hydrochloric acid through recovery.The first step reaction does not finish Repone K and is converted into sal enixum when having chlorion in the solution substantially and exist.In the product of this reaction, feed ammonia subsequently, make sal enixum further change vitriolate of tartar and ammonium sulfate into ammonia gas react.The reaction of second step is to carry out under normal pressure, and no longer heats.When the pH value of solution reaches 6.5～7, be reaction end.The composition that this binary does not have chlorine composite fertilizer can change, and promptly changes the composition of raw material and the structure that ratio can change final product, and the nitration mixture that adopts sulfuric acid and phosphoric acid as raw material acid then phosphoric acid and ammonia reacts again, so just can also be contained the Nitrogen, Phosphorus and Potassium of phosphorus.If the trace element that changes the ratio of sulfuric acid and phosphoric acid and add other also can obtain the multi-component composite fertilizer of different ratios.
The present invention has following advantage compared to existing technology: flow process is short, technology is simple, reaction conditions is put down, be suitable for suitability for industrialized production; The cost of product is low, the saving energy, good in economic efficiency; In the product content of chlorine root at the chloride content that is lower than in the world regulation about 1.5% in the index below 2.5%.
Embodiment 1
Repone K (K with 97.5 grams
2O61.5%) sulfuric acid with 233 grams 75% places there-necked flask, and heating makes temperature of charge maintain 80 ℃ under agitation condition, also makes the negative pressure that keeps 1333Pa in the bottle simultaneously.Through stopping heating and decompression after 1 hour the reaction, material in the there-necked flask feeds ammonia then, reach at 7 o'clock through the pH value of 15 minutes materials and be reaction end, the content of vitriolate of tartar is 98 grams in the gained slurry that stops to ventilate, and then the transformation efficiency of this reaction is 88.3%.
Embodiment 2
Repone K (K with 97.5 grams
2O61.5%) place there-necked flask with 75% sulfuric acid, 200 grams, heating makes temperature of reaction maintain 120 ℃ under agitation condition, also make the negative pressure that keeps 4000Pa in the bottle simultaneously, through stopped reaction and decompression after 2 hours the reaction, in the material of there-necked flask, feed ammonia then, reach at 7 o'clock through the pH value of 15 minutes materials, be reaction end, stop ventilation, the content of vitriolate of tartar is 102 grams in the gained slurry, and then the transformation efficiency of this reaction is 91.8%.
Embodiment 3
Repone K (K with 97.5 grams
2O61.5%) place there-necked flask with 75% sulfuric acid, 300 grams, heating makes temperature of charge maintain 70 ℃ under agitation condition, also make the negative pressure that keeps 1333Pa in the bottle simultaneously, through stopped reaction and decompression after 1.5 hours the reaction, in the material of there-necked flask, feed ammonia then, reach at 7 o'clock through the pH value of 15 minutes materials, be reaction end, stop ventilation, the content of vitriolate of tartar is 99 grams in the gained slurry, and then the transformation efficiency of this reaction is 89.0%.
Embodiment 4
Repone K (K with 97.5 grams
2O61.5%) place there-necked flask with 75% sulfuric acid, 266 grams, heating makes temperature of reaction maintain 110 ℃ under agitation condition, also make the negative pressure that keeps 2666Pa in the bottle simultaneously, through stopped reaction and decompression after 0.5 hour the reaction, in the material of there-necked flask, feed ammonia then, reach at 7 o'clock through the pH value of 15 minutes materials, be reaction end, stop ventilation, the content of vitriolate of tartar is 107 grams in the gained slurry, and then the transformation efficiency of this reaction is 96.3%.
Embodiment 5
Repone K (K with 97.5 grams
2O61.5%) with 75% sulfuric acid, 183 grams, P
2O
5Be 52% phosphoric acid, 27.2 grams, place there-necked flask, heating makes temperature of charge maintain 100 ℃ under agitation condition, also makes the negative pressure that keeps 2666Pa in the bottle simultaneously, through stopped reaction and decompression after 1 hour the reaction, in the material of there-necked flask, feed ammonia then, pH value through 15 minutes materials reaches at 6.5 o'clock, is reaction end, stops ventilation, the content of vitriolate of tartar is 98.8 grams in the gained slurry, and then the transformation efficiency of this reaction is 89%.At this moment just can obtain nitrogen, phosphorus, potassium Nitrogen, Phosphorus and Potassium slurry.
Claims (4)
1, a kind of method of not having chlorine composite fertilizer with Repone K as raw material production, it is that a certain proportion of Repone K and acid were made it to generate sal enixum in 0.5～2 hour 60～120 ℃ of reactions, and it is characterized in that: normal pressure feeds ammonia till PH reaches at 6.5～7 o'clock in the product that makes under these conditions.
2, according to claim 1 do not have the method for chlorine composite fertilizer with Repone K as raw material production, it is characterized in that: with the acid of Repone K reaction can be sulfuric acid, also can be the nitration mixture of sulfuric acid and phosphoric acid.
3, according to claim 1 and 2 do not have the method for chlorine composite fertilizer with Repone K as raw material production, and it is characterized in that: Repone K and sulfuric acid react in the ratio of 1: 1.2 above (mol ratio).
4, according to claim 3 do not have the method for chlorine composite fertilizer with Repone K as raw material production, it is characterized in that: the reaction that generates sal enixum is preferably in 80 ℃ of reactions 1 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91109650 CN1039222C (en) | 1991-10-07 | 1991-10-07 | Chloroless compound fertilizer using potassium chloride as raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91109650 CN1039222C (en) | 1991-10-07 | 1991-10-07 | Chloroless compound fertilizer using potassium chloride as raw material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1071408A true CN1071408A (en) | 1993-04-28 |
| CN1039222C CN1039222C (en) | 1998-07-22 |
Family
ID=4909912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91109650 Expired - Lifetime CN1039222C (en) | 1991-10-07 | 1991-10-07 | Chloroless compound fertilizer using potassium chloride as raw material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1039222C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045947C (en) * | 1997-03-26 | 1999-10-27 | 山东红日化工股份有限公司 | Method for preparing sulfonyl azophoska compound fertilizer |
| CN100337994C (en) * | 2006-03-24 | 2007-09-19 | 宜兴申利化工有限公司 | Method for preparing composite fertilizer of potassium sulfate and ammonium |
| CN102126737A (en) * | 2011-01-20 | 2011-07-20 | 山东金正大生态工程股份有限公司 | Method for producing nitrate-and-sulfur-based compound fertilizer and co-producing gypsum by utilizing potassium hydrogen sulfate |
| CN102515924A (en) * | 2011-12-29 | 2012-06-27 | 深圳市芭田生态工程股份有限公司 | Preparation method of chlorine-free compound fertilizer |
| CN102531748A (en) * | 2011-12-29 | 2012-07-04 | 深圳市芭田生态工程股份有限公司 | Production method for chlorine-free compound fertilizer |
| CN103588543A (en) * | 2013-11-28 | 2014-02-19 | 郑州大学 | Production method for multi-nutrient urea sulfuric acid sulfur-based composite fertilizer |
| CN107032834A (en) * | 2017-06-15 | 2017-08-11 | 开封大学 | The technique that liquid phase mortar gunite method produces potassium sulfate |
-
1991
- 1991-10-07 CN CN 91109650 patent/CN1039222C/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045947C (en) * | 1997-03-26 | 1999-10-27 | 山东红日化工股份有限公司 | Method for preparing sulfonyl azophoska compound fertilizer |
| CN100337994C (en) * | 2006-03-24 | 2007-09-19 | 宜兴申利化工有限公司 | Method for preparing composite fertilizer of potassium sulfate and ammonium |
| CN102126737A (en) * | 2011-01-20 | 2011-07-20 | 山东金正大生态工程股份有限公司 | Method for producing nitrate-and-sulfur-based compound fertilizer and co-producing gypsum by utilizing potassium hydrogen sulfate |
| CN102515924A (en) * | 2011-12-29 | 2012-06-27 | 深圳市芭田生态工程股份有限公司 | Preparation method of chlorine-free compound fertilizer |
| CN102531748A (en) * | 2011-12-29 | 2012-07-04 | 深圳市芭田生态工程股份有限公司 | Production method for chlorine-free compound fertilizer |
| CN103588543A (en) * | 2013-11-28 | 2014-02-19 | 郑州大学 | Production method for multi-nutrient urea sulfuric acid sulfur-based composite fertilizer |
| CN103588543B (en) * | 2013-11-28 | 2015-05-27 | 郑州大学 | Production method for multi-nutrient urea sulfuric acid sulfur-based composite fertilizer |
| CN107032834A (en) * | 2017-06-15 | 2017-08-11 | 开封大学 | The technique that liquid phase mortar gunite method produces potassium sulfate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1039222C (en) | 1998-07-22 |
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Owner name: DAHUA GROUP CO.,LTD. Free format text: FORMER NAME OR ADDRESS: DALIAN CHEMICAL INDUSTRY CO. |
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Patentee after: Dahua Group Co., Ltd. Patentee before: Dalian Chemical Industry Co. |
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Expiration termination date: 20111007 Granted publication date: 19980722 |