CN102515924A - Preparation method of chlorine-free compound fertilizer - Google Patents
Preparation method of chlorine-free compound fertilizer Download PDFInfo
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- CN102515924A CN102515924A CN2011104503487A CN201110450348A CN102515924A CN 102515924 A CN102515924 A CN 102515924A CN 2011104503487 A CN2011104503487 A CN 2011104503487A CN 201110450348 A CN201110450348 A CN 201110450348A CN 102515924 A CN102515924 A CN 102515924A
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Abstract
The invention discloses a preparation method of chlorine-free compound fertilizer, which has the process characteristics that: phosphoric acid, sulfuric acid or nitric acid reacts with phosphorite to form the phosphoric acid, and then the sulfuric acid is added in to form mixed acid; or excessive sulfuric acid reacts with the phosphorite to form the mixed acid of phosphoric acid and sulfuric acid; the mixed acid further reacts with potassium chloride at low temperature to generate intermediate products potassium dihydrogen phosphate, potassium hydrogen sulfate and hydrogen chloride, hydrogen chloride is absorbed by water and hydrochloric acid is formed; the intermediate products potassium dihydrogen phosphate and potassium hydrogen sulfate are neutralized by ammonia, mixed with the added nitrogen fertilizer or/and additive or/and phosphorus and potassium fertilizer required by a prescription, granulated, dried, cooled and screened, and the chlorine-free compound fertilizer is prepared. The product prepared through the method is suitable to serve as medium-grade and high-grade economic crop fertilizer for various crops. The preparation method of the chlorine-free compound fertilizer prepares the chlorine-free compound fertilizer by converting the mixed acid into potassium chloride at low temperature, and has the advantages of low reaction temperature, little energy consumption, short process, little investment, low cost and high product quality.
Description
Technical field
The present invention relates to a kind of no chlorine composite fertilizer producing process, the production of especially a kind of Repone K low-temp reaction does not have the chlorine-based compound fertilizer working method.
Background technology
Potassium primary phosphate is a kind of efficient phosphorus potassium complex fertilizer of high density, and because of it has nutritive ingredient height (P, K effective constituent>84%), chemical property is stable, and nothing is smelt, and is tasteless, nontoxic, soluble in water, do not lump, thereby is applicable to various soil and crop.Nutrient all can be absorbed by crop, can not cause soil compaction.Particularly low salt index is difficult for burning root and burns seedling.Be widely used in seed soaking, soak root, medicine seed dressing, pouring and foliage-spray, farm crop are quickened grouting, promote metabolism, resist hot dry wind and prevent that from all there is unusual effect aspect such as lodging.As farm crop base fertilizer and farm crop middle and later periods foliage application; Extensively be applied to various grains, cash crop and melon and fruit, vegetables etc. (as: various crops such as paddy rice, wheat, corn, sugarcane, soybean, cotton, flax, fruit, vegetables and tobacco); Being particularly useful for fear-chlorion crops such as tobacco, oranges and tangerines, tealeaves, is that the Ministry of Agriculture specifies the good fertilizer variety of promoting development.In recent years, not only find remarkable raising the output, drought resisting, the cold-resistant function of potassium primary phosphate, but also find that it also has special role to controlling crop diseases and insect pests.Thereby obtained in recent years developing rapidly and widespread use.Pure potassium primary phosphate even can be used as foodstuff additive is mineral element improved seeds of mending phosphorus and potassium.
The working method of potassium primary phosphate is a lot, roughly is summarised as neutralisation, extraction process, ion exchange method, double decomposition, direct method, crystallization process and electrolytic process etc.In China, production technique adopts neutralisation mostly, secondly also has organic extraction method, double decomposition, ion exchange method etc.Because the potassium primary phosphate quality is higher, the potassium primary phosphate price is also higher on the market, and the unit nutrient price is more than 1.5 ~ 2 times of other phosphate fertilizer, potash fertilizer price.But the existing working method cost of China's potassium primary phosphate is all higher, and high-quality potassium primary phosphate can not more extensively be produced in conventional composite fertilizer and use.
It generally is sulfuric acid and Repone K reaction that existing Repone K low temperature conversion is produced S-based compound fertilizer; The sal enixum that generates; Mix the formation nitration mixture with the phosphoric acid that the sulfuric acid acidation phosphorus ore produces again, nitration mixture neutralizes with ammonia again, and whitewashings such as interpolation nitrogenous fertilizer such as urea produce no chlorine S-based compound fertilizer.This production technique low temperature conversion Repone K, product is no chlorine S-based compound fertilizer, and adaptable across various crops, flow process is compact, and production cost is low.Production technique obtains large-scale popularization in China.It is China's sulphur base compound fertilizer main production.
But existing Repone K low temperature conversion is produced S-based compound fertilizer and had some problems: 1, nitrogen content is difficult to improve.It is general multiple fertile particularly to produce 15-15-15; Nitrogen is difficult to mention 15%; Therefore now domestic have the Repone K of employing low temperature conversion to produce sal enixum after, add other nitrogenous fertilizer and additives such as monoammonium phosphate and urea, with middle sal enixum in the ammonia as granulation slurry; Granule is produced nitrogen Gao Fufei, can produce various proportioning products after the improvement.This technology is also applied, and also needs outsourcing phosphorus ammonium and other nitrogenous fertilizer but improve back technology, and production cost does not have greater advantage.2, ammonium nitrogen content is high, is prone to burn seedling.No matter existing Repone K low temperature conversion is the ammonium group material method after mortar jetting method or the improvement if being produced S-based compound fertilizer; All contain a large amount of ammonium nitrogens, after the fertilising, ammonium nitrogen volatilizees easily; Be prone to burn leaf and burn seedling; If improper use also might cause crop production reduction, cause fertilizer efficiency general, the fertilizer quality is not high.Therefore, obtain large-scale popularization and be widely used though China's present stage Repone K low temperature conversion is produced the sulphur base compound fertilizer, the quality aspect all will be lower than import fertilizer, reaches the sulphur base compound fertilizer that using sulfated potassium, monoammonium phosphate, nitrogenous fertilizer etc. produce.
In view of this, necessary provide a kind of can low cost prodn, the no chlorine compound fertilizer production technology that quality is high.
Summary of the invention
The object of the present invention is to provide a kind of no chlorine composite fertilizer producing process, the reduction of product tooling cost, product quality are improved.
A kind of no chlorine composite fertilizer producing process comprises the steps:
(1) be that 18 ~ 85% phosphoric acid and mass concentration are that the nitration mixture that 30 ~ 100% sulfuric acid forms adds in the reaction unit with mass concentration; Add Repone K again; Reacted 0.5 ~ 6 hour under 100 ~ 350 ℃ of temperature, obtain containing the slip and the gas chlorination hydrogen of potassium primary phosphate, sal enixum;
(2) slip of gained in the step (1) and ammonia or carbon ammonium are carried out neutralization reaction in neutralization reactor, obtain granulation slurry;
(3) granulation slurry with gained in the step (2) carries out granulation;
(4) carry out drying, cooling, screening after the granulation, can obtain described no chlorine composite fertilizer, no chlorine composite fertilizer always supports and divides ≧ 25%, chlorine ≦ 3%; Granule after the screening is pulverized the back with big grain and is formed returning charge.
H 2 so 4 concentration described in the step (1) is 60 ~ 98%; Described phosphoric acid quality concentration is 20 ~ 35%.
Nitration mixture described in the step (1) and Repone K low-temp reaction temperature are 120 ~ 300 ℃.
The material proportion of phosphoric acid, sulfuric acid and Repone K is 1:0 ~ 10:0.1 ~ 13.5 described in the step (1).
Phosphoric acid described in the step (1) is thermal phosphoric acid, or phosphoric acid by wet process; Described phosphoric acid by wet process is by nitric acid and phosphorus ore reacted, or by sulfuric acid and phosphorus ore reacted.
Described phosphoric acid by wet process is by sulfuric acid and phosphorus ore reacted.
Neutralization reaction to slip pH value is 2 ~ 8 in the step (2).
In the granulating working procedure of step (3) with the common granulation of granulation slurry of gained in the returning charge in the step (4) and the step (2).
Also be added with in nitrogenous fertilizer, additive, phosphate fertilizer, the potash fertilizer one or more in the granulating working procedure in the step (3).
Described nitrogenous fertilizer comprises a kind of or its combination in urea, an ammonium nitrate, ammonium nitrate phosphate fertilizer, the ammonium sulfate; Described phosphate fertilizer comprises a kind of or its combination in monoammonium phosphate, diammonium phosphate, potassium primary phosphate, double superhosphate, superphosphate of lime, the fused(calcium magnesium)phosphate; Described potash fertilizer comprises a kind of or its combination in vitriolate of tartar, saltpetre, the salt of wormwood; Described additive comprises middle microelement fertilizer, functional additive and filler.
Beneficial effect of the present invention: with respect to prior art; A kind of no chlorine-based compound fertilizer working method of the present invention; The composite fertilizer that article are produced for no chlorine potassium primary phosphate in the middle of producing is equivalent to Repone K is combined with phosphoric acid metathesis production potassium primary phosphate production technique and Repone K low temperature conversion production production of sulfur-based compound fertilizer technology.Production technique is compact, and technical process weak point, less investment, temperature of reaction are low, less energy consumption, cost are low.Produce the product quality height, be applicable to various crops with fertile, particularly medium-to-high grade cash crop are with fertile.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is an another kind of process flow sheet of the present invention.
Embodiment
Be further described with embodiment below:
Specific embodiment 1:
Excessive sulfuric acid and phosphorus ore reaction, solid part filters, and remaining liquid promptly is phosphoric acid and sulfuric acid nitration mixture; The phosphoric acid quality concentration 18% of nitration mixture, phosphoric acid need not concentrate, vitriolic mass concentration 73%; With pump nitration mixture is delivered to reactive tank, in nitration mixture, add Repone K and react, addition is: pure 100% phosphoric acid: pure 100% sulfuric acid: pure 100% Repone K ratio 1:0.2:0.87; Reactive tank adopts the chuck heating that the reaction slurry temperature is raised to 300 ℃ except that utilizing reaction heat simultaneously, and the reaction times is controlled to be 2 hours; The hydrogen chloride gas water that reaction produces absorbs, and produces the quality percentage composition and be 32% hydrochloric acid sub product.The slip partial reaction generates intermediates potassium primary phosphate, sal enixum and a small amount of spent acid; The neutralization of application ammonia; Produce next step middle article potassium primary phosphate, vitriolate of tartar, ammonium sulfate, monoammonium phosphate, diammonium phosphate mixture; And contain 28% moisture, in slip as granulation slurry, mix the dense slurry granulation of formation with an ammonium nitrate that from revert system, adds and essential middle trace element.Granulation is after drying is cooled off operations such as screening, and producing 15-15-15 does not have chlorine composite fertilizer.
This production technique is with the production of phosphoric acid by wet process, and Repone K low temperature conversion sal enixum, the potassium primary phosphate technological process of production combine, and produces no chlorine composite fertilizer.Production cost is low, and production technique is compact, and technical process weak point, less investment, temperature of reaction are low, less energy consumption, cost are low.
Change ratio and concentration such as sulfuric acid, phosphorus ore and Repone K, nitrogenous fertilizer, additive change the operating procedure temperature, just can produce various different proportioning compound manure, and production formula is flexible.
Specific embodiment 2:
Adopt mass concentration 75% phosphoric acid; With mass concentration 98% sulfuric acid nitration mixture, with pump nitration mixture is delivered to reactive tank, in nitration mixture, add Repone K and react; Addition is: pure 100% phosphoric acid: pure 100% sulfuric acid: pure 100% Repone K ratio 1:0.4:0.87; Reactive tank adopts the chuck heating that the reaction slurry temperature is raised to 120 ℃ except that utilizing reaction heat simultaneously, and the reaction times is controlled to be 1.5 hours; The hydrogen chloride gas water that reaction produces absorbs, and produces the quality percentage composition and be 32% hydrochloric acid sub product.The slip partial reaction generates intermediates potassium primary phosphate, sal enixum and a small amount of spent acid; The neutralization of application ammonia; Produce next step middle article potassium primary phosphate, vitriolate of tartar, ammonium sulfate, monoammonium phosphate, diammonium phosphate mixture; And contain the moisture of quality percentage composition 15%, in slip as granulation slurry, mix the dense slurry granulation of formation with urea that from revert system, adds and essential middle trace element.Granulation is after drying is cooled off operations such as screening, and producing 15-15-15 does not have chlorine composite fertilizer.
This production technique changes the operating procedure temperature with change ratio and concentration such as phosphoric acid, sulfuric acid and Repone K, nitrogenous fertilizer, additives, just can produce various different proportioning compound manure, and production formula is flexible.
It is low that this production technique is produced no chlorine composite fertilizer production cost, the production technique compactness, and technical process weak point, less investment, temperature of reaction are low, less energy consumption, cost are low.
A kind of no chlorine composite fertilizer producing process production cost of the present invention is low, less investment.It is the phosphorus source that the contained nutrient of compound fertilizer product is equivalent to adopt potassium primary phosphate, with vitriolate of tartar, an ammonium nitrate or urea etc. and in little fertile no chlorine composite fertilizer that produces, the product ammonium nitrogen is low, be difficult for burning root and burn seedling, good fertilizer efficiency, quality is high.
According to the announcement and the instruction of above-mentioned specification sheets, those skilled in the art in the invention can also change and revise above-mentioned embodiment.Therefore, the embodiment that discloses and describe above the present invention is not limited to also should fall in the protection domain of claim of the present invention modifications more of the present invention and change.In addition, although used some specific terms in this specification sheets, these terms are explanation for ease just, the present invention is not constituted any restriction.
Claims (10)
1. a no chlorine composite fertilizer producing process is characterized in that, comprises the steps:
(1) be that 18 ~ 85% phosphoric acid and mass concentration are that the nitration mixture that 30 ~ 100% sulfuric acid forms adds in the reaction unit with mass concentration; Add Repone K again; Reacted 0.5 ~ 6 hour under 100 ~ 350 ℃ of temperature, obtain containing the slip and the gas chlorination hydrogen of potassium primary phosphate, sal enixum;
(2) slip of gained in the step (1) and ammonia or carbon ammonium are carried out neutralization reaction in neutralization reactor, obtain granulation slurry;
(3) granulation slurry with gained in the step (2) carries out granulation;
(4) carry out drying, cooling, screening after the granulation, can obtain described no chlorine composite fertilizer, no chlorine composite fertilizer always supports and divides ≧ 25%, chlorine ≦ 3%; Granule after the screening is pulverized the back with big grain and is formed returning charge.
2. the said no chlorine composite fertilizer producing process of claim 1, it is characterized in that: the h 2 so 4 concentration described in the step (1) is 60 ~ 98%; Described phosphoric acid quality concentration is 20 ~ 35%.
3. the described no chlorine composite fertilizer producing process of claim 1, it is characterized in that: nitration mixture described in the step (1) and Repone K low-temp reaction temperature are 120 ~ 300 ℃.
4. the described no chlorine composite fertilizer producing process of claim 1, it is characterized in that: the material proportion of phosphoric acid, sulfuric acid and Repone K is 1:0 ~ 10:0.1 ~ 13.5 described in the step (1).
5. the described no chlorine composite fertilizer producing process of claim 1, it is characterized in that: the phosphoric acid described in the step (1) is thermal phosphoric acid, or phosphoric acid by wet process; Described phosphoric acid by wet process is by nitric acid and phosphorus ore reacted, or by sulfuric acid and phosphorus ore reacted.
6. the described no chlorine composite fertilizer producing process of claim 5, it is characterized in that: described phosphoric acid by wet process is by sulfuric acid and phosphorus ore reacted.
7. the described no chlorine composite fertilizer producing process of claim 1 is characterized in that: neutralization reaction to slip pH value is 2 ~ 8 in the step (2).
8. the described no chlorine composite fertilizer producing process of claim 1 is characterized in that: in the granulating working procedure of step (3) with the common granulation of granulation slurry of gained in returning charge in the step (4) and the step (2).
9. the described no chlorine composite fertilizer producing process of claim 1 is characterized in that: also be added with in nitrogenous fertilizer, additive, phosphate fertilizer, the potash fertilizer one or more in the granulating working procedure in the step (3).
10. the described no chlorine composite fertilizer producing process of claim 9, it is characterized in that: described nitrogenous fertilizer comprises a kind of or its combination in urea, an ammonium nitrate, ammonium nitrate phosphate fertilizer, the ammonium sulfate; Described phosphate fertilizer comprises a kind of or its combination in monoammonium phosphate, diammonium phosphate, potassium primary phosphate, double superhosphate, superphosphate of lime, the fused(calcium magnesium)phosphate; Described potash fertilizer comprises a kind of or its combination in vitriolate of tartar, saltpetre, the salt of wormwood; Described additive comprises middle microelement fertilizer, functional additive and filler.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011104503487A CN102515924A (en) | 2011-12-29 | 2011-12-29 | Preparation method of chlorine-free compound fertilizer |
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| CN2011104503487A CN102515924A (en) | 2011-12-29 | 2011-12-29 | Preparation method of chlorine-free compound fertilizer |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588543A (en) * | 2013-11-28 | 2014-02-19 | 郑州大学 | Production method for multi-nutrient urea sulfuric acid sulfur-based composite fertilizer |
| CN104401951A (en) * | 2014-11-27 | 2015-03-11 | 贵州开磷（集团）有限责任公司 | Nitrogen, phosphorus and magnesium compound fertilizer produced from high-magnesium phosphate ore and production method of compound fertilizer |
| CN105294210A (en) * | 2015-11-23 | 2016-02-03 | 贵州开磷集团股份有限公司 | Method and apparatus for preparation of nitrogen and phosphorus composite fertilizer by mixing nitric acid and phosphoric acid |
| CN105294195A (en) * | 2015-10-20 | 2016-02-03 | 安庆市丰裕农林发展有限公司 | Liquid fertilizer applying method for plants |
| RU2608813C1 (en) * | 2015-07-20 | 2017-01-24 | федеральное государственное бюджетное образовательное учреждение высшего образования "Ставропольский государственный аграрный университет" (ФГБОУ ВО Ставропольский ГАУ) | Biological fertilizer |
| CN108484322A (en) * | 2018-04-11 | 2018-09-04 | 李玉华 | Fulvic acid double superhosphate potassium dihydrogen phosphate ammophos preparation method and system |
| CN108530207A (en) * | 2018-07-02 | 2018-09-14 | 郑州大学 | A method of preparing particle urea nitro-compound fertilizer with urea decomposing phosphorite by using nitric acid |
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| CN1071408A (en) * | 1991-10-07 | 1993-04-28 | 大连化学工业公司 | There is not chlorine composite fertilizer with Repone K as raw material production |
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| CN1071408A (en) * | 1991-10-07 | 1993-04-28 | 大连化学工业公司 | There is not chlorine composite fertilizer with Repone K as raw material production |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104401951A (en) * | 2014-11-27 | 2015-03-11 | 贵州开磷（集团）有限责任公司 | Nitrogen, phosphorus and magnesium compound fertilizer produced from high-magnesium phosphate ore and production method of compound fertilizer |
| RU2608813C1 (en) * | 2015-07-20 | 2017-01-24 | федеральное государственное бюджетное образовательное учреждение высшего образования "Ставропольский государственный аграрный университет" (ФГБОУ ВО Ставропольский ГАУ) | Biological fertilizer |
| CN105294195A (en) * | 2015-10-20 | 2016-02-03 | 安庆市丰裕农林发展有限公司 | Liquid fertilizer applying method for plants |
| CN105294210A (en) * | 2015-11-23 | 2016-02-03 | 贵州开磷集团股份有限公司 | Method and apparatus for preparation of nitrogen and phosphorus composite fertilizer by mixing nitric acid and phosphoric acid |
| CN108484322A (en) * | 2018-04-11 | 2018-09-04 | 李玉华 | Fulvic acid double superhosphate potassium dihydrogen phosphate ammophos preparation method and system |
| CN108530207A (en) * | 2018-07-02 | 2018-09-14 | 郑州大学 | A method of preparing particle urea nitro-compound fertilizer with urea decomposing phosphorite by using nitric acid |
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Application publication date: 20120627 |