CN102531748A - Production method for chlorine-free compound fertilizer - Google Patents
Production method for chlorine-free compound fertilizer Download PDFInfo
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- CN102531748A CN102531748A CN2011104503148A CN201110450314A CN102531748A CN 102531748 A CN102531748 A CN 102531748A CN 2011104503148 A CN2011104503148 A CN 2011104503148A CN 201110450314 A CN201110450314 A CN 201110450314A CN 102531748 A CN102531748 A CN 102531748A
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Abstract
The invention discloses a production method for a chlorine-free compound fertilizer. The process is characterized by comprising the following steps of: reacting phosphoric acid or sulfuric acid or nitric acid with phosphorite to form phosphoric acid; adding sulfuric acid to form mixed acid; or reacting an excess amount of sulfuric acid with phosphorite to form phosphoric acid and sulfuric acid mixed acid; then reacting with potassium chloride at a low temperature to produce intermediate products of potassium dihydrogen phosphate, potassium hydrogen sulfate and hydrogen chloride; absorbing hydrogen chloride gas by water to produce a hydrochloric acid byproduct; adding slurry part, which is the intermediate products of potassium dihydrogen phosphate and potassium hydrogen sulfate and a part of remaining acid, into phosphorite powder for hybrid reaction and aging; and mixing aged products with added nitrogen fertilizer, additive or/and phosphorous fertilizer and potassium fertilizer to be replenished for a formula and granulating, drying, cooling and screening to produce the chlorine-free compound fertilizer. The product provided by the invention is a fertilizer which is applicable to various crops, particularly high and medium grade economic crops. According to the production method, the potassium chloride is converted through the mixed acid at the low temperature to produce the chlorine-free compound fertilizer; and the method has the advantages of low reaction temperature, low energy consumption, short process flow, less 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 is 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 with gained in the step (1) adds in the ground phosphate rock, and thorough mixing reacts also ageing 0.5 ~ 240 hour, obtains containing the mixture of potassium dihydrogen sulfate, vitriolate of tartar, secondary calcium phosphate, calcium sulfate, and mixture pH value is 2 ~ 8;
(3) mixture with step (2) gained 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.
Phosphoric acid quality concentration described in the step (1) is 20 ~ 35%; Described h 2 so 4 concentration is 60 ~ 98%.
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.
Evaporate under the gas chlorination hydrogen heating condition that produces in the step (1), water absorbs the back and generates hydrochloric acid.
In the granulating working procedure in the step (3) with the common granulation of mixture of returning charge in the step (4) and step (2) gained.
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.
The present invention adopts to have phosphoric acid to participate in producing multiple fertile method with the dechlorination of Repone K reaction, can low cost prodn less salt composite fertilizer, and the various nitrogen phosphorus of flexible potassium does not have chlorine composite fertilizer prescription.
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, and vitriolic mass concentration 73% is delivered to reactive tank with pump with nitration mixture; In nitration mixture, add Repone K and react, addition is: pure 100% phosphoric acid: pure 100% sulfuric acid: pure 100% Repone K ratio 1:0.1:1.3.Reactive tank adopts 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, and the hydrogen chloride gas water that reaction produces absorbs, and produces the quality percentage composition and be 32% hydrochloric acid sub product.Slip partly is intermediates potassium primary phosphate, sal enixum and part spent acid, adds hybrid reaction in the ground phosphate rock, carries out ageing.Adding the ground phosphate rock amount is spent acid 1.7 times by sulphur acid meter weight, and digestion time is 3 days.An ammonium nitrate of product and interpolation and essential middle micro-mixing granulation after the ageing.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 1:0.2:1.3.Reactive tank adopts 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, and the hydrogen chloride gas water that reaction produces absorbs, and produces the quality percentage composition and be 32% hydrochloric acid sub product.Slip partly is intermediates potassium primary phosphate, sal enixum and part spent acid, adds hybrid reaction in the ground phosphate rock, carries out ageing.Adding the ground phosphate rock amount is spent acid 1.7 times by sulphur acid meter weight, and digestion time is 7 days.The urea of product and interpolation and essential middle micro-mixing granulation after the ageing.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 or do not contain ammonium nitrogen, 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 with gained in the step (1) adds in the ground phosphate rock, and thorough mixing reacts also ageing 0.5 ~ 240 hour, obtains containing the mixture of potassium dihydrogen sulfate, vitriolate of tartar, secondary calcium phosphate, calcium sulfate, and mixture pH value is 2 ~ 8;
(3) mixture with step (2) gained 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 phosphoric acid quality concentration described in the step (1) is 20 ~ 35%; Described h 2 so 4 concentration is 60 ~ 98%.
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: evaporate under the gas chlorination hydrogen heating condition that produces in the step (1), generate hydrochloric acid after water absorbs.
8. the described no chlorine composite fertilizer producing process of claim 1 is characterized in that: in the granulating working procedure in the step (3) with the common granulation of mixture of returning charge in the step (4) and step (2) gained.
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104503148A CN102531748A (en) | 2011-12-29 | 2011-12-29 | Production method for chlorine-free compound fertilizer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011104503148A CN102531748A (en) | 2011-12-29 | 2011-12-29 | Production method for chlorine-free compound fertilizer |
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| CN102531748A true CN102531748A (en) | 2012-07-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261376A (en) * | 2014-09-19 | 2015-01-07 | 贵阳中化开磷化肥有限公司 | Preparation method of special compound fertilizer for haricot |
| CN110483125A (en) * | 2019-08-02 | 2019-11-22 | 史丹利化肥当阳有限公司 | Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101618985A (en) * | 2009-08-07 | 2010-01-06 | 中国-阿拉伯化肥有限公司 | System and method for producing chlorine-free phospho potash complex fertilizer using method of low-temperature decomposition by fusion |
-
2011
- 2011-12-29 CN CN2011104503148A patent/CN102531748A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101618985A (en) * | 2009-08-07 | 2010-01-06 | 中国-阿拉伯化肥有限公司 | System and method for producing chlorine-free phospho potash complex fertilizer using method of low-temperature decomposition by fusion |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261376A (en) * | 2014-09-19 | 2015-01-07 | 贵阳中化开磷化肥有限公司 | Preparation method of special compound fertilizer for haricot |
| CN104261376B (en) * | 2014-09-19 | 2016-04-27 | 贵州开磷集团股份有限公司 | A kind of preparation method of French beans composite fertilizer special |
| CN110483125A (en) * | 2019-08-02 | 2019-11-22 | 史丹利化肥当阳有限公司 | Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material |
| CN110483125B (en) * | 2019-08-02 | 2022-03-04 | 史丹利化肥当阳有限公司 | Method for producing raw material for sulfur-based compound fertilizer by using waste phosphoric acid |
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Application publication date: 20120704 |