CN103570410A - Method for one-step-method preparation of nitrogen-phosphorus-potassium composite fertilizer by using potash feldspar - Google Patents
Method for one-step-method preparation of nitrogen-phosphorus-potassium composite fertilizer by using potash feldspar Download PDFInfo
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- CN103570410A CN103570410A CN201210268458.6A CN201210268458A CN103570410A CN 103570410 A CN103570410 A CN 103570410A CN 201210268458 A CN201210268458 A CN 201210268458A CN 103570410 A CN103570410 A CN 103570410A
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Abstract
The invention discloses a method for one-step-method preparation of a nitrogen-phosphorus-potassium composite fertilizer by using potash feldspar, relates to comprehensive utilization of resources of mining industry, chemical industry and environmental protection and other fields, particularly relates to a production method which uses a technology for using the potash feldspar for extraction of effective potassium and simultaneously for preparation of the nitrogen-phosphorus-potassium composite fertilizer, and belongs to the technical field of fertilizer production. The method uses an acidic reaction solution for decomposition of phosphorus ore and the potash feldspar to prepare the nitrogen-phosphorus-potassium composite fertilizer with different nutrient contents. According to the method, slightly soluble potassium in the potash feldspar can be transferred into the effective potassium under relatively mild conditions for realizing the effective use of potash feldspar resources so as to solve the problem that potash fertilizers in China are depended on imports. By use of the method, the production cycle can be shortened, a fluorine recovery system can be simplified, the production efficiency is improved, and the construction investment is saved. The produced fertilizer product is full in nitrogen, phosphorus and potassium nutrients, is rapid and long-term in effect, effectively improves the fertilizer nutrient use efficiency, meets agricultural scientific fertilization requirements, and is environmental-friendly. The method is cheap and easily-available in raw materials, simple in process, convenient in operation and easy in realization of large-scale industrial production.
Description
Technical field the present invention relates to the comprehensive utilization of resources in the fields such as mining industry, chemical industry and environmental protection, and the potassium felspar sand of particularly take extracts the manufacture method that effective potassium is produced nitrogenous, phosphorus, K composite fertilizer simultaneously as raw material single stage method.
Technical background sylvite is the general name that occurring in nature contains potassium class mineral, can be divided into solubility and insoluble two classes.The Potash Resources of solubility is the main potassium resource that the present whole world develops and utilizes, and China's soluble potassium resource reserve extremely lacks comparatively speaking, and the Potash Resources reserves of insoluble are very abundant, has broad application prospects and huge economic potential.
Potassium felspar sand stable in properties, contained potassium element is fixed in silica-aluminum-oxygen tetrahedron grid, can not be directly as being absorbed by plant containing potassic fertilizer, how under the prerequisite of economy, become soluble potassium element and become a worldwide application difficult problem guaranteeing; Adopted kinds of processes research both at home and abroad, but due to economy restriction, always can not heavy industrialization utilization.The method that the potassium felspar sand of take is raw material production potash fertilizer has been carried out many-sided discussion, and main method has following several:
1, press hot method.Reaction mass is placed in pressure reactor, under 200～500 ℃, 0.3～6.1MPa, with containing CaCl
2, Ca (OH)
2, CaO+CaCl
2, CaO+NaCl etc. aqueous solution decomposing of potassium feldspar prepare sylvite.
2, microorganism decomposition method.The method of utilizing microorganism and potassium felspar sand generation biochemical reaction decomposing of potassium feldspar that potassium is wherein extracted.Investigator has found that some bacteriums, fungi can destroy the crystalline network of potassium-bearing mineral, discharges effective potassium element.
3, high-temperature decomposition.Comprise pyrogenic process, hot legal system solubility in citric acid potassium, thermolysis water seaoning etc.This class reaction is reacted after referring to potassium felspar sand evenly being mixed according to proportioning with auxiliary agent or additive at the temperature of 900～1500 ℃, makes insoluble potassium be transformed into soluble potassium.
4, low-temperature decomposition method.Comprise sulphur-fluorine nitration mixture decomposition method, sulfuric acid adding assistant decomposition method, potassium felspar sand-phosphorus ore-mineral acid decomposition method and alkaline process decomposition etc.This class decomposition method refers to after potassium felspar sand mixes with auxiliary agents such as hydrofluoric acid or additive and sulfuric acid or calcium oxide and reacts at lower temperature.
Above-mentionedly take potassium felspar sand and prepare the whole bag of tricks of potash fertilizer as raw material, in preparation process energy consumption high, comprehensive utilization of resources is reasonable not, discharge in various degree " three wastes " material is given environment.The potash fertilizer products nutrient of producing more single simultaneously.Except part high-temperature decomposition, all there is not stable large-scale production,
Soluble potassium ore resources shortage that can direct production potash fertilizer for China, and soil and the farm crop present situation large to the demand of potash fertilizer, the object of the invention be to provide a kind of take reserves very abundant and again potassium felspar sand cheap but that be difficult to utilize be raw material, by its contained insoluble potassium component single stage method is converted into can be absorbed by crops soluble potassium (solubility in citric acid and water-soluble), obtain having the preparation method of the nitrogen-phosphorus-potassium compound fertilizer of higher plant recovery of nutrient simultaneously.
This technique of summary of the invention is prepared into acid urea reactant salt liquid with mineral acid and urea reaction, after mixing with potassium felspar sand and phosphorus ore, put into reactor, after reacting at a certain temperature certain hour, take out, and continue slaking certain hour, be prepared into nitrogen-phosphorus-potassium compound fertilizer.Its concrete steps are described below:
(1) by urea respectively at normal temperatures and mineral acid (sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid etc.) be prepared into acid urea reactant salt liquid,
(2) by feldspar in powder and ground phosphate rock by certain mass than adding in the reactor that prepares acid urea reactant salt liquid, mix,
(3) react for some time at a certain temperature, take out,
(4) slaking certain hour makes nitrogen-phosphorus-potassium compound fertilizer.
Wherein, the mol ratio of described acid urea reactant salt liquid is: n (urea): n (sulfuric acid)=(0～4): 1, n (urea): n (nitric acid)=(0～3): 1, n (urea): n (phosphoric acid)=(0～3): 1, n (urea): n (hydrochloric acid)=(0～5): 1.
50～130 ℃ of described temperature of reaction,
Described reaction times 0.5～5h,
The mass ratio of described feldspar in powder and ground phosphate rock is (0.1～2): 1,
Described curing time 0.5～8h.
Compared with prior art, the present invention has the following advantages:
A environmental pollution of the present invention is little, and resource utilization is high.Based on the theoretical investigation of fluorine form is shown, the urea of application of the present invention reacts and can generate silicofluoric acid urea with phosphorus ore with the acid urea reactant salt liquid that mineral acid forms, reaction conditions is gentleer, significantly reduce the vapour pressure of silicofluoric acid, the effusion rate of fluorine is reduced, operational condition is obviously improved, and with existing various technique comparisons, is low, the environmentally friendly technique of a kind of energy expenditure.
B the present invention due to application acid urea reactant salt liquid; improved indissoluble phosphorus and potassium to the level of response of effective constituent, and by single step reaction, just obtained having the product of appropriate slow, technique is simple; operation index is easily realized and is controlled, and is easy to realize large-scale industrial and produces.
C. this technique main raw material adaptability is very strong, is particularly suited for China's potassium and phosphor resource present situation.Except using insoluble potassium felspar sand, in can using, low-grade phosphorus ore, be conducive to making full use of of resource, cost is lower than similar composite fertilizer simultaneously, has obvious economic competitiveness.
D。In the present invention, a step is produced nitrogen-phosphorus-potassium compound fertilizer, nutrient is complete, wherein contain quick-acting water-soluble nitrogen, phosphorus and potassium simultaneously, and long-acting slow nitrogen, citric acid soluble phosphorus and the potassium of appropriateness, can meet the demand of crop different growing stages to nutrient, improve plant recovery of nutrient, reduce the impact of nutrient loss on environment, being conducive to enforcement and the popularization of agriculture balance fertilizing, is high, the eco-friendly fertilizer product of a kind of plant recovery of nutrient.
Embodiment, in order to understand better the present invention, is further illustrated content of the present invention below in conjunction with example, but content of the present invention is not only confined to exemplifying embodiment below.
Embodiment 1
(1) vitriol oil that is 98% by urea and massfraction adds in reactor for 2: 1 in molar ratio, urea and sulfuric acid generation solubilizing reaction generate urea sulfuric acid solution (acid urea reactant salt liquid), then adding mass ratio is feldspar in powder and the ground phosphate rock of 0.8: 1, mixes.Reactor is placed at 120 ℃ and reacts 3h, take out cooling and continue slaking 1.5h, be prepared into nitrogen-phosphorus-potassium compound fertilizer.
(2) 20g/L citric acid solution 200mL leaching for the product (1) being obtained, put into vibrator and shake 1h, dry filtration immediately, discard initial several milliliters of filtrates, with tetraphenyl, close the content of its effective potassium oxide of potassium borate gravimetric determination, now effectively Potassium leaching rate can reach more than 84%, and water-soluble potassium solubility rate can reach more than 29%.
Embodiment 2
(1) nitric acid of urea and 5.5mol/L is added in reactor for 1: 2 in molar ratio, urea and nitric acid generation solubilizing reaction generate urea salpeter solution (acid hydrolysis solution), and then adding mass ratio is feldspar in powder and the ground phosphate rock of 0.8: 1, mixes.Reactor is placed at 120 ℃ and reacts 2h, and taking-up is cooled to room temperature and continues slaking 1.5h again, is prepared into nitrogen-phosphorus-potassium compound fertilizer.
(2) 20g/L citric acid solution 200mL leaching for the product (1) being obtained, put into vibrator and shake 1h, dry filtration immediately, discard initial several milliliters of filtrates, with tetraphenyl, close the content of its effective potassium oxide of potassium borate gravimetric determination, now effectively Potassium leaching rate can reach more than 83%, and water-soluble potassium solubility rate can reach 46.08%.
Embodiment 3
(1) phosphoric acid of urea and massfraction 50% is added in reactor for 0.65: 1 in molar ratio, urea and phosphoric acid generation solubilizing reaction generate urea phosphoric acid solution (acid hydrolysis solution), then adding mass ratio is feldspar in powder and the ground phosphate rock of 0.8: 1, mixes.Reactor is placed at 130 ℃ and reacts 3h, and taking-up is cooled to room temperature and continues slaking 1.5h again, is prepared into nitrogen-phosphorus-potassium compound fertilizer.
(2) 20g/L citric acid solution 200mL leaching for the product (1) being obtained, put into vibrator and shake 1h, dry filtration immediately, discard initial several milliliters of filtrates, with tetraphenyl, close the content of its effective potassium oxide of potassium borate gravimetric determination, now effectively Potassium leaching rate can reach more than 90%, and water-soluble potassium solubility rate can reach 23.20%.
Embodiment 4
(1) phosphoric acid of urea and massfraction 50% is added in reactor for 0.65: 1 in molar ratio, urea and phosphoric acid generation solubilizing reaction generate urea phosphoric acid solution (acid hydrolysis solution), then adding mass ratio is feldspar in powder and the ground phosphate rock of 0.8: 1, mixes.Reactor is placed at 110 ℃ and reacts 3h, and taking-up is cooled to room temperature and continues slaking 1.5h again, is prepared into nitrogen-phosphorus-potassium compound fertilizer.
(2) 20g/L citric acid solution 200mL leaching for the product (1) being obtained, put into vibrator and shake 1h, dry filtration immediately, discard initial several milliliters of filtrates, with tetraphenyl, close the content of its effective potassium oxide of potassium borate gravimetric determination, now effectively Potassium leaching rate can reach more than 89%, and water-soluble potassium solubility rate can reach 17%.
Claims (8)
1. one kind is used that reserves are very abundant and potassium felspar sand and Phosphate Rock of China (main component is calcium monofluorophosphate) cheap but that be difficult to utilize are raw material again, with the acid urea reactant salt liquid reaction generating with urea and mineral acid, One-step production is nitrogenous, the manufacture method of phosphorus, K composite fertilizer.
2. preparation method claimed in claim 1, is characterized in that first adding mineral acid and urea to be prepared into acid urea reactant salt liquid, then by phosphorus ore, potassium felspar sand and the acid urea reactant salt liquid that is prepared into by metering than adding hybrid reaction in reactor.
3. preparation method claimed in claim 1, the mass ratio that it is characterized in that described feldspar in powder and ground phosphate rock is (0.1～2): 1.
4. preparation method claimed in claim 2, is characterized in that described mineral acid is selected from sulfuric acid or nitric acid or phosphoric acid or hydrochloric acid etc.
5. preparation method claimed in claim 1, it is characterized in that urea to be dissolved in and in inorganic acid solution, to make the acid urea reactant salt liquid (urea mineral acid adducts) of urea salt, its batching mol ratio is: n (urea): n (sulfuric acid)=(0～4): 1, n (urea): n (nitric acid)=(0～3): 1, n (urea): n (phosphoric acid)=(0～3): 1, n (urea): n (hydrochloric acid)=(0～5): 1.
6. preparation method claimed in claim 2, is characterized in that material is 50～130 ℃ of reactor temperature of reaction.
7. preparation method claimed in claim 2, is characterized in that material is at reactor reaction times 0.5～5h.
8. method claimed in claim 6, is characterized in that reactor at room temperature continues slaking 0.5～8h after reaction for some time.Make nitrogen-phosphorus-potassium compound fertilizer.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481506A (en) * | 2015-12-22 | 2016-04-13 | 成都新柯力化工科技有限公司 | Method for preparing novel composite fertilizer combining quick-acting property with long-acting property by taking minerals as raw materials |
| CN106631284A (en) * | 2017-01-04 | 2017-05-10 | 山西农业大学 | Preparation method of citrate-soluble potassium inorganic compound fertilizer |
| 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 |
| CN108558556A (en) * | 2018-07-04 | 2018-09-21 | 郑州大学 | A method of preparing particle urea groups composite fertilizer with urea-sulfuric acid decomposing rock phosphate with hydrogen |
| CN109593003A (en) * | 2019-01-31 | 2019-04-09 | 云南云天化以化磷业研究技术有限公司 | A kind of production method improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer |
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2012
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| CN1138567A (en) * | 1996-03-19 | 1996-12-25 | 化学工业部长沙化学矿山设计研究院 | Wetting decomposition process of potash feldspar ore |
| CN101225008A (en) * | 2007-10-30 | 2008-07-23 | 陈慧珍 | Production technology of controlled release multiple-effect fertilizer |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481506A (en) * | 2015-12-22 | 2016-04-13 | 成都新柯力化工科技有限公司 | Method for preparing novel composite fertilizer combining quick-acting property with long-acting property by taking minerals as raw materials |
| CN106631284A (en) * | 2017-01-04 | 2017-05-10 | 山西农业大学 | Preparation method of citrate-soluble potassium inorganic compound fertilizer |
| 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 |
| CN108558556A (en) * | 2018-07-04 | 2018-09-21 | 郑州大学 | A method of preparing particle urea groups composite fertilizer with urea-sulfuric acid decomposing rock phosphate with hydrogen |
| CN109593003A (en) * | 2019-01-31 | 2019-04-09 | 云南云天化以化磷业研究技术有限公司 | A kind of production method improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer |
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Application publication date: 20140212 |