CN105712778A - Method for preparing compound fertilizer by low-temperature ultrasonic hydrothermal process - Google Patents
Method for preparing compound fertilizer by low-temperature ultrasonic hydrothermal process Download PDFInfo
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- CN105712778A CN105712778A CN201610285602.5A CN201610285602A CN105712778A CN 105712778 A CN105712778 A CN 105712778A CN 201610285602 A CN201610285602 A CN 201610285602A CN 105712778 A CN105712778 A CN 105712778A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B11/00—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
- C05B11/02—Pretreatment
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Abstract
The invention discloses a method for preparing a compound fertilizer by a low-temperature ultrasonic hydrothermal process. The method comprises the following steps: 1) ore pretreatment: respectively carrying out crushing, iron removal, screening and pulverization on potash feldspar and apatite, adding a hydrothermal reaction aid to obtain a mixture, and grinding the mixture to the particle size of less than 1000 mu m, thereby generating a crude material for later use; 2) ultrasonic hydrothermal desilication: adding the crude material, an ammonium salt and water into a hydrothermal reaction kettle while being assisted by 300-500W ultrasonic, carrying out reaction at 80-150 DEG C for 0.5-2 hours, and carrying out vacuum filtration on the reaction product to obtain clinker; and 3) hydrothermal acid leaching: adding sulfuric acid into the powder, continuing curing at 60-120 DEG C for 10-40 minutes, filtering, washing and drying to obtain the potassium/phosphorus/nitrogen-containing compound fertilizer. The method has the characteristics of simple preparation technique, high efficiency, low cost and excellent product performance, and is beneficial to high-efficiency industrial production of the potassium/phosphorus/nitrogen compound fertilizer.
Description
[technical field]
The comprehensive high-efficiency that the present invention relates to mineral resources utilizes, a kind of method preparing compound fertilizer particularly to low temperature ultrasonic hydro-thermal.
[background technology]
Potassium element is one of three big elements determining agricultural high yield, but the nitrogen of China's soil, phosphorus, potassium serious disproportion, potash fertilizer
Proportion is too low, and utilization rate is the lowest, and how natural potassium feldspar being converted into soluble potassium salt is key point.Potassium feldspar develops
It is crucial that on the premise of the aspect sustainable developments such as economy, environment and resource, use various method to destroy potassium to greatest extent long
The stability structure of stone, makes K+Dissolution, decomposes the kalium contained mineral such as potassium feldspar so that it is in natural minerals potassium be changed into water solublity
Potassium compound.Main method includes: high-temperature roasting method, low temperature fluorine system method, microbial method and hydro-thermal method etc. are several.Patent " profit
The method producing coproduction of potassium sulfate calcium and magnesium phosphorus silicon composite fertilizer with potassium feldspar " use the potassium of 1150 DEG C～the 1250 DEG C certain proportionings of high-temperature calcination
The mixture of Anhydrite, Gypsum Fibrosum, apatite, cadmia and dolomite prepares compound fertilizer.Patent " producing compound fertilizer by wet decomposing potassium feldspar
Method " use hexafluosilicic acid system to process potassium feldspar under the conditions of 97-100 DEG C and prepare potassium sulfate in 2-4 hour, although reducing instead
Answer system temperature, but environmental pollution is the most serious.Microbial decomposition technology is to utilize microorganism fungus kind, with potassium feldspar, biochemistry occurs
Reaction carrys out decomposing of potassium feldspar, although energy consumption is low, pollutes little, but it is oversize to there is the spawn culture cycle, and decomposition rate is slow, survival ability
More weak, the unfavorable factors such as Potassium leaching rate is low.
[summary of the invention]
It is an object of the invention to provide a kind of method that low temperature ultrasonic hydro-thermal prepares compound fertilizer, the method has that technique is simple, efficiency
The features such as height, low cost, excellent product performance.
The present invention is to be achieved through the following technical solutions:
A kind of method that low temperature ultrasonic hydro-thermal prepares compound fertilizer, comprises the following steps:
1) Ore pretreatment: first by potassium feldspar, apatite respectively broken, except ferrum, screening and pulverizing, and add hydro-thermal reaction and help
Agent, after mix, further pulverizing, is milled to particle diameter ＜ 1000 μm, obtains raw material；Wherein, according to percetage by weight, potassium is long
Stone 72～85%, apatite 10～24%, hydro-thermal reaction auxiliary agent 4～6%；
2) supersonic, water-heating desiliconization: join in hydrothermal reaction kettle by raw material, water and ammonium salt, uses ultrasonic transducer to assist
Ultrasonic, at ultrasonic power 300-500W, under the conditions of temperature 80-150 DEG C, carry out hydro-thermal reaction, make the silicon source in potassium feldspar with SiO3 2-
Form completely out, product sucking filtration is obtained grog；Wherein, the weight ratio of raw material, water and ammonium salt is (60～80): (45～55):
(1～1.5)；
3) hydro-thermal Acid leaching: add sulphuric acid in grog, grog is (2～3) with the weight ratio of sulphuric acid: 1, is 60-120 DEG C in temperature
Under the conditions of, it is filtered, washed and dried after continuing ripening 10-40min, prepares the compound fertilizer containing potassium phosphorus nitrogen.
Described hydro-thermal reaction auxiliary agent is the mixture of one or more in CaO, MgO and NaO.
Described ammonia salt is ammonium chloride, ammonium hydrogen carbonate or ammonium nitrate.
The packing ratio of described hydrothermal reaction kettle is 40～60%.
The mass concentration of described sulphuric acid is 90%.
The described hydro-thermal reaction time is 0.5-2h.
Compared with prior art, the present invention has a following useful technique effect:
The present invention, with natural minerals potassium feldspar and apatite as raw material, extracts soluble potassium, introduces hydro-thermal auxiliary agent and accelerates potassium feldspar knot
The destruction of structure, can effectively accelerate the reaction process of potassium feldspar and apatite, promotes the carrying out of desilication reaction, and makes full use of super
Sound hydrothermal technique, at a lower temperature with in the short period, prepares compound fertilizer, improves decomposition efficiency, increase productivity.By ultrasonic
Combine with hydrothermal technique and activity except pasc reaction is greatly improved in potassium feldspar structure, by system reaction temperature from 220～280 DEG C
It is reduced to 80-150 DEG C.Acid leaching can reduce reaction temperature and shorten the response time simultaneously under hydrothermal conditions.In sum, this
Bright have that preparation technology is simple, efficiency is high, the feature of low cost, excellent product performance, the beneficially efficient work of potassium phosphorus nitrogen composite fertilizer
Industry metaplasia is produced.
[detailed description of the invention]
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Embodiment 1
A kind of method that low temperature ultrasonic hydro-thermal prepares compound fertilizer, comprises the following steps:
1) by potassium feldspar and apatite grinding after broken and ore dressing pretreatment, according to 85 parts of potassium feldspars, 10 parts of apatite and 5
The weight ratio of part calcium oxide hydro-thermal auxiliary agent, mixing is milled to particle diameter further is ＜ 1000 μm, becomes raw material, standby.
2) being added to the water by ammonium chloride, join in hydrothermal reaction kettle by raw material subsequently, the weight portion of raw material, water and ammonium salt is
60 parts, 45 parts and 1 part；Assisting ultrasonic power is 300W, and controlling its packing ratio is 56%, anti-under the conditions of temperature is 100 DEG C
After answering 1.5h, sucking filtration powder.
3) using concentration is the sulphuric acid of 90%, and grog is 2:1 with the weight ratio of sulphuric acid, and in hydrothermal reaction kettle, 60 DEG C are continued ripening
After 40min, it is filtered, washed and dried the compound fertilizer prepared containing potassium phosphorus nitrogen.
Embodiment 2
A kind of method that low temperature ultrasonic hydro-thermal prepares compound fertilizer, comprises the following steps:
1) by potassium feldspar and apatite grinding after broken and ore dressing pretreatment, according to 82 parts of potassium feldspars, 14 parts of apatite and 4
The weight ratio of part calcium oxide hydro-thermal auxiliary agent, mixing is milled to particle diameter further is ＜ 1000 μm, becomes raw material, standby.
2) being added to the water by ammonium chloride, join in hydrothermal reaction kettle by raw material subsequently, the weight portion of raw material, water and ammonium salt is
80 parts, 55 parts and 1.5 parts, assisting ultrasonic power is 420W, and controlling its packing ratio is 52%, under the conditions of temperature is 120 DEG C
After reaction 1.2h, sucking filtration powder.
3) using concentration is the sulphuric acid of 90%, and grog is 3:1 with the weight ratio of sulphuric acid, and in hydrothermal reaction kettle, 70 DEG C are continued ripening
After 35min, it is filtered, washed and dried the compound fertilizer prepared containing potassium phosphorus nitrogen.
Embodiment 3
A kind of method that low temperature ultrasonic hydro-thermal prepares compound fertilizer, comprises the following steps:
1) by potassium feldspar and apatite grinding after broken and ore dressing pretreatment, according to 78 parts of potassium feldspars, 18 parts of apatite and 4
The weight ratio of part calcium oxide hydro-thermal auxiliary agent, mixing is milled to particle diameter further is ＜ 1000 μm, becomes raw material, standby.
2) being added to the water by ammonium chloride, join in hydrothermal reaction kettle by raw material subsequently, the weight ratio of raw material, water and ammonium salt is
70:50:1.3；Assisting ultrasonic power is 400W, and controlling its packing ratio is 50%, after reacting 1.0h under the conditions of temperature is 140 DEG C,
Sucking filtration powder.
3) using concentration is the sulphuric acid of 90%, and grog is (2～3) with the weight ratio of sulphuric acid: 1, and grog with the weight ratio of sulphuric acid is
2.5:1, in hydrothermal reaction kettle after 80 DEG C of continuation ripening 30min, is filtered, washed and dried the compound fertilizer prepared containing potassium phosphorus nitrogen.
Embodiment 4
A kind of method that low temperature ultrasonic hydro-thermal prepares compound fertilizer, comprises the following steps:
1) by potassium feldspar and apatite grinding after broken and ore dressing pretreatment, according to 75 parts of potassium feldspars, 20 parts of apatite and 5
The weight ratio of part NaO and CaO hydro-thermal auxiliary agent, mixing is milled to particle diameter further is ＜ 1000 μm, becomes raw material, standby.
2) being added to the water by ammonium chloride, join in hydrothermal reaction kettle by raw material subsequently, the weight ratio of raw material, water and ammonium salt is
60:44:1；Assisting ultrasonic power is 380W, and controlling its packing ratio is 48%, after reacting 0.8h, takes out under the conditions of temperature is 150 DEG C
Filter powder.
3) using concentration is the sulphuric acid of 90%, and grog is 3:1 with the weight ratio of sulphuric acid, and in hydrothermal reaction kettle, 90 DEG C are continued ripening
After 25min, it is filtered, washed and dried the compound fertilizer prepared containing potassium phosphorus nitrogen.
Embodiment 5
A kind of method that low temperature ultrasonic hydro-thermal prepares compound fertilizer, comprises the following steps:
1) by potassium feldspar and apatite grinding after broken and ore dressing pretreatment, according to 72 parts of potassium feldspars, 24 parts of apatite and 6
The weight ratio of part MgO hydro-thermal auxiliary agent, mixing is milled to particle diameter further is ＜ 1000 μm, becomes raw material, standby.
2) being added to the water by ammonium nitrate, join in hydrothermal reaction kettle by raw material subsequently, the weight ratio of raw material, water and ammonium salt is
75:50:1.5；Assisting ultrasonic power is 330W, and controlling its packing ratio is 45%, after reacting 0.5h under the conditions of temperature is 150 DEG C,
Sucking filtration powder.
3) using concentration is the sulphuric acid of 90%, and grog is 2.5:1 with the weight ratio of sulphuric acid, and in hydrothermal reaction kettle, 95 DEG C of continuation are ripe
After changing 20min, it is filtered, washed and dried the compound fertilizer prepared containing potassium phosphorus nitrogen.
Embodiment 6
A kind of method that low temperature ultrasonic hydro-thermal prepares compound fertilizer, comprises the following steps:
1) by potassium feldspar and apatite grinding after broken and ore dressing pretreatment, according to 80 parts of potassium feldspars, 16 parts of apatite and 4
The weight ratio of part calcium oxide hydro-thermal auxiliary agent, mixing is milled to particle diameter further is ＜ 1000 μm, becomes raw material, standby.
2) ammonium hydrogen carbonate is added to the water, subsequently raw material is joined in hydrothermal reaction kettle, the weight ratio of raw material, water and ammonium salt
For 60:55:1；Assisting ultrasonic power is 500W, and controlling its packing ratio is 45%, after reacting 2h, takes out under the conditions of temperature is 80 DEG C
Filter powder.
3) using concentration is the sulphuric acid of 90%, and grog is 3:1 with the weight ratio of sulphuric acid, and in hydrothermal reaction kettle, 120 DEG C of continuation are ripe
After changing 10min, it is filtered, washed and dried the compound fertilizer prepared containing potassium phosphorus nitrogen.
In sum, present invention introduces hydro-thermal auxiliary agent and accelerate potassium feldspar structural damage, promote the carrying out of desilication reaction, and fill
Divide and utilize supersonic, water-heating technology, at a lower temperature with in the short period, prepare compound fertilizer.
Above said content is to combine concrete preferred implementation further description made for the present invention, is not all of or only
The embodiment of one, it is any etc. that technical solution of the present invention is taked by those of ordinary skill in the art by reading description of the invention
The conversion of effect, the claim being the present invention is contained.
Claims (6)
1. the method that a low temperature ultrasonic hydro-thermal prepares compound fertilizer, it is characterised in that comprise the following steps:
1) Ore pretreatment: first by potassium feldspar, apatite respectively broken, except ferrum, screening and pulverizing, and add hydro-thermal reaction and help
Agent, after mix, further pulverizing, is milled to particle diameter ＜ 1000 μm, obtains raw material；Wherein, according to percetage by weight, potassium is long
Stone 72～85%, apatite 10～24%, hydro-thermal reaction auxiliary agent 4～6%；
2) supersonic, water-heating desiliconization: join in hydrothermal reaction kettle by raw material, water and ammonium salt, uses ultrasonic transducer to assist
Ultrasonic, at ultrasonic power 300-500W, under the conditions of temperature 80-150 DEG C, carry out hydro-thermal reaction, make the silicon source in potassium feldspar with SiO3 2-
Form completely out, product sucking filtration is obtained grog；Wherein, the weight ratio of raw material, water and ammonium salt is (60～80): (45～55):
(1～1.5)；
3) hydro-thermal Acid leaching: add sulphuric acid in grog, grog is (2～3) with the weight ratio of sulphuric acid: 1, is 60-120 DEG C in temperature
Under the conditions of, it is filtered, washed and dried after continuing ripening 10-40min, prepares the compound fertilizer containing potassium phosphorus nitrogen.
The method that a kind of low temperature ultrasonic hydro-thermal the most according to claim 1 prepares compound fertilizer, it is characterised in that: described hydro-thermal
Reaction promoter is the mixture of one or more in CaO, MgO and NaO.
The method that a kind of low temperature ultrasonic hydro-thermal the most according to claim 1 prepares compound fertilizer, it is characterised in that: described ammonia salt
For ammonium chloride, ammonium hydrogen carbonate or ammonium nitrate.
The method that a kind of low temperature ultrasonic hydro-thermal the most according to claim 1 prepares compound fertilizer, it is characterised in that: described hydro-thermal
The packing ratio of reactor is 40～60%.
The method that a kind of low temperature ultrasonic hydro-thermal the most according to claim 1 prepares compound fertilizer, it is characterised in that: described sulphuric acid
Mass concentration be 90%.
The method that a kind of low temperature ultrasonic hydro-thermal the most according to claim 1 prepares compound fertilizer, it is characterised in that: described water
The thermal response time is 0.5-2h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610285602.5A CN105712778A (en) | 2016-04-29 | 2016-04-29 | Method for preparing compound fertilizer by low-temperature ultrasonic hydrothermal process |
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| CN201610285602.5A CN105712778A (en) | 2016-04-29 | 2016-04-29 | Method for preparing compound fertilizer by low-temperature ultrasonic hydrothermal process |
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| CN105712778A true CN105712778A (en) | 2016-06-29 |
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| CN201610285602.5A Pending CN105712778A (en) | 2016-04-29 | 2016-04-29 | Method for preparing compound fertilizer by low-temperature ultrasonic hydrothermal process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113583694A (en) * | 2021-08-02 | 2021-11-02 | 哈尔滨伟福和安科技有限责任公司 | Rapid hydrothermal degradation treatment method for crop straws |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432367A (en) * | 2011-09-21 | 2012-05-02 | 安徽华岳矿物材料有限公司 | Method for preparing mineral potash fertilizer with potassium feldspar |
| CN102603367A (en) * | 2012-03-05 | 2012-07-25 | 华南农业大学 | Physical and chemical comprehensive release promotion method of non-water-soluble potassium ore |
| CN104878197A (en) * | 2015-05-15 | 2015-09-02 | 龙岩学院 | Ultrasonic-assisted method for leaching potassium at low temperature under normal pressure |
| CN105084395A (en) * | 2015-08-05 | 2015-11-25 | 铜仁市万山区盛和矿业有限责任公司 | Method for producing soluble potassium through potassium feldspar |
-
2016
- 2016-04-29 CN CN201610285602.5A patent/CN105712778A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432367A (en) * | 2011-09-21 | 2012-05-02 | 安徽华岳矿物材料有限公司 | Method for preparing mineral potash fertilizer with potassium feldspar |
| CN102603367A (en) * | 2012-03-05 | 2012-07-25 | 华南农业大学 | Physical and chemical comprehensive release promotion method of non-water-soluble potassium ore |
| CN104878197A (en) * | 2015-05-15 | 2015-09-02 | 龙岩学院 | Ultrasonic-assisted method for leaching potassium at low temperature under normal pressure |
| CN105084395A (en) * | 2015-08-05 | 2015-11-25 | 铜仁市万山区盛和矿业有限责任公司 | Method for producing soluble potassium through potassium feldspar |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113583694A (en) * | 2021-08-02 | 2021-11-02 | 哈尔滨伟福和安科技有限责任公司 | Rapid hydrothermal degradation treatment method for crop straws |
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Application publication date: 20160629 |