CN103274815A - Preparation method of water-soluble silicon-potassium fertilizer - Google Patents
Preparation method of water-soluble silicon-potassium fertilizer Download PDFInfo
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- potash fertilizer
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Abstract
The invention aims at providing a preparation method of a water-soluble silicon-potassium fertilizer which takes rich reserves of potassium feldspar and silica as materials and has high fertilizer use ratio through converting contained insoluble potassium and silicon components to water-soluble components so as to slowly release in soil. According to the preparation method, the technical scheme for solving the technical problem is that a method for preparing the silicon-potassium fertilizer comprises the following steps of: step one, mixing with ammonium hydrogen carbonate after crushing potassium feldspar ore and silica mining, putting the mixture in water to stir, processing for 2-5 hours under certain reaction temperature and pressure in the presence of a catalyst; and step two, adding proper amount of KOH in the solution, stirring for 1-3 hours at normal temperature, stopping stirring until the pH value is 6-7 to obtain the water-soluble silicon-potassium fertilizer, concentrating or drying to granulate.
Description
Invention field
The present invention relates to a kind of preparation method of water-soluble silicon potash fertilizer, belong to the agrochemistry category.
Background technology
In the most of area of China, soil potassium deficiency phenomenon has become the main restricting factor of increasing crop yield.According to national soil survey information, China has 70% arable land potassium deficiency approximately, wherein 45% arable land severe potassium deficiency.As the soluble potassium ore resources of producing the potash fertilizer main raw material, few and distributed pole is unbalanced at China's reserves.The throughput of present domestic potash fertilizer can not satisfy the demands far away, therefore domestic potash fertilizer overwhelming majority dependence on import.
China's soluble potassium salt ore deposit reserve seldom only accounts for 0.66% of world saving.But the insoluble potassium ore resources of China is abundant, and is of a great variety, mainly contains potassium felspar sand, white garnet, alunite, illite, potassium-bearing shale and all kinds of potassium matter volcanics etc.These potassium ore resources almost spread all over the country each province, city autonomous region.According to incompletely statistics, national insoluble potassium resource has nearly 10,000,000,000 tons approximately.Therefore, utilizing insoluble potassium ore deposit to carry potassium is the new way of producing potash fertilizer.
Traditional method is as raw material with potassium, the ash that many use plants burn till or the natural mineral matter that contains potassium, but the conversion that appears at the sodium that contains in the natural mineral matter is difficult, the phenomenon of plant absorbing potassium difficulty, and used vitriolate of tartar, the Repone K for preparing with chemical mode again.
From the whole nation, because China's refractory potassic mine resource is abundanter, especially the insoluble potassium resource reserves based on potassium felspar sand are big, distribution is wide, and be distributed in China middle part and agricultural developed regions, east more, thereby utilize insoluble potassium resources such as potassium felspar sand as raw material, carry out the extracting potassium from potash feldspar technical study, produce potash fertilizer and composite fertilizer, have important economy and strategic importance.
Potassium felspar sand (potash feldspar) is a kind of shape structure silicate minerals, is KAlSi
3O
8The general name of 3 polymorph sanidines, potash feldspar and microlines.Its mineral theoretical content is K
2O16.9%, Al
2O
318.4%, SiO
264.7%.The standard weave unit is sial oxygen tetrahedron in its structure, and 4 tetrahedrons are total to the top, angle and form the tetrad ring, are total to the continuous chain that becomes the bent axle shape in top, angle between the tetrad ring each other, and interchain links to each other with bridging oxygen and forms three-dimensional frame shape structure.Because Si
4+By Al
3+Part replaces and the negative charge residue occurs, needs network-modifier cation such as K
+The effect of balancing charge is played in filling in the interannular space.Measure according to Molecular Orbital Calculation and sosoloid thermodynamics, because the polarized action of oxo bridge causes the sial oxygen tetrahedron character of feldspar highly stable, except the vitriol oil, hydrofluoric acid, decomposed by any acid, alkali hardly under the normal temperature and pressure.These compositions and the constructional feature of potassium felspar sand had both determined to add suitable fusing assistant to reduce Technology characteristic such as temperature of reaction in its decomposition reaction, also determined multipath and the feasible direction of utilizing of its comprehensive utilization.In addition, the aluminium in the potassium felspar sand and silicon are all formed the coordination tetrahedron with oxygen, form firm tetrahedral network structure, and its chemical property stabilizer pole is not decomposed by any soda acid except hydrofluoric acid under the normal temperature.But have bigger space in the potassium felspar sand structure significantly, under certain conditions, Ca
2+, Na
+Deng the network-modifying ion K that can replace in the potassium felspar sand structure
+
Early stage extracting potassium from potash feldspar technology is mainly thermal decomposition method.There is more scholar that it is studied, chosen multiple auxiliary agent and optimized the kinds of processes condition.Specifically can be divided into: high-temperature sintering process, blast-furnace smelting method, press hot method, hot legal system water-soluble potassium, low-temperature decomposition method, low temperature acid decomposition, microbial method etc.But the whole bag of tricks is not that temperature is too high, energy consumption is big, is exactly that operational path is numerous and diverse, and equipment requirements is also too high, thereby does not have industrial value.For example, high-temperature sintering process, blast-furnace smelting method, the hot method of pressure etc. are applicable to that under the high temperature (1600 degree) of producing various potassic fertilizers, the potassic fertilizer of production is because existing the shortcoming of high energy consumption and high production cost etc.At present, domestic also have some to utilize insoluble potassium ore deposit to put forward the new achievement in research of potassium, but because these method ubiquities reasons such as technical process is long, investment is big, energy consumption is high, product cost is high, tailings is many, deficiency in economic performance, and quality is low, can not implement to promote, and have no chance with potash fertilizer market.
And with more than contain potassium fertilizer, when long-term fertilization, the phenomenon of soil acidityization appears easily, therefore be badly in need of wanting a kind of new for from potassium felspar sand, extracting the method for active potassium.
Siliceous fertilizer is a kind of to contain the water-soluble mineral manure of Calucium Silicate powder, has features such as nonpoisonous and tasteless nothing corrosion and difficult loss, is the required important nutritive element of plant.Experimental study shows that siliceous fertilizer has important effect to the growth of farm crop such as paddy rice, wheat, corn, cotton, peanut, soybean, oil honor, sugarcane, potato class, fruit tree.In China, be that the soil in a lot of areas lacks silicon on the one hand, as the scarce silicon of the soil of the Yangtze valley 70%, the Yellow River and Huai He River sea region and Liaoning have the soil of half to lack silicon approximately, and the zone that lacks silicon is also progressively enlarging.Be that people are not enough to the effect understanding of siliceous fertilizer in crop growth on the other hand, the throughput less investment of siliceous fertilizer yields poorly, siliceous fertilizer is not added in the farmland substantially for many years, growth to farm crop is very unfavorable, and particularly the serious acid soil that lacks silicon in south is very unfavorable to the growth of paddy rice.And the production of siliceous fertilizer is in the ground zero stage in China, at present is mostly to utilize to have the active scrap silicon production that contains, as yellow phosphorus slag, waste steel slag.Siliceous fertilizer with these raw material production is single siliceous fertilizer, and solubility is not high, and fertilizer efficiency is also lower.The potassium ore resources shortage of the solubility of be directly used in the productions potash fertilizer that exists at the fertilizer production technology field, the demand of potash fertilizer soil big and vast region need replenish siliceous fertilizer, and the output of present siliceous fertilizer is low.
In order to overcome the defective of above-mentioned prior art, the applicant has proposed to prepare from potassium felspar sand, silica a kind of method of water-soluble silicon potash fertilizer after the physico-chemical property to potassium felspar sand, silica has carried out further investigation.
Summary of the invention
The object of the invention provide a kind of with reserves very abundant and again very cheap potassium felspar sand, silica be raw material, be converted into water soluble component by the insoluble potassium that it is contained, silicon composition, in soil, can slowly discharge, have the Si-K fertilizer preparation method of higher utilization rate of fertilizer.
Therefore, the present invention is in order to solve the problem that above prior art produces, a kind of method for preparing water-soluble silicon potash fertilizer to be provided.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of method for preparing water-soluble silicon potash fertilizer fertilizer, and it may further comprise the steps:
Step 1, potassium felspar sand ore, silica mine are pulverized the back mix, mix with bicarbonate of ammonia, insert in the water and stir, under catalyzer, under certain temperature of reaction and pressure, handled 2-5 hour;
Step 2, in above-mentioned solution, add an amount of KOH, stirred at normal temperatures 1-3 hour, stop stirring until pH value during for 6-7, obtain water-soluble silicon potash fertilizer, concentrated or drying and granulating.
On the basis of technique scheme, the present invention can also do further restriction:
Further, in the described step 1 potash feldspar ore and silica mine pulverizing are 4-125 purpose size.
Further, be 1 with the weight ratio of potash feldspar ore and silica mine in the described step 1: 0.2-0.5.
Further, the weight ratio of potassium felspar sand breeze and bicarbonate of ammonia is 1: 0.5～5 in the described step 1.
Further, the weight ratio of amount of water and potassium felspar sand breeze is 1-10 in the described step 1: 1.
Further, catalyzer is cupric chloride or iron protochloride in the described step 1, preferred iron protochloride, and its consumption is the 0.02-0.2% of potash feldspar ore grain weight amount.
Further, temperature of reaction is 300～750 ℃ in the described step 1.
Further, pressure is 5～20 normal atmosphere in the described step 1.
Further, normal temperature is 15-35 ℃ in the described step 2.
According to a kind of method of extracting water-soluble silicon potash fertilizer from potassium felspar sand, silica of the present invention, the described product that contains water-soluble silicon potash fertilizer can be prepared as liquid fertilizer, also can be prepared as solid fertilizer.
According to a kind of method of from potassium felspar sand, silica, extracting water-soluble silicon potash fertilizer of the present invention, also contain by products such as silicon-dioxide in the described reaction product, these by products are inertia, stay soil and are conducive to loosing soil, execute in the soil and also can not destroy soil.
According to a kind of method of from potassium felspar sand, extracting active potassium of the present invention, the utilization ratio of potassium 〉=90% in the potassium felspar sand wherein, the utilization ratio of silicon 〉=30% in the silica, prepared high-concentration water-soluble silicon potassium compound fertilizer, total nutrient 〉=70% is taller more a lot of than the total nutrient 40% of GB-15063-94 regulation.
According to according to a kind of method of from potassium felspar sand, silica, extracting water-soluble silicon potash fertilizer of the present invention, in the arable soil that lacks potassium, use the fertilizer fertilising of method preparation of the present invention in soil, not only solved the problem of Si-K fertilizer material existence in the past, and can high density be dissolved in the soil, continue, forever improve the effect of soil.
And the method for the invention is not brought environmental pollution, environmental protection in implementation process.
Embodiment
The present invention can reference example illustrate that with following embodiment it is including but not limited to this.
The employed potassium felspar sand of the embodiment of the invention is provided by Guizhou Province's Tongren City enterprise, pick up from Wanshan Mountain district, be flesh pink, testing used breeze forms by potash feldspar tailings is treated, full potassium content is 15.2% in the used breeze, silicon oxide-containing 65.2%, trioxygen-containingization two aluminium 19.6%, 1163 ℃ of fusing points, density are 2.55g/cm
3The embodiment of the invention is employed to be provided by Guizhou Province's Tongren City enterprise, picks up from Wanshan Mountain district, and the content of silica is about 98.5%, also contains oxide compounds such as micro-iron, aluminium, chromium, is Steel Gray.
Obtain water-soluble silicon potash fertilizer with present method, sampling analysis potassium content from solution, calculate the potassium rate of putting forward:
Potassium content (quality) * 100% in potassium content (quality)/potassium felspar sand in the utilization ratio of potassium=water-soluble silicon potash fertilizer;
Obtain water-soluble silicon potash fertilizer with present method, sampling analysis silicone content from solution, calculate the potassium rate of putting forward:
Silicone content (quality) * 100% in silicone content (quality)/silica in the utilization ratio of silicon=water-soluble silicon potash fertilizer.
The method of extracting water-soluble silicon potash fertilizer with three the present invention of embodiment from potassium felspar sand, silica is done further detailed description below.
Embodiment 1:
With potassium felspar sand 200g, silica 40g be broken into breeze, to cross 125 mesh sieves standby, in reactor, add bicarbonate of ammonia 100g, add 200g water simultaneously and stir, add iron protochloride 0.4g simultaneously, be that pressure is to react 2h under 5 normal atmosphere under 300 ℃ the temperature in temperature.
Adding an amount of KOH in above-mentioned solution, stirred at normal temperatures 1 hour, is to stop stirring at 6 o'clock to obtain water-soluble silicon potash fertilizer until pH value.
Also drying and granulating after the water-soluble silicon potash fertilizer solution concentration can be obtained finished product.
The potassium rate of carrying of extracting water-soluble potassium through present embodiment 1 from potassium felspar sand is 90.3%.
The silicon rate of carrying of extracting water-soluble silicon through present embodiment 1 from silica is 31.2%.
Embodiment 2:
With potassium felspar sand 200g, silica 100g be broken into breeze, to cross 4 mesh sieves standby, in reactor, add bicarbonate of ammonia 200g, add 500g water simultaneously and stir, add iron protochloride 0.1g simultaneously, be that pressure is to react 5h under 20 normal atmosphere under 750 ℃ the temperature in temperature.
Adding an amount of KOH in above-mentioned solution, stirred at normal temperatures 3 hours, is to stop to stir in 7 o'clock obtaining water-soluble silicon potash fertilizer until pH value, and concentrating afterwards, drying and granulating obtains finished product.
The potassium rate of carrying of extracting water-soluble potassium through present embodiment 2 from potassium felspar sand is 91.5%.
The silicon rate of carrying of extracting water-soluble silicon through present embodiment 2 from silica is 33.9%.
Embodiment 3:
With potassium felspar sand 200g, silica 60g be broken into breeze, to cross 50 mesh sieves standby, in reactor, add bicarbonate of ammonia 1000g, add 1000g water simultaneously and stir, add iron protochloride 0.2g simultaneously, be that pressure is to react 3h under 10 normal atmosphere under 400 ℃ the temperature in temperature.
Adding an amount of KOH in above-mentioned solution, stirred at normal temperatures 2 hours, is to stop to stir in 6.5 o'clock obtaining water-soluble silicon potash fertilizer until pH value, and concentrating afterwards, drying and granulating obtains finished product.
The potassium rate of carrying of extracting water-soluble potassium through present embodiment 3 from potassium felspar sand is 91.2%.
The silicon rate of carrying of extracting water-soluble silicon through present embodiment 3 from silica is 32.8%.
Below be the result of use of fertilizer of the present invention, the contrast plot all is located at the field of test plot periphery equal conditions.
Embodiment 4:
The test kind: potato,
Test period, place: Chifeng, the Inner Mongol in 2012.
The mu fertilising of test plot: homemade diamines 10Kg urea 3Kg Si-K fertilizer 2Kg of the present invention,
Contrast plot mu fertilising: homemade diamines 10Kg urea 3Kg potash fertilizer 3Kg.
Test plot disease and pest situation: seedling is neat, seedling is strong, and potato seedling look dark green, and no disease and pest takes place,
Test plot disease and pest situation: disease all takes place in the potato seedling, and the potato seedling is withered and yellow, and growing way is poor.
Test plot per mu yield: 1236 kilograms,
Contrast plot per mu yield: 985 kilograms.
Embodiment 5:
The test kind: paddy rice,
Test period, place: Heilungkiang Nehe in 2012.
The mu fertilising of test plot: homemade diamines 15Kg urea 9Kg Si-K fertilizer 5Kg of the present invention,
Contrast plot mu fertilising: homemade diamines 15Kg urea 9Kg potash fertilizer 7Kg.
Test plot disease and pest situation: the paddy rice stalk is sturdy, and fringe is big, and no disease and pest takes place,
Test plot disease and pest situation: disease and pest in various degree occurs, the paddy rice stalk is thin, fringe is little, owes ripe.
Test plot per mu yield: 650 kilograms,
Contrast plot per mu yield: 510 kilograms.
Above-mentioned test shows, uses Si-K fertilizer of the present invention and can obviously improve the per mu yield of farm crop, and effect is remarkable, is worth big area to be promoted and use.
Claims (10)
1. a water-soluble silicon potash fertilizer fertilizer is characterized in that described water-soluble silicon potash fertilizer fertilizer can be liquid fertilizer, also can be solid fertilizer.
2. method for preparing water-soluble silicon potash fertilizer fertilizer, it may further comprise the steps:
Step 1, potassium felspar sand ore, silica mine are pulverized the back mix, mix with bicarbonate of ammonia, insert in the water and stir, under catalyzer, under certain temperature of reaction and pressure, handled 2-5 hour;
Step 2, in above-mentioned solution, add an amount of KOH, stirred at normal temperatures 1-3 hour, stop stirring until pH value during for 6-7, obtain water-soluble silicon potash fertilizer, concentrated or drying and granulating.
3. according to the described method for preparing water-soluble silicon potash fertilizer fertilizer of claim 2, in the wherein said step 1 potash feldspar ore and silica mine pulverizing are 4-125 purpose size.
4. according to the described method for preparing water-soluble silicon potash fertilizer fertilizer of claim 2, be 1 with the weight ratio of potash feldspar ore and silica mine in the step 1 wherein: 0.2-0.5.
5. according to the described method for preparing water-soluble silicon potash fertilizer fertilizer of claim 2, the weight ratio of potassium felspar sand breeze and bicarbonate of ammonia is 1: 0.5～5 in the wherein said step 1.
6. according to the described method for preparing water-soluble silicon potash fertilizer fertilizer of claim 2, the weight ratio of amount of water and potassium felspar sand breeze is 1-10 in the wherein said step 1: 1.
7. according to the described method for preparing water-soluble silicon potash fertilizer fertilizer of claim 2, catalyzer is cupric chloride or iron protochloride in the wherein said step 1, preferred iron protochloride, and its consumption is the 0.02-0.2% of potash feldspar ore grain weight amount.
8. according to the described method for preparing water-soluble silicon potash fertilizer fertilizer of claim 1, temperature of reaction is 300～750 ℃ in the wherein said step 1.
9. according to the described method for preparing water-soluble silicon potash fertilizer fertilizer of claim 2, pressure is 5～20 normal atmosphere in the wherein said step 1.
10. according to the described method for preparing water-soluble silicon potash fertilizer fertilizer of claim 2, normal temperature is 15-35 ℃ in the wherein said step 2.
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Cited By (7)
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|---|---|---|---|---|
| CN103864496A (en) * | 2014-02-26 | 2014-06-18 | 化工部长沙设计研究院 | Technology for preparing potash fertilizer with potash feldspar |
| CN103880481A (en) * | 2014-03-07 | 2014-06-25 | 佛山市健地农业科技有限公司 | Fully-dissolvable silicon-based compound fertilizer and preparation method thereof |
| CN104649784A (en) * | 2015-02-09 | 2015-05-27 | 山西大学 | Method for preparing silicon-potash fertilizer based on magnesium slag |
| CN109912369A (en) * | 2019-04-26 | 2019-06-21 | 珠海三豫环保新材料科技有限公司 | A kind of formula and preparation method thereof preparing Si-K fertilizer using gangue |
| CN110183268A (en) * | 2019-05-21 | 2019-08-30 | 滁州市给力肥料科技有限公司 | A kind of preparation method of high-concentration liquid silicon fertilizer |
| CN111116241A (en) * | 2019-08-02 | 2020-05-08 | 陈桂芳 | Method for preparing fully water-soluble silicon fertilizer from silicon ore |
| CN111170766A (en) * | 2019-12-28 | 2020-05-19 | 张锋 | Production method of silicon-potassium fertilizer |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864496A (en) * | 2014-02-26 | 2014-06-18 | 化工部长沙设计研究院 | Technology for preparing potash fertilizer with potash feldspar |
| CN103864496B (en) * | 2014-02-26 | 2016-03-09 | 化工部长沙设计研究院 | The technique of potash fertilizer prepared by a kind of potassium felspar sand |
| CN103880481A (en) * | 2014-03-07 | 2014-06-25 | 佛山市健地农业科技有限公司 | Fully-dissolvable silicon-based compound fertilizer and preparation method thereof |
| CN103880481B (en) * | 2014-03-07 | 2016-08-10 | 佛山市健地农业科技有限公司 | A kind of complete silica-based multi-component composite fertilizer of dissolubility and preparation method thereof |
| CN104649784A (en) * | 2015-02-09 | 2015-05-27 | 山西大学 | Method for preparing silicon-potash fertilizer based on magnesium slag |
| CN104649784B (en) * | 2015-02-09 | 2017-06-23 | 山西大学 | A kind of method that Si-K fertilizer is prepared based on magnesium slag |
| CN109912369A (en) * | 2019-04-26 | 2019-06-21 | 珠海三豫环保新材料科技有限公司 | A kind of formula and preparation method thereof preparing Si-K fertilizer using gangue |
| CN110183268A (en) * | 2019-05-21 | 2019-08-30 | 滁州市给力肥料科技有限公司 | A kind of preparation method of high-concentration liquid silicon fertilizer |
| CN111116241A (en) * | 2019-08-02 | 2020-05-08 | 陈桂芳 | Method for preparing fully water-soluble silicon fertilizer from silicon ore |
| CN111170766A (en) * | 2019-12-28 | 2020-05-19 | 张锋 | Production method of silicon-potassium fertilizer |
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