CN104291295A - Method for preparing monopotassium phosphate and co-producing special compound fertilizer for highland barley - Google Patents
Method for preparing monopotassium phosphate and co-producing special compound fertilizer for highland barley Download PDFInfo
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- CN104291295A CN104291295A CN201410477846.4A CN201410477846A CN104291295A CN 104291295 A CN104291295 A CN 104291295A CN 201410477846 A CN201410477846 A CN 201410477846A CN 104291295 A CN104291295 A CN 104291295A
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Abstract
The invention discloses a method for preparing monopotassium phosphate and co-producing a special compound fertilizer for highland barley. The method comprises the following steps: carrying out a mixed reaction on raw materials; preparing monopotassium phosphate; and preparing the special compound fertilizer for highland barley. The purity of monopotassium phosphate prepared by the method is relatively high. The special compound fertilizer for highland barley is prepared by processing and adjusting the filtrate in the production process, thereby providing sufficient nutrition to normal growth of highland barley.
Description
Technical field
The present invention relates to technical field of fertilizer, be specifically related to a kind of method preparing potassium primary phosphate coproduction highland barley composite fertilizer special.
Background technology
Highland barley is a kind of cereal crop of Gramineae Hordeum, and because shell coetonium in it is separated, seed is exposed, therefore also known as hull-less barley, highland barley, meter great Mai.Mainly originating from the ground such as Tibet, China, Qinghai, Sichuan, Yunnan, is the main food of Tibetan people.Highland barley plants the history about having 4,000,000 years on Qinghai-Tibet Platean, extends to inspirit culture field among material and culture, Qinghai-Tibet Platean defines rich connotation, is rich in the culture of the highland barley of national characters.There is medicinal and nutritive value widely, be proposed the highland barley products such as highland barley fine dried noodles, highland barley steamed bun, barley nutritional powder.The growth of highland barley be unable to do without fertilizer, and highland barley is short for breeding time, and early stage is very responsive to nutrient requirement.According to this feature, highland barley requires that fertilizer will become thoroughly decomposed.Nitrogen, phosphorus, potassium three elements are joined to execute and are wanted science, and common fertilizer is after arable land applies, and a part is rising, dissipation and outflowing with water, and a part is fixed by soil and soil microorganisms and utilized, and only have a part wherein just absorbed by crops and utilize.Show after deliberation: the utilization ratio of urea, carbon ammonium is 20% one 46%, phosphate fertilizer (two ammoniums, an ammonium, coarse whiting) is 10% one 25%, potash fertilizer 45% one 60%.As can be seen here, common fertilizer utilization ratio is very low.For this reason, the present inventor is for the feature of highland barley and a kind of method preparing highland barley special fertilizer of the fertile characteristic research of happiness, need in a growth cycle of highland barley to absorb more nutritive substance, being not only nitrogen that common fertilizer provides, phosphorus, potassium, as lacked other nutrients, just can not growing by normal growth, plant slight of stature, ear uneven, pollination rate is low, has a strong impact on output.The present invention is the synthesis containing multiple nutrient, not the chemical fertilizer that nutrient is single, it is also rich in the required element of the crops such as zinc, iron, magnesium except the macronutrient such as nitrogenous, phosphorus, potassium, serving the effect regulating soil balanced nutrients, is a kind of new and effective no-pollution full nutrition chelating dedicated fertilizer.This special fertilizer be grow normally according to highland barley, cultivation feature, irrigate habit, prepared by the nutritive element of needs.Add various nutrient elements, protection highland barley is healthy, and fertility is more lasting, and effective regulating plant body defensive ability/resistance ability, alleviates disease, improves output.Greatly improve crop quality, improve the immunizing power of highland barley self, can well prevent highland barley regular incidence.
Potassium primary phosphate, agriculturally be used as efficient phosphorus potassium complex fertilizer, be widely used in the crop of the almost all types such as all types of cash crop, grain, melon and fruit, vegetables, there is remarkable increasing both production and income, the amount of changing optimizes many excellent effects such as quality, resistant to lodging, disease and insect resistance, control early ageing, and have and overcome the aging receptivity of plant growth later stage root system and decline and the malnourished effect that causes.The production method of potassium primary phosphate is a lot, is roughly summarised as neutralisation, extraction process, ion exchange method, double decomposition, direct method, crystallization process and electrolytic process etc.In China, production technique many employings neutralisation, secondly also has organic extraction, double decomposition, ion exchange method.
Preparing potassium primary phosphate at present, also to there is product purity low, impurity is many, equipment requirements is high, the problems such as disposing mother liquor is difficult, and the problem of fertilization of highland barley mainly appears at unevenness of application, residual many, cause environmental pollution etc., present inventor is by a large amount of experiments and research, and exploring a kind of purity that can improve potassium primary phosphate again can the method for coproduction highland barley composite fertilizer special.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method preparing potassium primary phosphate coproduction highland barley composite fertilizer special, it has, and environmental pollution is low, equipment requirements is low, production cost is low, potassium dihydrogen phosphate product purity advantages of higher, and the highland barley composite fertilizer special of by-product fully can be absorbed by plant, composite fertilizer's nutritive element collocation is proper, has certain value of environmental protection and economic worth.
The present invention is achieved by the following technical programs:
A kind of method preparing potassium primary phosphate coproduction highland barley composite fertilizer special, with urea and phosphoric acid in molar ratio 1:1.2-1.6 mix, temperature is risen to 120-135 DEG C, stirring reaction 3h, separation obtains intermediate, by intermediate and alkaline potassium hybrid reaction, control pH value is 3.6-3.9, obtain containing nitrogen after reaction terminates, phosphorus, the mother liquor of potassium, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 15.5-16.5%, phosphorus pentoxide content is 7.5-8.5%, when potassium oxide content is 8.5-9.5%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate, then in the filtrate obtained, add the element needed for highland barley, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product.
Specifically comprise the following steps:
(1) raw material hybrid reaction: use urea and phosphoric acid in molar ratio 1:1.2-1.5 mix, and temperature is risen to 120-134 DEG C, and stirring velocity is 65-75r/min stirring reaction 3h, is separated and obtains intermediate;
(2) prepare potassium primary phosphate: by step 1) in the intermediate that obtains and alkaline potassium hybrid reaction, control pH value is 3.6-3.8, the mother liquor containing nitrogen, phosphorus, potassium is obtained after reaction terminates, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 15.5-16.4%, phosphorus pentoxide content is 8.5-9.4%, when potassium oxide content is 8.5-9.4%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate;
(3) prepare highland barley composite fertilizer special: then to step 2) in add element needed for highland barley in the filtrate that obtains, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product;
The reaction of described urea and phosphoric acid is that urea solid and phosphoric acid solution react.
The concentration of described phosphoric acid is 74-76%.
Described alkaline potassium is potassium hydroxide.
The cooling temperature of described crystallisation by cooling is 25 DEG C.
Element needed for described highland barley is zinc, iron, magnesium.
Described highland barley composite fertilizer special is chemical combination state Chemical Mixed Fertilizer.
Described chemical combination state Chemical Mixed Fertilizer, containing following N P and K chemical combination state structural formula in its composition:
wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
Beneficial effect of the present invention is: prepare potassium primary phosphate by phosphoric acid and urea reaction, make the potassium dihydrogen phosphate product purity of output high, compensate for conventional wet phosphoric acid when preparing potassium primary phosphate, the problem of impurity treatment difficulty, reduce production cost, and in the process preparing potassium primary phosphate, by to raw material, temperature, the control of constituent content, obtain the filtrate that can be prepared into highland barley composite fertilizer special, use this filtrate to prepare composite fertilizer can not only meet the demand of highland barley to nutritive element, and there will not be the problem causing Soil Environmental Pollution because fertile amount is residual, there is the higher value of environmental protection and economic worth.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described, but described in claimed scope is not limited to.
Reaction principle illustrates:
Urea and phosphatase reaction generate Ureaphil, and Ureaphil can form the ion double salt that a kind of positive and negative charge attracts mutually under containing phosphoric acid and hot environment, and under the environment that exists at phosphoric acid of Ureaphil ion double salt, H wherein
2nCONH
3 +ion and phosphoric acid close, form the intermediate-ion of C → O coordinate bond, be CO
5pN
2h
8 +ion, and then make in Ureaphil intermediate containing a large amount of H
2pO
4 -and CO
5pN
2h
8 +ion, when adding excessive and appropriate potassium ion, dihydrogen phosphate and potassium ion form potassium dihydrogen phosphate crystal and are precipitated, unnecessary potassium ion and CO
5pN
2h
8 +ionic reaction, and displace part NH4+, make in solution containing CO
5pNH
4k
+double salt ion, by element adjustment, finally adding dried filtrate can obtain composite fertilizer.Concrete reaction equation is as follows:
Reaction equation one:
H
2PO
3+CO(NH
2)
2—CO(NH
2)
2·H
3PO
4
Reaction equation two:
CO(NH
2)
2·H
3PO
4—H
2NCONH
3 ++H
2PO
4 -
Reaction equation three:
H
2PO
4 -+K
+—KH
2PO
4
Reaction equation four:
Reaction equation five:
Below in conjunction with embodiment, the present invention is further elaborated:
Embodiment 1
Prepare a method for potassium primary phosphate coproduction highland barley composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: use urea and phosphoric acid in molar ratio 1:1.2 mix, and temperature is risen to 120 DEG C, stirring velocity is 65-75r/min stirring reaction 3h, is separated and obtains intermediate;
(2) prepare potassium primary phosphate: by step 1) in the intermediate that obtains and 1.4mol potassium hydroxide hybrid reaction, controlling pH value is 3.6, the mother liquor containing nitrogen, phosphorus, potassium is obtained after reaction terminates, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 15.6%, phosphorus pentoxide content is 8.6%, when potassium oxide content is 8.6%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate;
(3) prepare highland barley composite fertilizer special: then to step 2) in add zinc, iron, magnesium elements needed for highland barley in the filtrate that obtains, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product;
Embodiment 2
Prepare a method for potassium primary phosphate coproduction highland barley composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: use urea and phosphoric acid in molar ratio 1:1.4 mix, and temperature is risen to 124 DEG C, stirring velocity is 65-75r/min stirring reaction 3h, is separated and obtains intermediate;
(2) prepare potassium primary phosphate: by step 1) in the intermediate that obtains and 1.4mol potassium hydroxide hybrid reaction, controlling pH value is 3.6, the mother liquor containing nitrogen, phosphorus, potassium is obtained after reaction terminates, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 15.8%, phosphorus pentoxide content is 8.7, when potassium oxide content is 8.7%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate;
(3) prepare highland barley composite fertilizer special: then to step 2) in add zinc, iron, magnesium elements needed for highland barley in the filtrate that obtains, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product;
Embodiment 3
Prepare a method for potassium primary phosphate coproduction highland barley composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: use urea and phosphoric acid in molar ratio 1:1.4 mix, and temperature is risen to 128 DEG C, stirring velocity is 65-75r/min stirring reaction 3h, is separated and obtains intermediate;
(2) prepare potassium primary phosphate: by step 1) in the intermediate that obtains and potassium hydroxide hybrid reaction, controlling pH value is 3.7, the mother liquor containing nitrogen, phosphorus, potassium is obtained after reaction terminates, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 15.9%, phosphorus pentoxide content is 8.7%, when potassium oxide content is 8.8%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate;
(3) prepare highland barley composite fertilizer special: then to step 2) in add zinc, iron, magnesium elements needed for highland barley in the filtrate that obtains, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product;
Embodiment 4
Prepare a method for potassium primary phosphate coproduction highland barley composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: use urea and phosphoric acid in molar ratio 1:1.5 mix, and temperature is risen to 131 DEG C, stirring velocity is 65-75r/min stirring reaction 3h, is separated and obtains intermediate;
(2) prepare potassium primary phosphate: by step 1) in the intermediate that obtains and 1.4mol potassium hydroxide hybrid reaction, controlling pH value is 3.7, the mother liquor containing nitrogen, phosphorus, potassium is obtained after reaction terminates, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 15.9%, phosphorus pentoxide content is 8.9%, when potassium oxide content is 9.1%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate;
(3) prepare highland barley composite fertilizer special: then to step 2) in add zinc, iron, magnesium elements needed for highland barley in the filtrate that obtains, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product;
Embodiment 5
Prepare a method for potassium primary phosphate coproduction highland barley composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: use urea and phosphoric acid in molar ratio 1:1.5 mix, and temperature is risen to 132 DEG C, stirring velocity is 65-75r/min stirring reaction 3h, is separated and obtains intermediate;
(2) prepare potassium primary phosphate: by step 1) in the intermediate that obtains and 1.4mol potassium hydroxide hybrid reaction, control pH value is 3.6-3.8, the mother liquor containing nitrogen, phosphorus, potassium is obtained after reaction terminates, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 16.1%, phosphorus pentoxide content is 9.1%, when potassium oxide content is 9.1%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate;
(3) prepare highland barley composite fertilizer special: then to step 2) in add zinc, iron, magnesium elements needed for highland barley in the filtrate that obtains, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product;
Embodiment 6
Prepare a method for potassium primary phosphate coproduction highland barley composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: use urea and phosphoric acid in molar ratio 1:1.5 mix, and temperature is risen to 134 DEG C, stirring velocity is 65-75r/min stirring reaction 3h, is separated and obtains intermediate;
(2) prepare potassium primary phosphate: by step 1) in the intermediate that obtains and 1.4mol potassium hydroxide hybrid reaction, controlling pH value is 3.8, the mother liquor containing nitrogen, phosphorus, potassium is obtained after reaction terminates, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 16.2%, phosphorus pentoxide content is 9.1%, when potassium oxide content is 8.9%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate;
(3) prepare highland barley composite fertilizer special: then to step 2) in add zinc, iron, magnesium elements needed for highland barley in the filtrate that obtains, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product;
Below in conjunction with specific experiment example, product of the present invention and technique effect are further described.
Experimental example 1
The embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, in the highland barley composite fertilizer special prepared detect according to GB1887-2002 standard, its result is as shown in table 1:
The detection of content of element of table 1 highland barley composite fertilizer special of the present invention
| Test item | Criterion of acceptability | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| N P and K | 30％ | 32.8％ | 33.2％ | 33.4％ | 33.9％ | 34.3％ | 34.2％ |
| Nitrogen | 15％ | 15.6％ | 15.8％ | 15.9％ | 15.9％ | 16.1％ | 16.2％ |
| Phosphorus | 7％ | 8.6％ | 8.7％ | 8.7％ | 8.9％ | 9.1％ | 9.1％ |
| Potassium | 8/％ | 8.6％ | 8.7％ | 8.8％ | 9.1％ | 9.1％ | 8.9％ |
[0070]?
| Water content | ≤10％ | 3.5％ | 3.5％ | 3.5％ | 3.5％ | 3.5％ | 3.5％ |
By learning in table 1 that the constituent content of highland barley composite fertilizer special prepared by the present invention not only reaches criterion of acceptability, and be much better than criterion of acceptability, illustrate that this composite fertilizer can meet the nutritive element demand of highland barley, technique effect has progress significantly.
Experimental example 2
The embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, in the potassium dihydrogen phosphate product prepared detect by the detection method of GBT278-1997.
Table 2 potassium dihydrogen phosphate product purity detecting of the present invention
As can be seen from Table 2, the potassium primary phosphate that technical scheme of the present invention is produced not only reaches criterion of acceptability, and the purity of product is also higher, illustrates that present method is prepared potassium dihydrogen phosphate product and had significant progress.
Claims (9)
1. prepare the method for potassium primary phosphate coproduction highland barley composite fertilizer special for one kind, it is characterized in that: use urea and phosphoric acid in molar ratio 1:1.2-1.6 mix, temperature is risen to 120-135 DEG C, stirring reaction 3h, separation obtains intermediate, by intermediate and alkaline potassium hybrid reaction, control pH value is 3.6-3.9, obtain containing nitrogen after reaction terminates, phosphorus, the mother liquor of potassium, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 15.5-16.5%, phosphorus pentoxide content is 7.5-8.5%, when potassium oxide content is 8.5-9.5%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate, then in the filtrate obtained, add the element needed for highland barley, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product.
2. the method preparing potassium primary phosphate coproduction highland barley composite fertilizer special according to claim 1, it is characterized in that, the method comprises the following steps:
(1) raw material hybrid reaction: use urea and phosphoric acid in molar ratio 1:1.2-1.5 mix, and temperature is risen to 120-134 DEG C, and stirring velocity is 65-75r/min stirring reaction 3h, is separated and obtains intermediate;
(2) prepare potassium primary phosphate: by step 1) in the intermediate that obtains and alkaline potassium hybrid reaction, control pH value is 3.6-3.8, the mother liquor containing nitrogen, phosphorus, potassium is obtained after reaction terminates, mother liquor is put and decrease temperature crystalline in cooling crystallizer, monitoring analysis is carried out to mother liquor simultaneously, when nitrogen content is 15.5-16.4%, phosphorus pentoxide content is 8.5-9.4%, when potassium oxide content is 8.5-9.4%, stop crystallization and filter, namely the filter cake obtained is potassium primary phosphate;
(3) prepare highland barley composite fertilizer special: then to step 2) in add element needed for highland barley in the filtrate that obtains, and take the heat-up rate of 3 DEG C/min filtrate to be warming up to 24 DEG C to carry out drying, after dry 28min, when water content is 3.5%, obtain highland barley composite fertilizer special finished product.
3. the method preparing potassium primary phosphate coproduction highland barley composite fertilizer special according to claim 1 and 2, is characterized in that: the reaction of described urea and phosphoric acid is that urea solid and phosphoric acid solution react.
4. the method preparing potassium primary phosphate coproduction highland barley composite fertilizer special according to claim 1 and 2, is characterized in that: the concentration of described phosphoric acid is 74-76%.
5. the method preparing potassium primary phosphate coproduction highland barley composite fertilizer special according to claim 1 and 2, is characterized in that: described alkaline potassium is potassium hydroxide.
6. the method preparing potassium primary phosphate coproduction highland barley composite fertilizer special according to claim 1 and 2, is characterized in that: the cooling temperature of described crystallisation by cooling is 25 DEG C.
7. the method preparing potassium primary phosphate coproduction highland barley composite fertilizer special according to claim 1 and 2, is characterized in that: the element needed for described highland barley is zinc, iron, magnesium.
8. the method preparing potassium primary phosphate coproduction highland barley composite fertilizer special according to claim 1 and 2, is characterized in that: described highland barley composite fertilizer special is chemical combination state Chemical Mixed Fertilizer.
9. the method preparing potassium primary phosphate coproduction highland barley composite fertilizer special according to claim 8, is characterized in that: described chemical combination state Chemical Mixed Fertilizer, containing following N P and K chemical combination state structural formula in its composition:
wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337383A (en) * | 2001-09-04 | 2002-02-27 | 慕智君 | Liquid potassium dihydrogen phosphate and its production process |
| CN103803518A (en) * | 2014-01-24 | 2014-05-21 | 贵阳中化开磷化肥有限公司 | Method for preparing monopotassium phosphate by using wet-process phosphoric acid |
-
2014
- 2014-09-19 CN CN201410477846.4A patent/CN104291295A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337383A (en) * | 2001-09-04 | 2002-02-27 | 慕智君 | Liquid potassium dihydrogen phosphate and its production process |
| CN103803518A (en) * | 2014-01-24 | 2014-05-21 | 贵阳中化开磷化肥有限公司 | Method for preparing monopotassium phosphate by using wet-process phosphoric acid |
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Application publication date: 20150121 |