A kind of method preparing potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special
Technical field
The present invention relates to technical field of fertilizer, be specifically related to a kind of potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special prepared
Method.
Background technology
Tung tree deciduous tree, bark grey, branch is sturdy, leaf oval, flower monoecism, close brown outside calyx
Look micro-pubescence, petal white, there are pale red vein, obovate, ovary is close by pubescence, and drupe is the most spherical, and seed coat is wooden.Flowering fruit bearing stage
The 3-9 month.Tung oil is essential industry oil, manufactures paint and coating, and economic worth is the highest.Tung oil and wood oil golden yellow color or palm fibre
Huang, is all excellent drying oil, glossy, it is impossible to edible, have waterproof, airtight, do not conduct electricity, antiacid alkali, anticorrosion, resistance to
The feature such as cold and hot.It is widely used in the manufacturing industry such as painting, plastics, electrical equipment, artificial rubber, dermatine, synthetic petroleum, ink.Oil
Paulownia is Chinese peculiar commodity trees, it with oil tea, walnut, Chinese tallow tree claim China four big traditional oil trees.Tung oil tree at least thousand
Cultivation history more than year, tung oil tree has higher economic worth, and the plantation of tung oil tree be unable to do without fertilizer, and common fertilizer is executed in arable land
After entering, a part is rising, dissipate and outflow with water, and a part is fixed by soil and edaphon and utilizes, wherein
A part just the most absorbed by crops and utilize.Show after deliberation: urea, the utilization rate of carbon ammonium are 20% one 46%, phosphate fertilizer (two
Ammonium, an ammonium, coarse whiting) it is 10% one 25%, potash fertilizer 45% one 60%.As can be seen here, common fertilizer utilization rate is the lowest.For
This, the present inventor is for a kind of method preparing tung oil tree special fertilizer of feature characteristic research fertile with happiness of tung oil tree, of tung oil tree
Growth cycle needs absorb more nutriment, be not only the provided nitrogen of common fertilizer, phosphorus, potassium, support as lacked other
Point, cannot growing by normal growth, the present invention is the synthesis containing multiple nutrient, is not the chemical fertilizer that nutrient is single, it
Also rich in the element that the crops such as calcium, iron, magnesium are required in addition to the macronutrient such as nitrogenous, phosphorus, potassium, serve regulation soil and put down
The effect of weighing apparatus nutrition, is that a kind of new and effective no-pollution full nutrition chelates dedicated fertilizer.This special fertilizer is to carry out normally according to tung oil tree
Grow, cultivation feature, irrigate habit, prepared by the nutrient of needs.Adding various nutrient elements, tung oil tree is good in protection
Health, fertility is more longlasting, and effectively regulation plant part defensive ability/resistance ability, alleviates disease, improves yield.It is substantially improved crop quality, carries
The immunity of high tung oil tree self, can well prevent tung oil tree regular incidence.
Potassium dihydrogen phosphate, is agriculturally used as efficient phosphorus potassium complex fertilizer, is widely used in all types of industrial crops, grain, melon
The crop of the almost all types such as fruits and vegetables, there is notable increasing both production and income, the amount of changing optimizes quality, resistant to lodging, disease and insect resistance, anti-
Control many excellent effects such as early ageing, and there is the nutrition overcoming the plant growth later stage aging absorbability of root system to decline and to cause
Not enough effect.The production method of potassium dihydrogen phosphate is a lot, is substantially summarised as neutralisation, extraction, ion-exchange, double decomposition
Method, direct method, crystallisation and electrolysis etc..In China, production technology many employings neutralisation, secondly also have organic extraction, answer
Decomposition method, ion-exchange.
As the patent document of Publication No. CN100999312A discloses a kind of potassium dihydrogen phosphate, S-based compound fertilizer and polymerization
The coproduction side of aluminium chloride, not only solves phosphoric acid by wet process and prepares the impurity interference problem of potassium dihydrogen phosphate, and can also by-product without
The S-based compound fertilizer of chlorine, the most coproducing polymerized aluminium chloride, raw material availability is high, improves economic benefit.
The technology of preparing mixing composite fertilizer is also had currently for crops, but not at Patents file and open literary composition
Offer the discovery difference for variety of crops by the research of element needed for crop, the compound state carrying out element arranging in pairs or groups
The technical scheme of composite fertilizer exists, and does not the most find the technology of coproduction tung oil tree composite fertilizer special during preparing potassium dihydrogen phosphate
Scheme occurs.
Therefore, by substantial amounts of research and practice, element collocation needed for tung oil tree is main to the present inventor, is improving phosphoric acid system
For crop, the absorptivity of required element is adjusted whole production technology and parameter while the purity of standby potassium dihydrogen phosphate product
Produce the special efficient composite fertilizer being applicable to tung oil tree.
Summary of the invention
For solving above-mentioned technical problem, the invention provides a kind of potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special prepared
Preparation method, it has, and environmental pollution is low, equipment requirement is low, production cost is low, potassium dihydrogen phosphate product purity advantages of higher, and
And the tung oil tree composite fertilizer special of by-product can be fully absorbed by plant, composite fertilizer's nutrient collocation is proper, has certain ring
Value of supporting value and economic worth.
The present invention is achieved by the following technical programs:
A kind of method preparing potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special, with urea and phosphoric acid 1:1.3-in molar ratio
1.7 mixing, rise to 100-130 DEG C by temperature, stirring reaction 2.2h, and intermediate is mixed by isolated intermediate with alkalescence potassium
Reaction, control pH value is 3.6-3.9, and reaction obtains, containing nitrogen, phosphorus, the mother liquor of potassium, being put by mother liquor and cooler crystallizer after terminating
Middle decrease temperature crystalline, is monitored mother liquor analyzing, when nitrogen content is 15.2-15.6%, and phosphorus pentoxide content is 7.2-simultaneously
7.6%, when potassium oxide content is 8.2-8.6%, stops crystallization and also filter, the filter cake obtained is i.e. potassium dihydrogen phosphate, then to
The filtrate obtained adds the element needed for tung oil tree, and takes the programming rate of 5 DEG C/min that filtrate is warming up to 25 DEG C to do
Dry, after being dried 20min, when water content is 4.5%, obtain tung oil tree composite fertilizer special finished product.
Specifically include following steps:
(1) raw material hybrid reaction: mix with phosphoric acid 1:1.3-1.6 in molar ratio with urea, temperature is risen to 100-129
DEG C, mixing speed is 65-75r/min stirring reaction 2.2h, isolated intermediate;
(2) prepare potassium dihydrogen phosphate: by step 1) in the intermediate that obtains and alkalescence potassium hybrid reaction, controlling pH value is
3.6-3.8, reaction obtains, containing nitrogen, phosphorus, the mother liquor of potassium, being put by mother liquor and decrease temperature crystalline in cooler crystallizer, simultaneously after terminating
It is monitored mother liquor analyzing, when nitrogen content is 15.2-15.5%, and phosphorus pentoxide content is 7.2-7.5%, potassium oxide content
During for 8.2-8.5%, stopping crystallization and filter, the filter cake obtained is i.e. potassium dihydrogen phosphate;
(3) prepare tung oil tree composite fertilizer special: then to step 2) in the filtrate that obtains adds the element needed for tung oil tree, and
Filtrate is warming up to 25 DEG C and is dried by the programming rate taking 5 DEG C/min, after being dried 20min, when water content is 4.5%,
Obtain tung oil tree composite fertilizer special finished product;
Described urea is that urea solid reacts with phosphoric acid solution with the reaction of phosphoric acid.
The concentration of described phosphoric acid is 70%.
Described alkalescence potassium is potassium hydroxide.
The chilling temperature of described crystallisation by cooling is 23 DEG C.
Element needed for described tung oil tree is calcium, iron, magnesium.
Described tung oil tree composite fertilizer special is compound state Chemical Mixed Fertilizer.
Described compound state Chemical Mixed Fertilizer, containing following N P and K compound state structural formula in its composition:
Wherein, the dotted line between carbon atom and oxygen atom represents C atom and O atom
Between there is coordinate bond.
The beneficial effects of the present invention is: prepare potassium dihydrogen phosphate by phosphoric acid and urea reaction so that the phosphoric acid of output
Potassium dihydrogen product purity is high, compensate for conventional wet phosphoric acid when preparing potassium dihydrogen phosphate, and the problem of impurity treatment difficulty reduces
Production cost, and during preparing potassium dihydrogen phosphate, by raw material, temperature, the control of constituent content, having obtained can
To be prepared as the filtrate of tung oil tree composite fertilizer special, use what this filtrate prepared composite fertilizer can not only meet tung oil tree to nutrition
The demand of element, and do not have and cause the problem of Soil Environmental Pollution because of fertile amount residual, there is higher environmental protection valency
Value and economic worth.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is further described, but claimed scope is not limited to
In described.
Reaction principle illustrates:
Urea generates urea phosphate with phosphatase reaction, and urea phosphate can form a kind of positive negative electricity under containing phosphoric acid and hot environment
The ion double salt that lotus attracts mutually, and urea phosphate ion double salt is in the environment of phosphoric acid exists, H therein2NCONH3 +Ion and phosphorus
Acid is close, forms the intermediate-ion of C → O coordinate bond, is CO5PN2H8 +Ion, and then make in urea phosphate intermediate containing big
The H of amount2PO4 -And CO5PN2H8 +Ion, when adding excessive and appropriate potassium ion, dihydrogen phosphate forms phosphorus with potassium ion
Acid dihydride potassium crystal is precipitated, unnecessary potassium ion and CO5PN2H8 +Ionic reaction, and displace part NH4+ so that in solution
Containing CO5PNH4K+Double salt ion, by element adjust, be eventually adding dried filtrate and can obtain composite fertilizer.Concrete reaction
Equation is as follows:
Reaction equation one:
H2PO3+CO(NH2)2—CO(NH2)2·H3PO4
Reaction equation two:
CO(NH2)2·H3PO4—H2NCONH3 ++H2PO4 -
Reaction equation three:
H2PO4 -+K+—KH2PO4
Reaction equation four:
Reaction equation five:
Below in conjunction with embodiment, the present invention is further elaborated:
Embodiment 1
A kind of method preparing potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: mix with phosphoric acid 1:1.3 in molar ratio with urea, temperature is risen to 100 DEG C, stirring speed
Spend for 65-75r/min stirring reaction 2.2h, isolated intermediate;
(2) prepare potassium dihydrogen phosphate: by step 1) in the intermediate that obtains and 1mol potassium hydroxide hybrid reaction, control PH
Value is 3.6, and reaction obtains, containing nitrogen, phosphorus, the mother liquor of potassium, being put by mother liquor and decrease temperature crystalline in cooler crystallizer, simultaneously after terminating
It is monitored mother liquor analyzing, when nitrogen content is 15.2%, and phosphorus pentoxide content is 7.2%, and potassium oxide content is 8.2%
Time, stop crystallization and filter, the filter cake obtained is i.e. potassium dihydrogen phosphate;
(3) prepare tung oil tree composite fertilizer special: then to step 2) in the filtrate that obtains adds the calcium needed for tung oil tree, iron,
Magnesium elements, and take the programming rate of 5 DEG C/min that filtrate is warming up to 25 DEG C to be dried, after being dried 20min, when water content is
When 4.5%, obtain tung oil tree composite fertilizer special finished product;
Embodiment 2
A kind of method preparing potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: mix with phosphoric acid 1:1.4 in molar ratio with urea, temperature is risen to 105 DEG C, stirring speed
Spend for 65-75r/min stirring reaction 2.2h, isolated intermediate;
(2) prepare potassium dihydrogen phosphate: by step 1) in the intermediate that obtains and 1mol potassium hydroxide hybrid reaction, control PH
Value is 3.6, and reaction obtains, containing nitrogen, phosphorus, the mother liquor of potassium, being put by mother liquor and decrease temperature crystalline in cooler crystallizer, simultaneously after terminating
It is monitored mother liquor analyzing, when nitrogen content is 15.3%, and phosphorus pentoxide content is 7.3%, and potassium oxide content is 8.3%
Time, stop crystallization and filter, the filter cake obtained is i.e. potassium dihydrogen phosphate;
(3) prepare tung oil tree composite fertilizer special: then to step 2) in the filtrate that obtains adds the calcium needed for tung oil tree, iron,
Magnesium elements, and take the programming rate of 5 DEG C/min that filtrate is warming up to 25 DEG C to be dried, after being dried 20min, when water content is
When 4.5%, obtain tung oil tree composite fertilizer special finished product;
Embodiment 3
A kind of method preparing potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: mix with phosphoric acid 1:1.4 in molar ratio with urea, temperature is risen to 110 DEG C, stirring speed
Spend for 65-75r/min stirring reaction 2.2h, isolated intermediate;
(2) prepare potassium dihydrogen phosphate: by step 1) in the intermediate that obtains and 1mol potassium hydroxide hybrid reaction, control PH
Value is 3.7, and reaction obtains, containing nitrogen, phosphorus, the mother liquor of potassium, being put by mother liquor and decrease temperature crystalline in cooler crystallizer, simultaneously after terminating
It is monitored mother liquor analyzing, when nitrogen content is 15.4%, and phosphorus pentoxide content is 7.4%, and potassium oxide content is 8.4%
Time, stop crystallization and filter, the filter cake obtained is i.e. potassium dihydrogen phosphate;
(3) prepare tung oil tree composite fertilizer special: then to step 2) in the filtrate that obtains adds the calcium needed for tung oil tree, iron,
Magnesium elements, and take the programming rate of 5 DEG C/min that filtrate is warming up to 25 DEG C to be dried, after being dried 20min, when water content is
When 4.5%, obtain tung oil tree composite fertilizer special finished product;
Embodiment 4
A kind of method preparing potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: mix with phosphoric acid 1:1.5 in molar ratio with urea, temperature is risen to 115 DEG C, stirring speed
Spend for 65-75r/min stirring reaction 2.2h, isolated intermediate;
(2) prepare potassium dihydrogen phosphate: by step 1) in the intermediate that obtains and 1mol potassium hydroxide hybrid reaction, control PH
Value is 3.7, and reaction obtains, containing nitrogen, phosphorus, the mother liquor of potassium, being put by mother liquor and decrease temperature crystalline in cooler crystallizer, simultaneously after terminating
It is monitored mother liquor analyzing, when nitrogen content is 15.5%, and phosphorus pentoxide content is 7.5%, and potassium oxide content is 8.5%
Time, stop crystallization and filter, the filter cake obtained is i.e. potassium dihydrogen phosphate;
(3) prepare tung oil tree composite fertilizer special: then to step 2) in the filtrate that obtains adds the calcium needed for tung oil tree, iron,
Magnesium elements, and take the programming rate of 5 DEG C/min that filtrate is warming up to 25 DEG C to be dried, after being dried 20min, when water content is
When 4.5%, obtain tung oil tree composite fertilizer special finished product;
Embodiment 5
A kind of method preparing potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: mix with phosphoric acid 1:1.6 in molar ratio with urea, temperature is risen to 115 DEG C, stirring speed
Spend for 65-75r/min stirring reaction 2.2h, isolated intermediate;
(2) prepare potassium dihydrogen phosphate: by step 1) in the intermediate that obtains and 1mol potassium hydroxide hybrid reaction, control PH
Value is 3.8, and reaction obtains, containing nitrogen, phosphorus, the mother liquor of potassium, being put by mother liquor and decrease temperature crystalline in cooler crystallizer, simultaneously after terminating
It is monitored mother liquor analyzing, when nitrogen content is 15.5%, and phosphorus pentoxide content is 7.2%, and potassium oxide content is 8.3%
Time, stop crystallization and filter, the filter cake obtained is i.e. potassium dihydrogen phosphate;
(3) prepare tung oil tree composite fertilizer special: then to step 2) in the filtrate that obtains adds the calcium needed for tung oil tree, iron,
Magnesium elements, and take the programming rate of 5 DEG C/min that filtrate is warming up to 25 DEG C to be dried, after being dried 20min, when water content is
When 4.5%, obtain tung oil tree composite fertilizer special finished product;
Embodiment 6
A kind of method preparing potassium dihydrogen phosphate coproduction tung oil tree composite fertilizer special, the method comprises the following steps:
(1) raw material hybrid reaction: mix with phosphoric acid 1:1.6 in molar ratio with urea, temperature is risen to 129 DEG C, stirring speed
Spend for 65-75r/min stirring reaction 2.2h, isolated intermediate;
(2) prepare potassium dihydrogen phosphate: by step 1) in the intermediate that obtains and 1mol potassium hydroxide hybrid reaction, control PH
Value is 3.8, and reaction obtains, containing nitrogen, phosphorus, the mother liquor of potassium, being put by mother liquor and decrease temperature crystalline in cooler crystallizer, simultaneously after terminating
It is monitored mother liquor analyzing, when nitrogen content is 15.2%, and phosphorus pentoxide content is 7.5%, and potassium oxide content is 8.5%
Time, stop crystallization and filter, the filter cake obtained is i.e. potassium dihydrogen phosphate;
(3) prepare tung oil tree composite fertilizer special: then to step 2) in the filtrate that obtains adds the calcium needed for tung oil tree, iron,
Magnesium elements, and take the programming rate of 5 DEG C/min that filtrate is warming up to 25 DEG C to be dried, after being dried 20min, when water content is
When 4.5%, obtain tung oil tree composite fertilizer special finished product;
Below in conjunction with specific experiment example, product and the technique effect of the present invention 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 tung oil tree prepared
Composite fertilizer special detects according to GB1887-2002 standard, and its result is as shown in table 1:
The detection of content of element of table 1 tung oil tree of the present invention composite fertilizer special
Detection project |
Criterion of acceptability |
Embodiment 1 |
Embodiment 2 |
Embodiment 3 |
Embodiment 4 |
Embodiment 5 |
Embodiment 6 |
N P and K |
30% |
30.6% |
30.9% |
31.2% |
31.5% |
31% |
31.2% |
Nitrogen |
15% |
15.2% |
15.3% |
15.4% |
15.5% |
15.5% |
15.2% |
Phosphorus |
7% |
7.2% |
7.3% |
7.4% |
7.5% |
7.2% |
7.5% |
Potassium |
8/% |
8.2% |
8.3% |
8.4% |
8.5% |
8.3% |
8.5% |
Water content |
≤ 10% |
4.5% |
4.5% |
4.5% |
4.5% |
4.5% |
4.5% |
Qualified mark has not been only reached by the constituent content being appreciated that tung oil tree composite fertilizer special prepared by the present invention in table 1
Standard, and it is much better than criterion of acceptability, illustrate that this composite fertilizer can meet the nutrient demand of tung oil tree, technique effect has aobvious
Write ground progressive.
Experimental example 2
The embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, in the phosphoric acid prepared
Potassium dihydrogen product is detected by the detection method of GBT278-1997.
Table 2 potassium dihydrogen phosphate product of the present invention purity detecting
As can be seen from Table 2, the potassium dihydrogen phosphate that technical scheme is produced has not only reached qualified mark
Standard, and the purity of product is the highest, illustrates that this method is prepared potassium dihydrogen phosphate product and had the most progressive.