CN104261374A - Production method for preparing ammonium dihydrogen phosphate with special astragalus membranaceus fertilizer as byproduct - Google Patents
Production method for preparing ammonium dihydrogen phosphate with special astragalus membranaceus fertilizer as byproduct Download PDFInfo
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Abstract
The invention relates to the technical field of chemical engineering, and particularly relates to a production method for preparing ammonium dihydrogen phosphate with a special astragalus membranaceus fertilizer as a byproduct. Through analysis on requirements on nutritional elements in the astragalus membranaceus growth process, analysis and realization of fertilization conditions of traditional astragalus membranaceus planting, research and discussion of the absorption conditions of crops on nitrogen, phosphorus and potassium, and analysis by combining with the defects in the preparation process of an ammonium dihydrogen phosphate product, a production process of the special fertilizer for astragalus membranaceus is combined with a preparation process of the ammonium dihydrogen phosphate product, so that the preparation process of the ammonium dihydrogen phosphate product and the preparation process of the special fertilizer for the astragalus membranaceus are complementary; production of the special fertilizer for the astragalus membranaceus is carried out by using liquid waste generated in the preparation process of the ammonium dihydrogen phosphate product; the added value of the product in the preparation process of the ammonium dihydrogen phosphate product is increased; the discharge of the liquid waste is lowered; and meanwhile, waste of nitrogen and phosphorus resources also can be avoided by the unnecessary deep crystal ammonium dihydrogen phosphate product in the ammonium dihydrogen phosphate process.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of production method preparing primary ammonium phosphate by-product Radix Astragali special fertilizer.
Background technology
The Radix Astragali is leguminous plants, its root is the famous conventional tonic Chinese medicine of China, modern pharmacological research shows, the Radix Astragali has immunity moderation, anti-ageing and anti-stress, resists myocardial ischemia, the effect such as anti-ephritis, anti-hepatitis and osteoporosis, at present in astragalus cultivation cultivation technique, investigative technique for Radix Astragali special fertilizer is less, and the fertilizer factor that to be Radix Astragali high-yield high-grade culture technique the most key.But the investigative technique in the prior art for Radix Astragali special fertilizer is less, and be all adopt traditional chemical fertilizer, composite fertilizer and other raw material fertilizer carry out mixed preparing, and if the patent No. is CN201010263167.9, " a kind of Radix Astragali special fertilizer " adopts astragalus root dregs, urea, diammonium phosphate, potassium sulfate to be mixed in proportion to form, and for example the patent No. is CN201310583089.4 " a kind of Radix Astragali increasing agent and preparation method thereof " is the increasing agent meeting Radix Astragali growth demand adopting ammonium sulfate, potassium primary phosphate, ammonium molybdate, boric acid, Trisodium Citrate, sodium hydroselenite etc. to make as raw material, as can be seen here, all that to adopt traditional chemical fertilizer and composite fertilizer to carry out certain proportion amount formulated in prior art, the fertilizer of this method preparation can meet the demand of astragalus cultivation, improve the output of the Radix Astragali, but, a large amount of this fertilizer, long-term puts in soil, Soil structure layer can be made to change, and then cause and harden and lose rate of utilization, its major cause is, although the demand of Radix Astragali crop can be met in this fertilizer, but the Radix Astragali is difficult to relatively large absorption n-p-k element wherein, make to also have a large amount of n-p-k elements in the fertilizer applied not by absorption completely, and then remain among soil, cause the cause of soil pollution, moreover, soil also can be made to eat more and more, and then improve the planting cost at plantation family.
Simultaneously, the preparation technology of primary ammonium phosphate product normally adopts phosphoric acid by wet process and thermal phosphoric acid to carry out producing, but be no matter that thermal phosphoric acid or Wet Processes of Phosphoric Acid are to prepare primary ammonium phosphate product, impact all can to the purity of primary ammonium phosphate product, make the purity of primary ammonium phosphate product poor, be difficult to meet industrial requirement, for this reason, in the process preparing primary ammonium phosphate product, the larger one-tenth of cost is needed originally to carry out the purification of primary ammonium phosphate product; For this reason, investigator is had to adopt intermediate substitute mode, with phosphoric acid and urea reaction to this, prepare Ureaphil intermediate, but this reaction completes below 80 DEG C, and then again by decrease temperature crystalline process, separate out primary ammonium phosphate product, and then raising primary ammonium phosphate product purity; ; often the needing of this processing step carries out degree of depth crystallization to primary ammonium phosphate; and then reduce the waste in the solution of nitrogen phosphoric to greatest extent, thus cost prepared by reduction primary ammonium phosphate product, relatively large discharging of waste liquid also can be avoided to cause certain pollution to environment; And in degree of depth crystallisation process, often along with the generation of other products, with primary ammonium phosphate crystallized mixed, and then can again have impact on the purity of primary ammonium phosphate product again.
For this reason, this investigator passes through in astragalus cultivation process, Radix Astragali nutrient demand situation, and in conjunction with the defect existed in primary ammonium phosphate product preparation process, the preparation technology of Radix Astragali special fertilizer preparation technology and primary ammonium phosphate product is combined, for the preparation technology of primary ammonium phosphate and Radix Astragali special fertilizer provides a kind of new approaches.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the invention provides a kind of production method preparing primary ammonium phosphate by-product Radix Astragali special fertilizer, have and the preparation technology of Radix Astragali special fertilizer preparation technology and primary ammonium phosphate product is combined, the waste liquid in primary ammonium phosphate product preparation process is adopted to carry out the preparation of Radix Astragali special fertilizer, improve the added value in primary ammonium phosphate product preparation process, avoid simultaneously and degree of depth crystallization is carried out to reduce production cost to primary ammonium phosphate, further improve purity and the quality of primary ammonium phosphate product, also can prepare simultaneously and meet Radix Astragali growth demand, and can guarantee to remain in the feature of the less N P and K double salt composite fertilizer of n-p-k element content in soil.
Be achieved particular by following technical scheme:
A kind of production method preparing primary ammonium phosphate by-product Radix Astragali special fertilizer, phosphoric acid is adopted to be (1.6-1.7) with urea according to mol ratio: 1 mixes, and to adjust temperature be 97-111 DEG C, stirring reaction 0.9-1.4h, obtain intermediate slip, and ammonia is passed in intermediate slip, control temperature of reaction is 65-75 DEG C, stirring reaction 30min, reaction end pH value is 4.2-4.4, obtain phosphoric acid ammonium dihydrogen slip, and the product of phosphoric acid ammonium dihydrogen slip is placed in circulation temperature lowering crystallizer, carry out circulation temperature lowering crystallization treatment, and detect the nitrogen phosphorus element content analyzed in filtrate, adjustment nitrogen phosphorus element content reaches 1:(1.1-1.3) time, stop the crystallization of primary ammonium phosphate product and filter, filter cake is primary ammonium phosphate product, in filtrate, add potassium composition and medium trace element compound be adjusted to chemical combination state composite fertilizer just finished product, the content of the potassium component content wherein added and nitrogen phosphoric is 1:(1.1-1.3 than for n-p-k element forms mol ratio): (1.3-1.5), and first finished product is placed in baker, adopt heat-up rate to be that 7 DEG C/min is warming up to 49-56 DEG C, after dry 0.8-1.3h, adjustment moisture content is 1.7-2.4%, can obtain the Radix Astragali special chemical combination state composite fertilizer.
Specifically comprise the following steps:
(1) raw material preparation mixing: be (1.6-1.7) according to mol ratio by phosphoric acid and urea: 1 in stirring-type reactor, be 97-111 DEG C in temperature, the stirring velocity controlling stirring tank is that 175-205r/min is uniformly mixed reaction 0.9-1.4h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 65-75 DEG C, be 65-75r/min according to stirring velocity, stirring reaction 30min, reaction end pH value is 4.2-4.4, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s and is cooled to temperature≤30 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, the mol ratio of phosphorus composition is 1:(1.1-1.3) time, stop crystallization and filter, acquisition filter cake is primary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1:(1.1-1.3): (1.3-1.5),
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, heat-up rate is adopted to be that 7 DEG C/min is warming up to 49-56 DEG C, after dry 0.8-1.3h, adjustment moisture content is 1.7-2.4%, can obtain the Radix Astragali special chemical combination state composite fertilizer.
Described potassium composition is the one in potassium oxalate, Potassium ethanoate, Repone K.
The volumetric molar concentration of potassium composition is 1.2-1.3mol/l.
Described medium trace element compound is the mixture of calcium sulfate, magnesium sulfate, zinc sulfate, ferric sulfate, manganous sulfate, humic acid, plant ash, Sodium orthomolybdate, boric acid, sodium ethylene diamine tetracetate, blast-furnace slag.
The addition of medium trace element compound is 14% of filtrate total amount.
Described chemical combination state composite 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.
When adding potassium composition and medium trace element compound, a small amount of Trisodium Citrate, sodium hydroselenite, modified zeolite powder, egg-shell meal, natural pond slag, natural pond liquid, poultry animal excretion, corn stalk powder, sugarcane straw powder, Chinese medicine slag and beneficial organism bacterium can also be added.
Meanwhile, a small amount of m-tetrachlorophthalodinitrile, Baijunling, EDTA etc. can also be added.
Compared with prior art, the technique effect of technical scheme of the present invention is embodied in:
1, by analyzing the demand of Radix Astragali process of growth Middle nutrition element, and undertaken analyzing and understand by fertile situation to traditional astragalus cultivation, and to the absorbing state of n-p-k element, research and discussion is carried out to crop, analyze in conjunction with the shortcoming in primary ammonium phosphate product preparation process, and then the preparation technology of the production technique of Radix Astragali special fertilizer and primary ammonium phosphate product is combined, the preparation technology of primary ammonium phosphate product and the preparation technology of Radix Astragali special fertilizer is made to carry out complementation, the waste liquid produced in primary ammonium phosphate product preparation process is adopted to carry out the production of Radix Astragali special fertilizer, improve the added value of product in primary ammonium phosphate product preparation process, reduce discharging of waste liquid amount, also make the waste also can avoiding nitrogen phosphor resource of unnecessary degree of depth crystalline ammonium dihydrogen product in primary ammonium phosphate technique simultaneously.
2, by the control of the processing parameter in phosphoric acid and urea reaction process, make the structural formula of Ureaphil that complicated change occur, and then form the complexity polymerization phosphorus urea gas ions of Nitrogen-and Phosphorus-containing, this gas ions can compared with the content of the n-p-k element in the control chemical combination state double salt structure of limits, and then the obtained azophoska salt chemical combination state composite fertilizer meeting Radix Astragali process of growth needs, and the seed output and quality of the Radix Astragali is improved largely, reduce the planting cost of peasant household, avoid the environmental pollution that Fertilization Effect is brought, there is the significant value of environmental protection and economic benefit, , the purity of primary ammonium phosphate product is substantially increased meanwhile, the quality of primary ammonium phosphate product is guaranteed.
3, by technical parameter in chemical combination state compound fertilizer production technology, namely be exactly temperature, the control of material concentration and proportioning, after making phosphoric acid and urea reaction, generate Ureaphil product, Ureaphil product itself has stronger acidity, and between phosphoric acid and urea, be the chemical combination state double salt be combined together to form by the mode of coordinate bond, also be fertile as crop in conventional art, and crop is to the specific absorption comparison urea of this chemical combination state double salt, volatile salt, the unitary such as ammonium nitrate, binary fertilizer specific absorption is a kind of chemical combination state composite fertilizer all preferably, but, under the environment that this chemical combination state double salt exists at phosphoric acid, at the temperature of 80-250 DEG C, complicated decomposition polyreaction can be there is, Ureaphil is made to form (H
2pO
4)
-(H
2nCONH
3)
+two ions, (H
2nCONH
3)
+ion and phosphoric acid close, and be under the environment of 80-160 DEG C in temperature, formed
intermediate-ion and dihydrogen phosphate, and coordinate bond is formed between C and O, this intermediate-ion can form multielement intermediate-ion with centering element compound chelating, and then the compound electronegative with other can be continued or ion forms inner complex, improve constituent content in double salt, and then the nutrient content that can adjust in the double salt of this ion existence, simultaneously, this inner complex can be hydrolyzed again and absorbed by crops, and then fertilizer efficiency can be provided for crop effectively for a long time, simultaneously, in conjunction with the mensuration of constituent content in the solution existed this ion, and then each constituent content during formation of adjustment double salt, dry the composite fertilizer obtained containing chemical combination state double salt structure, improve the quality of Radix Astragali special fertilizer.
Embodiment
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Principle illustrates:
The present invention carries out research and discussion by the mechanism of reacting phosphoric acid and carboxamide, and arrives in conjunction with prior art literature, and phosphoric acid and carboxamide react and generate Ureaphil, and its molecular formula is: CO (NH
2)
2.H
3pO
4under the environment of comparatively high temps, the chemical bond meeting dialysis between H and O in phosphoric acid, hydrogen ion is combined the ionic state formed containing positive charge with urea, the ion double salt making Ureaphil form a kind of positive and negative charge to attract mutually, its mechanism structural response following expression: CO (NH
2)
2.H
3pO
4→ (H
2pO
4)
-. (H
2nCONH
3)
+
Further, under the environment that Ureaphil ion double salt exists at phosphoric acid, (H wherein
2nCONH
3)
+positive ion and phosphoric acid close, form the intermediate-ion of C → O coordinate bond, be (CO
5pN
2h
8)
+, and then make in Ureaphil intermediate containing a large amount of (H
2pO
4)
-(CO
5pN
2h
8)
+ion, when adding excessive and appropriate ammonium radical ion, dihydrogen phosphate and ammonium radical ion form ammonium dihydrogen phosphate crystal and are precipitated, and by detecting the content of the nitrogen phosphoric analyzed in filtrate, and add potassium element, magnesium elements, ferro element and other medium trace element according to the demand of the Radix Astragali, trophic structure in adjustment filtrate, makes trophic structure layer meet the demand of the Radix Astragali, then dries the Radix Astragali special chemical combination state composite fertilizer that can obtain containing N, P, K and other elements.
Its concrete reaction principle will carry out further instruction by following reaction structure formula and reaction mechanism:
Reaction formula one:
CO(NH
2)
2+H
3PO
4→CO(NH
2)
2.H
3PO
4
Reaction formula two:
Reaction formula three:
Wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
Reaction formula four:
Primary ammonium phosphate product to be crystallized out after, then in filtrate, add potassium element and other elements, then can with the dihydrogen phosphate remained in filtrate, hydrogen phosphate and
intermediate-ion react, generate the chemical combination state Radix Astragali composite fertilizer special of Multiple salts forms.
Noun illustrates:
Ureaphil (Ureaphosphate, UP), No. CAS is 4861-19-2, and molecular formula is CH
7n
2o
5p, can be expressed as CO (NH
2)
2h
3pO
4:
It is a kind of fine chemical product being widely used in the fields such as livestock industry, industry, agricultural, its solid is white crystals or crystalline powder, and soluble in water and alcohol is insoluble to ethers, toluene and tetracol phenixin, the aqueous solution, in acid, start during melting to decompose and releases carbonic acid gas and ammonia.
Embodiment: with concrete operation embodiment, the present invention is further elaborated below.
Embodiment 1
Prepare a production method for primary ammonium phosphate by-product Radix Astragali special fertilizer, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.6:1 in stirring-type reactor, be 97 DEG C in temperature, the stirring velocity controlling stirring tank is that 175r/min is uniformly mixed and reacts 0.9h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 65 DEG C, is 75r/min according to stirring velocity, stirring reaction 30min, reaction end pH value is 4.2, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s and is cooled to temperature 30 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, when the mol ratio of phosphorus composition is 1:1.1, stop crystallization and filter, acquisition filter cake is primary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1:1.1:1.3,
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, heat-up rate is adopted to be that 7 DEG C/min is warming up to 49 DEG C, after dry 0.8h, adjustment moisture content is 1.7%, can obtain the Radix Astragali special chemical combination state composite fertilizer.
Described potassium composition is potassium oxalate.
The volumetric molar concentration of potassium composition is 1.2mol/l.
Described medium trace element compound is the mixture of 0.8% calcium sulfate, 0.09% magnesium sulfate, 0.08% zinc sulfate, 0.07% ferric sulfate, 0.04% manganous sulfate, 3.1% humic acid, 4.2% plant ash, 0.06% Sodium orthomolybdate, 0.06% boric acid, 0.05% sodium ethylene diamine tetracetate, 2.5% blast-furnace slag.
Embodiment 2
Prepare a production method for primary ammonium phosphate by-product Radix Astragali special fertilizer, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.7:1 in stirring-type reactor, be 111 DEG C in temperature, the stirring velocity controlling stirring tank is that 205r/min is uniformly mixed and reacts 1.4h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 75 DEG C, is 65r/min according to stirring velocity, stirring reaction 30min, reaction end pH value is 4.4, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s and is cooled to temperature 28 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, when the mol ratio of phosphorus composition is 1:1.3, stop crystallization and filter, acquisition filter cake is primary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1:1.3:1.5,
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, heat-up rate is adopted to be that 7 DEG C/min is warming up to 56 DEG C, after dry 1.3h, adjustment moisture content is 2.4%, can obtain the Radix Astragali special chemical combination state composite fertilizer.
Described potassium composition is Potassium ethanoate.
The volumetric molar concentration of potassium composition is 1.3mol/l.
Described medium trace element compound is the mixture of 0.6% calcium sulfate, 0.08% magnesium sulfate, 0.05% zinc sulfate, 0.03% ferric sulfate, 0.05% manganous sulfate, 4.1% humic acid, 3.2% plant ash, 0.03% Sodium orthomolybdate, 0.07% boric acid, 0.04% sodium ethylene diamine tetracetate, 5.2% blast-furnace slag.
Embodiment 3
Prepare a production method for primary ammonium phosphate by-product Radix Astragali special fertilizer, comprise the following steps:
(1) raw material preparation mixing: by phosphoric acid and urea according to mol ratio be 1.65:1 in stirring-type reactor, be 105 DEG C in temperature, the stirring velocity controlling stirring tank is that 185r/min is uniformly mixed and reacts 1.2h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 70 DEG C, is 70r/min according to stirring velocity, stirring reaction 30min, reaction end pH value is 4.3, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s and is cooled to temperature 25 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, when the mol ratio of phosphorus composition is 1:1.2, stop crystallization and filter, acquisition filter cake is primary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1:1.2:1.4,
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, heat-up rate is adopted to be that 7 DEG C/min is warming up to 52.5 DEG C, after dry 1.1h, adjustment moisture content is 1.9%, can obtain the Radix Astragali special chemical combination state composite fertilizer.
Described potassium composition is the one in potassium oxalate, Potassium ethanoate, Repone K.
The volumetric molar concentration of potassium composition is 1.25mol/l.
Described medium trace element compound is the mixture of 0.5% calcium sulfate, 0.06% magnesium sulfate, 0.05% zinc sulfate, 0.04% ferric sulfate, 0.07% manganous sulfate, 2.9% humic acid, 3.8% plant ash, 0.02% Sodium orthomolybdate, 0.04% boric acid, 0.02% sodium ethylene diamine tetracetate, 6.1% blast-furnace slag.
Test example: the technique effect of technical scheme of the present invention and product performance are described further below in conjunction with specific embodiment content.
Test example 1 Radix Astragali special fertilizer of the present invention is on the impact of Radix Astragali quality
1.1 test process
Test group: adopt each 1000kg of Radix Astragali special fertilizer that embodiments of the invention 1, embodiment 2, embodiment 3 are obtained, and 1000kg is divided into two groups, often organize 500kg, label is 1a, 1b respectively; 2a, 2b; 3a, 3b; The a group plantation Erie Radix Astragali, b group plantation Radix Astagali, and when planting according to every mu of fertilising 125kg, plant four mu of Radixs Astragali.
Control group: adopt traditional primary ammonium phosphate, potassium primary phosphate, monoammonium phosphate, potassium hydrogen phosphate and other composite fertilizers and trace element, bacteria agent is that 1:1.2:1.4,1:1.3:1.5,1:1.1:1.3 are mixed with three groups of fertile 1000kg of the Radix Astragali according to N-P-K content ratio, label is A, B, C tri-groups respectively, again A, B, C are divided into two groups, label is A1, A2 respectively; B1, B2; C1, C2, each group fertilizer amount is 500kg, 1 group of the plantation Erie Radix Astragali, 2 groups of plantation Radix Astagali, and according to every mu of fertilising 125kg, plants four mu of Radixs Astragali.
Crop cycle: implantation time is 1 year.
Plant and within 1 year, observe Radix Astragali growth situation, after 1 year, the Radix Astragali of gathering, and the Radix Astragali is weighed process, its result is as shown in table 1.
Table 1
Shown as can be seen from the data in table 1 and growth situation result, the Radix Astragali special fertilizer that the compound method that the present invention is relatively traditional is prepared out has preferably advantage, the Radix Astragali about about 30% can be increased production, the growth situation of the growth cycle of the whole Radix Astragali is excellent, the time length of visible fertilizer is longer, can provide sufficient nutritive element to the Radix Astragali.
Claims (5)
1. prepare the production method of primary ammonium phosphate by-product Radix Astragali special fertilizer for one kind, it is characterized in that, phosphoric acid is adopted to be (1.6-1.7) with urea according to mol ratio: 1 mixes, and to adjust temperature be 97-111 DEG C, stirring reaction 0.9-1.4h, obtain intermediate slip, and ammonia is passed in intermediate slip, control temperature of reaction is 65-75 DEG C, stirring reaction 30min, reaction end pH value is 4.2-4.4, obtain phosphoric acid ammonium dihydrogen slip, and the product of phosphoric acid ammonium dihydrogen slip is placed in circulation temperature lowering crystallizer, carry out circulation temperature lowering crystallization treatment, and detect the nitrogen phosphorus element content analyzed in filtrate, adjustment nitrogen phosphorus element content reaches 1:(1.1-1.3) time, stop the crystallization of primary ammonium phosphate product and filter, filter cake is primary ammonium phosphate product, in filtrate, add potassium composition and medium trace element compound be adjusted to chemical combination state composite fertilizer just finished product, the content of the potassium component content wherein added and nitrogen phosphoric is 1:(1.1-1.3 than for n-p-k element forms mol ratio): (1.3-1.5), and first finished product is placed in baker, adopt heat-up rate to be that 7 DEG C/min is warming up to 49-56 DEG C, after dry 0.8-1.3h, adjustment moisture content is 1.7-2.4%, can obtain the Radix Astragali special chemical combination state composite fertilizer.
2. prepare the production method of primary ammonium phosphate by-product Radix Astragali special fertilizer as claimed in claim 1, it is characterized in that, comprise the following steps:
(1) raw material preparation mixing: be (1.6-1.7) according to mol ratio by phosphoric acid and urea: 1 in stirring-type reactor, be 97-111 DEG C in temperature, the stirring velocity controlling stirring tank is that 175-205r/min is uniformly mixed reaction 0.9-1.4h, obtains intermediate slip;
(2) primary ammonium phosphate is prepared: to step 1) pass into ammonia in the intermediate slip that obtains, and the temperature controlled in reactor is 65-75 DEG C, be 65-75r/min according to stirring velocity, stirring reaction 30min, reaction end pH value is 4.2-4.4, obtains the slip of phosphoric acid ammonium dihydrogen product;
(3) circulation crystallization filters: by step 2) slip that obtains phosphoric acid ammonium dihydrogen is placed in cooling crystallizer 10s and is cooled to temperature≤30 DEG C, down cycles crystallization filtration treatment, and detect the nutrient content analyzed in filtrate, treat nitrogen component, the mol ratio of phosphorus composition is 1:(1.1-1.3) time, stop crystallization and filter, acquisition filter cake is primary ammonium phosphate, potassium composition is added and medium trace element compound adjustment fertilizer structure becomes chemical combination state composite fertilizer just finished product in filtrate, the ratio that the potassium component content wherein added is n-p-k element with the content ratio of nitrogen phosphoric is 1:(1.1-1.3): (1.3-1.5),
(4) filtrate dries: by step 3) the chemical combination state composite fertilizer that obtains just finished product be placed in baker, heat-up rate is adopted to be that 7 DEG C/min is warming up to 49-56 DEG C, after dry 0.8-1.3h, adjustment moisture content is 1.7-2.4%, can obtain the Radix Astragali special chemical combination state composite fertilizer.
3. prepare the production method of primary ammonium phosphate by-product Radix Astragali special fertilizer as claimed in claim 1 or 2, it is characterized in that, described potassium composition is the one in potassium oxalate, Potassium ethanoate, Repone K.
4. prepare the production method of primary ammonium phosphate by-product Radix Astragali special fertilizer as claimed in claim 1 or 2, it is characterized in that, described medium trace element compound is the mixture of calcium sulfate, magnesium sulfate, zinc sulfate, ferric sulfate, manganous sulfate, humic acid, plant ash, Sodium orthomolybdate, boric acid, sodium ethylene diamine tetracetate, blast-furnace slag.
5. prepare the production method of primary ammonium phosphate by-product Radix Astragali special fertilizer as claimed in claim 1 or 2, it is characterized in that, described chemical combination state composite 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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| CN107258426A (en) * | 2017-05-28 | 2017-10-20 | 陈俊豪 | Improve the cultural method of emperor's mandarin orange pulp quality |
| CN107295924A (en) * | 2017-05-28 | 2017-10-27 | 陈俊豪 | The high-yield cultivating method of emperor mandarin orange |
| CN107347547A (en) * | 2017-05-28 | 2017-11-17 | 陈俊豪 | The implantation methods of emperor mandarin orange |
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| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| CN103787293A (en) * | 2014-01-24 | 2014-05-14 | 贵阳中化开磷化肥有限公司 | Method for preparing sodium dihydrogen phosphate by utilizing phosphoric acid by wet process |
| CN104016323A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for monoammonium phosphate |
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2014
- 2014-09-19 CN CN201410478218.8A patent/CN104261374B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| CN103787293A (en) * | 2014-01-24 | 2014-05-14 | 贵阳中化开磷化肥有限公司 | Method for preparing sodium dihydrogen phosphate by utilizing phosphoric acid by wet process |
| CN104016323A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for monoammonium phosphate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107258426A (en) * | 2017-05-28 | 2017-10-20 | 陈俊豪 | Improve the cultural method of emperor's mandarin orange pulp quality |
| CN107295924A (en) * | 2017-05-28 | 2017-10-27 | 陈俊豪 | The high-yield cultivating method of emperor mandarin orange |
| CN107347547A (en) * | 2017-05-28 | 2017-11-17 | 陈俊豪 | The implantation methods of emperor mandarin orange |
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| CN104261374B (en) | 2016-04-27 |
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