CN104310330A - Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for orange trees as byproduct - Google Patents
Method for preparing ammonium dihydrogen phosphate and preparing special composite fertilizer for orange trees as byproduct Download PDFInfo
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- CN104310330A CN104310330A CN201410477886.9A CN201410477886A CN104310330A CN 104310330 A CN104310330 A CN 104310330A CN 201410477886 A CN201410477886 A CN 201410477886A CN 104310330 A CN104310330 A CN 104310330A
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Abstract
The invention discloses a method for preparing ammonium dihydrogen phosphate and preparing a special composite fertilizer for orange trees as a byproduct. The method comprises the steps of preparing raw materials, preparing ammonium dihydrogen phosphate, adding elements to a filtrate, and drying. The highly pure ammonium dihydrogen phosphate is prepared through a reaction of phosphoric acid, urea and ammonia water, and the composite fertilizer suitable for the growth of orange trees is prepared through processing adjustment of a mother liquor generated through the reaction, so the resource waste is reduced, and the method has certain environmentally-friendly and economic values.
Description
Technical field
The present invention relates to technical field of fertilizers, be specifically related to a kind of method preparing primary ammonium phosphate by-product orange tree composite fertilizer special.
Background technology
Orange tree is that shrub is to dungarunga.Branch is more, and branch expansion or slightly sagging, stings less.Unifoliate compound leaf. winged petiole is usually narrow, or only has vestige, blade lanceolar.Oval or wealthy avette, size variation is larger.Often there is recess on top, and middle arteries and veins becomes dichotomy by near base portion to recess, and leaf margin at least upper semisection has blunt or circle carnassial tooth usually, seldom full edge.The fruit that orange tree is born is orange, and orange is often collectively referred to as oranges and tangerines together with mandarin orange, bright-colored, sweet and sour taste, and generally in safran, also have cyan or other colors, be one of modal fruit during people live, pericarp can be used as medicine.And the orange of high-quality be unable to do without good fertilizer, the main nutrient elements that orange tree absorbs is nitrogen, phosphorus, potassium, boron, magnesium etc., but in common fertilizer, the utilization ratio of N P and K is very low, and in general composite fertilizer, nitrogen use efficiency is 20%-40%, phosphorus only has about 20%, and potassium can reach more than 30%.It can thus be appreciated that this season utilization ratio of phosphorus is minimum, and the utilization ratio of nitrogen, potassium is suitable.It is high to there is loss of elements in common fertilizer, and Soil Environmental Pollution is large, high in cost of production problem, so for the difference of crop, the specificity of composite fertilizer has great importance.
The technology of preparing of mixing composite fertilizer is also had at present for farm crop, but in Patents file and open source literature, do not find that difference for variety of crops is by the research of element needed for crop, the technical scheme of element being carried out the composite fertilizer of the chemical combination state of arranging in pairs or groups exists, and does not also find that the technical scheme preparing primary ammonium phosphate byproduct in process orange tree composite fertilizer special occurs.
Therefore, the present inventor is main by a large amount of research and practices from element collocation needed for orange tree, adjusts the special efficient composite fertilizer that whole production technique and parameter by-product go out to be applicable to orange tree improving while phosphoric acid prepares the purity of primary ammonium phosphate product for the specific absorption of crop to required element.
Summary of the invention
For solving the problems of the technologies described above, the invention provides that a kind of loss of elements is few, environmental pollution is low, rationally, while improving primary ammonium phosphate product purity by-product can make orange tree element be carried out to the preparation method of the orange tree composite fertilizer special absorbed fully in element collocation.
The present invention is achieved by the following technical programs:
Prepare a method for primary ammonium phosphate by-product orange tree composite fertilizer special, the method comprises the following steps:
Prepared by a, raw material: the ratio being first 2:1.3 ~ 1.7 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 69 ~ 75%, is that 5 DEG C/min rises to 85-125 DEG C by heat-up rate, stirring reaction 25min, and obtained slip, is separated and obtains Ureaphil;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.1 ~ 3.7 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 25 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and orange tree obtains the mother liquor of orange tree composite fertilizer special;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, and after dry 25min, controlling water content is 4% obtain orange tree special fertilizer.
In described step a, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid, and phosphoric acid and urea mix for the ratio of 2:1.5 in molar ratio, and the concentration of phosphoric acid is 73%.
Described step c medium trace element compound is the inner complex of calcium, magnesium, and in the mother liquor of orange tree composite fertilizer special, the content of nitrogen element is 15.6%, Vanadium Pentoxide in FLAKES is 7.6%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.5%.
In described steps d, the nitrogen element content of orange tree composite fertilizer special is 15.3%, calcium element content is 3.9%, the content of magnesium elements is 4.2%, the content of Vanadium Pentoxide in FLAKES is 7.3%, the content of potassium element is 8.2%.
In described steps d, orange tree composite fertilizer special is chemical combination state Chemical Mixed Fertilizer.
Following N P and K chemical combination state is contained in its composition of orange tree composite fertilizer special in described steps d
Structural formula:
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: slip remaining while preparing highly purified primary ammonium phosphate by phosphoric acid and urea reaction can also be added by element, the techniques such as drying are prepared into the composite fertilizer special needed for orange tree, mother liquor is fully utilized, reduce cost, for the constituent content needed for orange tree and orange tree to the research and analysis of the specific absorption of element, the chemical combination state composite fertilizer requirement meeting orange tree to the full extent prepared, decrease the waste of element, avoid the residual soil contamination problem caused of composite fertilizer.
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:
First by the adjustment to phosphoric acid and urea reaction parameter, prepare Ureaphil, Ureaphil can continue to react with phosphoric acid to form H
2nCONH
3 +and H
2pO
4 -, H
2nCONH
3 +containing under the environment of phosphoric acid, formed when temperature is 85 ~ 120 DEG C
intermediate-ion and dihydrogen phosphate, after adding excessive ammonium radical ion, dihydrogen phosphate and ammonium radical ion react and generate primary ammonium phosphate and separate out, and the ammonium radical ion reaction after adding potassium ion and in intermediate-ion is formed
then add the inner complex of calcium constituent and magnesium elements, form chemical combination state composite fertilizer, after drying treatment, namely obtain orange tree composite fertilizer special.The reaction equation of above-mentioned reaction principle is as follows:
Chemical equation one:
H
2PO
3+CO(NH
2)
2—CO(NH
2)
2·H
3PO
4
Chemical equation two:
CO(NH
2)
2·H
3PO
4—H
2NCONH
3 ++H
2PO
4 -
Chemical equation three:
H
2PO
4 -+NH
4 +—NH
4H
2PO
4
Chemical equation four:
Chemical equation five:
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment one
Prepared by a, raw material: the ratio being first 2:1.3 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 69%, is that 5 DEG C/min rises to 85 DEG C by heat-up rate, stirring reaction 25min, obtained slip, be separated and obtain Ureaphil, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.1 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 25 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and orange tree obtains the mother liquor of orange tree composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of orange tree composite fertilizer special, the content of nitrogen element is 15.6%, Vanadium Pentoxide in FLAKES is 7.6%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, after dry 25min, controlling water content is 4% obtain orange tree special fertilizer, and the nitrogen element content of orange tree composite fertilizer special is 15.3%, calcium element content is 3.9%, the content of magnesium elements is 4.2%, the content of Vanadium Pentoxide in FLAKES is 7.3%, the content of potassium element is 8.2%.
Embodiment two
Prepared by a, raw material: the ratio being first 2:1.4 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 70%, is that 5 DEG C/min rises to 90 DEG C by heat-up rate, stirring reaction 25min, obtained slip, be separated and obtain Ureaphil, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.2 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 25 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and orange tree obtains the mother liquor of orange tree composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of orange tree composite fertilizer special, the content of nitrogen element is 15.6%, Vanadium Pentoxide in FLAKES is 7.6%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, after dry 25min, controlling water content is 4% obtain orange tree special fertilizer, and the nitrogen element content of orange tree composite fertilizer special is 15.3%, calcium element content is 3.9%, the content of magnesium elements is 4.2%, the content of Vanadium Pentoxide in FLAKES is 7.3%, the content of potassium element is 8.2%.
Embodiment three
Prepared by a, raw material: the ratio being first 2:1.5 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 71%, is that 5 DEG C/min rises to 95 DEG C by heat-up rate, stirring reaction 25min, obtained slip, be separated and obtain Ureaphil, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.3 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 25 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and orange tree obtains the mother liquor of orange tree composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of orange tree composite fertilizer special, the content of nitrogen element is 15.6%, Vanadium Pentoxide in FLAKES is 7.6%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, after dry 25min, controlling water content is 4% obtain orange tree special fertilizer, and the nitrogen element content of orange tree composite fertilizer special is 15.3%, calcium element content is 3.9%, the content of magnesium elements is 4.2%, the content of Vanadium Pentoxide in FLAKES is 7.3%, the content of potassium element is 8.2%.
Embodiment four
Prepared by a, raw material: the ratio being first 2:1.6 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 72%, is that 5 DEG C/min rises to 100 DEG C by heat-up rate, stirring reaction 25min, obtained slip, be separated and obtain Ureaphil, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.4 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 25 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and orange tree obtains the mother liquor of orange tree composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of orange tree composite fertilizer special, the content of nitrogen element is 15.6%, Vanadium Pentoxide in FLAKES is 7.6%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, after dry 25min, controlling water content is 4% obtain orange tree special fertilizer, and the nitrogen element content of orange tree composite fertilizer special is 15.3%, calcium element content is 3.9%, the content of magnesium elements is 4.2%, the content of Vanadium Pentoxide in FLAKES is 7.3%, the content of potassium element is 8.2%.
Embodiment five
Prepared by a, raw material: the ratio being first 2:1.6 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 70%, is that 5 DEG C/min rises to 105 DEG C by heat-up rate, stirring reaction 25min, obtained slip, be separated and obtain Ureaphil, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.6 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 25 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and orange tree obtains the mother liquor of orange tree composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of orange tree composite fertilizer special, the content of nitrogen element is 15.6%, Vanadium Pentoxide in FLAKES is 7.6%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, after dry 25min, controlling water content is 4% obtain orange tree special fertilizer, and the nitrogen element content of orange tree composite fertilizer special is 15.3%, calcium element content is 3.9%, the content of magnesium elements is 4.2%, the content of Vanadium Pentoxide in FLAKES is 7.3%, the content of potassium element is 8.2%.
Embodiment six
Prepared by a, raw material: the ratio being first 2:1.7 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 75%, is that 5 DEG C/min rises to 125 DEG C by heat-up rate, stirring reaction 25min, obtained slip, be separated and obtain Ureaphil, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.7 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 25 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and orange tree obtains the mother liquor of orange tree composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of orange tree composite fertilizer special, the content of nitrogen element is 15.6%, Vanadium Pentoxide in FLAKES is 7.6%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, after dry 25min, controlling water content is 4% obtain orange tree special fertilizer, and the nitrogen element content of orange tree composite fertilizer special is 15.3%, calcium element content is 3.9%, the content of magnesium elements is 4.2%, the content of Vanadium Pentoxide in FLAKES is 7.3%, the content of potassium element is 8.2%.
Below in conjunction with specific experiment example, product of the present invention and technique effect are further described.
Experimental example one
The primary ammonium phosphate product prepared in the embodiment of the present invention one, embodiment two, embodiment three, embodiment four, embodiment five, embodiment six detects by the standard of GB25569-2010,
Detected result is as shown in table 1:
Table 1
Primary ammonium phosphate product purity of the present invention detects
| Primary ammonium phosphate | Criterion of acceptability | Embodiment one | Embodiment two | Embodiment three | Embodiment four | Embodiment five | Embodiment six |
| Purity >=% | 96 | 98.2 | 98.3 | 98.4 | 98.2 | 98.1 | 98.3 |
| Moisture≤% | 0.5 | 0.4 | 0.4 | 0.41 | 0.43 | 0.42 | 0.42 |
As can be seen from Table 1, the primary ammonium 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 primary ammonium phosphate product and had significant progress.
Experimental example two
According to the absorption of orange tree to constituent content and the growing state of orange tree, test is compared to orange tree composite fertilizer special and Common compound fertilizer.With 9 orange trees for subjects, label is A, B, C, D, E, F, G, H, I, uses common fertilizer to the orange tree of A, B, C tri-labels respectively, use orange tree special fertilizer prepared in embodiment one, embodiment two, embodiment three, embodiment four, embodiment five, embodiment six respectively to the orange tree of six labels such as D, E, F, G, H, I, contrast and experiment is as shown in table 2:
Table 2 use Common compound fertilizer and orange tree composite fertilizer special on orange tree element absorption rate on when on the impact that orange tree grows
The orange tree composite fertilizer special that as can be seen from the above table prepared by the present invention can be absorbed fully by orange tree, and the nutritive element be rich in needed for the orange trees such as Ca, Me, guarantee is provided to the normal growth of orange tree, improve the growing way of orange tree, add the output of orange, thus improve economic benefit.
Claims (6)
1. prepare a method for primary ammonium phosphate by-product orange tree composite fertilizer special, it is characterized in that, the method comprises the following steps:
Prepared by a, raw material: the ratio being first 2:1.3-1.7 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 69-75%, is that 5 DEG C/min rises to 85-125 DEG C by heat-up rate, stirring reaction 25min, and obtained slip, is separated and obtains Ureaphil;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.1-3.7 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 25 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and orange tree obtains the mother liquor of orange tree composite fertilizer special;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, and after dry 25min, controlling water content is 4% obtain orange tree special fertilizer.
2. the method preparing primary ammonium phosphate by-product orange tree composite fertilizer special according to claim 1, it is characterized in that: in described step a, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid, phosphoric acid and urea mix for the ratio of 2:1.5 in molar ratio, and the concentration of phosphoric acid is 73%.
3. the method preparing primary ammonium phosphate by-product orange tree composite fertilizer special according to claim 1, it is characterized in that: described step c medium trace element compound is the inner complex of calcium, magnesium, in the mother liquor of orange tree composite fertilizer special, the content of nitrogen element is 15.6%, Vanadium Pentoxide in FLAKES is 7.6%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.5%.
4. the method preparing primary ammonium phosphate by-product orange tree composite fertilizer special according to claim 1, is characterized in that: in described steps d, the nitrogen element content of orange tree composite fertilizer special is 15.3%, calcium element content is 3.9%, the content of magnesium elements is 4.2%, the content of Vanadium Pentoxide in FLAKES is 7.3%, the content of potassium element is 8.2%.
5. the method preparing primary ammonium phosphate by-product orange tree composite fertilizer special according to claim 1, is characterized in that: in described steps d, orange tree composite fertilizer special is chemical combination state Chemical Mixed Fertilizer.
6. the method preparing primary ammonium phosphate by-product orange tree composite fertilizer special according to claim 1, is characterized in that: contain following N P and K chemical combination state structural formula in its composition of orange tree composite fertilizer special in described steps d:
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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046226A (en) * | 2017-12-22 | 2018-05-18 | 贵阳开磷化肥有限公司 | A kind of production method of PHOSPHORIC ACID TECH.GRADE dihydro coproducing ammonium Water soluble fertilizer |
Citations (6)
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| GB1191635A (en) * | 1966-07-27 | 1970-05-13 | Marchon Products Ltd | Improvements in the manufacture of Orthophosphates |
| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| WO2000055104A1 (en) * | 1999-03-18 | 2000-09-21 | Oms Investments, Inc. | Processes for preparing granular composite fertilizer compositions and products produced thereby |
| CN1583681A (en) * | 2004-05-24 | 2005-02-23 | 陈天骏 | Agricultural composite manure and preparing method thereof |
| 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 |
| CN104016322A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for diammonium hydrogen phosphate |
-
2014
- 2014-09-19 CN CN201410477886.9A patent/CN104310330B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1191635A (en) * | 1966-07-27 | 1970-05-13 | Marchon Products Ltd | Improvements in the manufacture of Orthophosphates |
| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| WO2000055104A1 (en) * | 1999-03-18 | 2000-09-21 | Oms Investments, Inc. | Processes for preparing granular composite fertilizer compositions and products produced thereby |
| CN1583681A (en) * | 2004-05-24 | 2005-02-23 | 陈天骏 | Agricultural composite manure and preparing method thereof |
| 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 |
| CN104016322A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for diammonium hydrogen phosphate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046226A (en) * | 2017-12-22 | 2018-05-18 | 贵阳开磷化肥有限公司 | A kind of production method of PHOSPHORIC ACID TECH.GRADE dihydro coproducing ammonium Water soluble fertilizer |
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Effective date of registration: 20161031 Address after: 550000 Huaxi District, Guizhou, Guiyang Applicant after: Guizhou University Applicant after: Phosphorylcholine group limited-liability company is opened in Guizhou Applicant after: Guizhou Ke Xinhua smelting company limited Address before: 550000 Huaxi District, Guizhou, Guiyang Applicant before: Guizhou University Applicant before: Zhonghuakai Phosphorous Chemical Fertilizer Co., Ltd., Guiyang Applicant before: Guizhou Ke Xinhua smelting company limited |
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