CN117800378A - Batching method for integrally producing ammonium calcium nitrate solution - Google Patents

Batching method for integrally producing ammonium calcium nitrate solution Download PDF

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Publication number
CN117800378A
CN117800378A CN202311721825.8A CN202311721825A CN117800378A CN 117800378 A CN117800378 A CN 117800378A CN 202311721825 A CN202311721825 A CN 202311721825A CN 117800378 A CN117800378 A CN 117800378A
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CN
China
Prior art keywords
solution
nitrate solution
calcium nitrate
dilute
nitric acid
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Pending
Application number
CN202311721825.8A
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Chinese (zh)
Inventor
崔瑞波
李腾飞
张梓榆
吕聪
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Shanxi Huaxin Fertilizer Corp
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Shanxi Huaxin Fertilizer Corp
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Priority to CN202311721825.8A priority Critical patent/CN117800378A/en
Publication of CN117800378A publication Critical patent/CN117800378A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/36Nitrates
    • C01F11/42Double salts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • B01J19/242Tubular reactors in series
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C1/00Ammonium nitrate fertilisers
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C5/00Fertilisers containing other nitrates
    • C05C5/04Fertilisers containing other nitrates containing calcium nitrate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

The invention belongs to the field of chemical industry, and particularly relates to a dosing method for integrally producing an ammonium calcium nitrate solution. S1, uniformly mixing dilute calcium nitrate solution and nitric acid solution according to a proportion to obtain mixed solution; s2, introducing an ammonia water solution into the mixed solution to react, and obtaining the ammonium calcium nitrate solution after the reaction is finished; the flow rate of the dilute calcium nitrate solution is used as a main parameter, the flow rate of the nitric acid solution is regulated in a ratio mode according to the flow rate of the dilute calcium nitrate solution, and the flow rate of the ammonia water solution is regulated in a ratio mode according to the flow rate of the nitric acid solution. The batching method provided by the invention comprises the steps of mixing filtrate with nitric acid solution, introducing ammonia water, and reacting to obtain the ammonium calcium nitrate dilute solution. The whole process does not need dangerous chemical ammonium nitrate solution, ensures the safety of production, and promotes the development of ammonium nitrate production enterprises.

Description

Batching method for integrally producing ammonium calcium nitrate solution
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a dosing method for integrally producing an ammonium calcium nitrate solution.
Background
Calcium ammonium nitrate is a compound fertilizer with a chemical formula of (5 Ca (NO 3 ) 2 ·NH 4 NO 3 ·10H 2 O) is white round granulation, is extremely easy to dissolve in water, has stronger hygroscopicity, caking property and explosive property, is a novel high-efficiency compound fertilizer containing nitrogen and quick-acting calcium, has the characteristic of quick nitrogen supplementation, wherein calcium is added, and the nutrient is more comprehensive than ammonium nitrate, so that plants can directly absorb the fertilizer. The calcium ammonium nitrate has wide application, is suitable for various soils and crops, and is widely applied to grain crops, cash crops, flowers, fruit trees, vegetables and the like planted in greenhouses and fields. Nitrate nitrogen in calcium ammonium nitrate is not required to be converted in soil, is rapidly dissolved in water and is directly absorbed by plants, and the method is suitable for base fertilizer, seed fertilizer and additional fertilizer.
At present, the process for preparing the ammonium nitrate and the calcium nitrate in China basically adopts the process of mixing the calcium nitrate dilute solution and the ammonium nitrate dilute solution according to a proportion, and the ammonium nitrate solution belongs to national important supervision dangerous chemicals, so that a process for preparing the ammonium nitrate and the calcium nitrate instead of the ammonium nitrate solution is needed.
Disclosure of Invention
The invention mainly aims to provide a dosing method for integrally producing an ammonium calcium nitrate solution, which aims to overcome the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
according to an aspect of the embodiment of the invention, there is provided a batching method for integrally producing an ammonium calcium nitrate solution, comprising the steps of:
s1, uniformly mixing dilute calcium nitrate solution and nitric acid solution according to a proportion to obtain mixed solution;
s2, introducing an ammonia water solution into the mixed solution to react, and obtaining the ammonium calcium nitrate solution after the reaction is finished;
the flow rate of the dilute calcium nitrate solution is used as a main parameter, the flow rate of the nitric acid solution is regulated in a ratio mode according to the flow rate of the dilute calcium nitrate solution, and the flow rate of the ammonia water solution is regulated in a ratio mode according to the flow rate of the nitric acid solution.
Further, the mass ratio of the calcium nitrate to the nitric acid to the ammonia water after folding is 45.6:3.5:1.
Further, the flow rates of the dilute calcium nitrate solution, the nitric acid solution and the ammonia water solution are controlled by a mass flowmeter and a flow regulating valve.
Further, the dilute calcium nitrate solution and the nitric acid solution are mixed in a primary mixing section of the multi-tube reactor.
Further, the mixed solution of the dilute calcium nitrate solution and the nitric acid solution is reacted in a reaction section of the multi-tube reactor.
Further, the mass percentage concentration of the ammonia water is 10-20%; preferably, the mass percentage concentration of the ammonia water is 15%.
Furthermore, the batching method for integrally producing the ammonium calcium nitrate solution further comprises a step S3 of adjusting the pH value of the ammonium calcium nitrate dilute solution, wherein the final pH value is 5-6.
Further, the dilute calcium ammonium nitrate solution is added with acid in the final mixing section of the multi-tube reactor for pH adjustment.
Further, the mass percentage concentration of the nitric acid solution is 45-60%.
Further, the preparation method of the dilute calcium nitrate solution comprises the steps of reacting limestone and nitric acid through an acidolysis tower to generate a dilute calcium nitrate solution, and removing insoluble substances from the dilute calcium nitrate solution through a filter press to obtain the dilute calcium nitrate solution.
Compared with the prior art, the invention has the advantages that:
the invention provides a batching method for integrally producing ammonium calcium nitrate solution, which comprises the steps of mixing filtrate with nitric acid solution, introducing ammonia water, and reacting to obtain the ammonium calcium nitrate dilute solution; the whole process does not need dangerous chemical ammonium nitrate solution, ensures the safety of production, and promotes the development of ammonium nitrate production enterprises. The flow of the dilute calcium nitrate solution is used as a main parameter in the whole process, the flow of the nitric acid solution is regulated in a ratio mode according to the flow of the dilute calcium nitrate solution, the flow of the ammonia water solution is regulated in a ratio mode according to the flow of the nitric acid solution, and proportioning regulation can be better carried out, so that the ammonium calcium nitrate solution with higher quality is produced.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to designate like parts throughout the figures. In the drawings:
FIG. 1 is a schematic diagram of a control system for integrated production of calcium ammonium nitrate in accordance with an exemplary embodiment of the present invention;
the marks in the figure: the device comprises a tubular reactor 1, a first nitric acid tank 2, a second nitric acid tank 3, an ammonia water tank 4, a dilute calcium nitrate tank 5, a mass flowmeter 6, a flow regulating valve 7, a sampling cooler 8, a pH meter 9 and a nitric acid regulating valve 10.
Detailed Description
In view of the shortcomings in the prior art, the inventor of the present invention has long studied and practiced in a large number of ways to propose the technical scheme of the present invention. The technical scheme, the implementation process, the principle and the like are further explained as follows.
The following detailed description of the invention is provided in connection with the accompanying drawings that are presented to illustrate the invention and not to limit the scope thereof. The examples provided below are intended as guidelines for further modifications by one of ordinary skill in the art and are not to be construed as limiting the invention in any way.
The experimental methods in the following examples, unless otherwise specified, are conventional methods, and are carried out according to techniques or conditions described in the literature in the field or according to the product specifications. Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
An aspect of the embodiment of the invention provides a batching method for integrally producing an ammonium calcium nitrate solution, which comprises the following steps:
s1, uniformly mixing dilute calcium nitrate solution and nitric acid solution with the mass percent concentration of 45-60% in a primary mixing section of a multi-tube reactor according to a proportion to obtain mixed solution;
s2, introducing 10-20% ammonia water solution into the mixed solution in a reaction section of the multitube reactor for reaction, and obtaining the ammonium calcium nitrate solution after the reaction is finished;
s3, adjusting the pH value of the ammonium calcium nitrate dilute solution in a final mixing section of the multi-tube reactor, wherein the final pH value is 5-6;
the flow rate of the dilute calcium nitrate solution is used as a main parameter, the flow rate of the nitric acid solution is regulated in a ratio mode according to the flow rate of the dilute calcium nitrate solution, and the flow rate of the ammonia water solution is regulated in a ratio mode according to the flow rate of the nitric acid solution.
Preferably, the mass ratio of the calcium nitrate to the nitric acid to the ammonia water after folding is 45.6:3.5:1.
Preferably, the flow rates of the dilute calcium nitrate solution, the nitric acid solution and the ammonia water solution are controlled by a mass flowmeter and a flow regulating valve.
Preferably, the mass percentage concentration of the ammonia water is 15%.
Preferably, the preparation method of the dilute calcium nitrate solution comprises the steps of reacting limestone and nitric acid through an acidolysis tower to generate a dilute calcium nitrate solution, and removing insoluble substances from the dilute calcium nitrate solution through a filter press to obtain the dilute calcium nitrate solution.
In implementations, the following system may also be employed for control operations.
As shown in fig. 1, the embodiment of the invention provides a control system for integrally producing calcium ammonium nitrate, which comprises a tubular reactor 1, a first nitric acid tank 2 loaded with nitric acid, a second nitric acid tank 3 loaded with nitric acid, an ammonia water tank 4 loaded with ammonia water, a dilute calcium nitrate liquid tank 5 loaded with dilute calcium nitrate liquid, and a control device, wherein the outlets of the first nitric acid tank 2 and the dilute calcium nitrate liquid tank 5 are respectively connected with the inlet of the tubular reactor 1;
the tubular reactor 1 comprises a first-stage mixing section, a reaction section and a final-stage mixing section, wherein the first-stage mixing section and the final-stage mixing section are respectively arranged at two ends of the reaction section, a first liquid inlet is formed in the reaction section, a second liquid inlet is formed in the final-stage mixing section, an outlet of the ammonia tank 4 is connected with the first liquid inlet in the reaction section, and an outlet of the second nitric acid tank 3 is connected with the second liquid inlet in the final-stage mixing section; in a specific implementation, the tubular reactor 1 is selected from SK-type multitubular reactors 1;
the control device comprises a flow control module and a pH control module, wherein the flow control module is used for adjusting the liquid discharge flow of the first nitric acid tank 2, the ammonia water tank 4 and the dilute calcium nitrate tank 5; the pH control module is used for adjusting the pH value of the liquid discharged from the final mixing section; the outlets of the first nitric acid tank 2, the ammonia water tank 4 and the dilute calcium nitrate tank 5 are provided with a mass flowmeter 6 and a flow regulating valve 7,
the pH control module comprises a sampling cooler 8, a pH meter 9 and a nitric acid regulating valve 10, the nitric acid regulating valve 10 being used to regulate the liquid discharge flow in the second nitric acid tank 3.
For a better understanding of the technical solution of the present invention, the following describes the present invention in detail with reference to specific embodiments.
Example 1
The embodiment provides a batching method for integrally producing an ammonium calcium nitrate solution, which comprises the following steps:
s1, uniformly mixing dilute calcium nitrate solution and nitric acid solution with the mass percent concentration of 45% in a primary mixing section of a multi-tube reactor in proportion to obtain mixed solution;
s2, introducing ammonia water solution with the mass percent concentration of 10% into the mixed solution in a reaction section of the multi-tube reactor to react, and obtaining the ammonium calcium nitrate solution after the reaction is finished;
s3, adjusting the pH value of the ammonium calcium nitrate dilute solution in a final mixing section of the multi-tube reactor, wherein the final pH value is 5;
the flow rate of the dilute calcium nitrate solution is used as a main parameter, the flow rate of the nitric acid solution is regulated in a ratio mode according to the flow rate of the dilute calcium nitrate solution, and the flow rate of the ammonia water solution is regulated in a ratio mode according to the flow rate of the nitric acid solution. The mass ratio of the calcium nitrate to the nitric acid to the ammonia water after folding is 45.6:3.5:1.
The preparation method of the dilute calcium nitrate solution comprises the steps of reacting limestone and nitric acid through an acidolysis tower to generate a dilute calcium nitrate solution, and removing insoluble substances from the dilute calcium nitrate solution through a filter press to obtain the dilute calcium nitrate solution.
Example 2
The embodiment provides a batching method for integrally producing an ammonium calcium nitrate solution, which comprises the following steps:
s1, uniformly mixing dilute calcium nitrate solution and nitric acid solution with the mass percent concentration of 60% in a primary mixing section of a multi-tube reactor in proportion to obtain mixed solution;
s2, introducing an ammonia water solution with the mass percent concentration of 20% into the mixed solution in a reaction section of the multi-tube reactor to react, and obtaining the ammonium calcium nitrate solution after the reaction is finished;
s3, adjusting the pH value of the ammonium calcium nitrate dilute solution in a final mixing section of the multi-tube reactor, wherein the final pH value is 5-6;
the flow rate of the dilute calcium nitrate solution is used as a main parameter, the flow rate of the nitric acid solution is regulated in a ratio mode according to the flow rate of the dilute calcium nitrate solution, and the flow rate of the ammonia water solution is regulated in a ratio mode according to the flow rate of the nitric acid solution. The mass ratio of the calcium nitrate to the nitric acid to the ammonia water after folding is 45.6:3.5:1.
The preparation method of the dilute calcium nitrate solution comprises the steps of reacting limestone and nitric acid through an acidolysis tower to generate a dilute calcium nitrate solution, and removing insoluble substances from the dilute calcium nitrate solution through a filter press to obtain the dilute calcium nitrate solution.
Example 3
The embodiment provides a batching method for integrally producing an ammonium calcium nitrate solution, which comprises the following steps:
s1, uniformly mixing dilute calcium nitrate solution and nitric acid solution with the mass percent concentration of 52.5% in a primary mixing section of a multi-tube reactor according to a proportion to obtain mixed solution;
s2, introducing an ammonia water solution with the mass percent concentration of 15% into the mixed solution in a reaction section of the multi-tube reactor to react, and obtaining the ammonium calcium nitrate solution after the reaction is finished;
s3, adjusting the pH value of the ammonium calcium nitrate dilute solution in a final mixing section of the multi-tube reactor, wherein the final pH value is 5.5;
the flow rate of the dilute calcium nitrate solution is used as a main parameter, the flow rate of the nitric acid solution is regulated in a ratio mode according to the flow rate of the dilute calcium nitrate solution, and the flow rate of the ammonia water solution is regulated in a ratio mode according to the flow rate of the nitric acid solution. The mass ratio of the calcium nitrate to the nitric acid to the ammonia water after folding is 45.6:3.5:1.
The preparation method of the dilute calcium nitrate solution comprises the steps of reacting limestone and nitric acid through an acidolysis tower to generate a dilute calcium nitrate solution, and removing insoluble substances from the dilute calcium nitrate solution through a filter press to obtain the dilute calcium nitrate solution.
While only certain embodiments of the present invention have been described, it will be apparent to those skilled in the art that other modifications and improvements can be made without departing from the inventive concept of the present invention.

Claims (10)

1. The batching method for integrally producing the ammonium calcium nitrate solution is characterized by comprising the following steps of:
s1, uniformly mixing dilute calcium nitrate solution and nitric acid solution according to a proportion to obtain mixed solution;
s2, introducing an ammonia water solution into the mixed solution to react, and obtaining the ammonium calcium nitrate solution after the reaction is finished;
the flow rate of the dilute calcium nitrate solution is used as a main parameter, the flow rate of the nitric acid solution is regulated in a ratio mode according to the flow rate of the dilute calcium nitrate solution, and the flow rate of the ammonia water solution is regulated in a ratio mode according to the flow rate of the nitric acid solution.
2. The dosing method for integrally producing a calcium ammonium nitrate solution according to claim 1, wherein: the mass ratio of the calcium nitrate to the nitric acid to the ammonia water after folding is 45.6:3.5:1.
3. The dosing method for integrally producing a calcium ammonium nitrate solution according to claim 1, wherein: the flow rates of the dilute calcium nitrate solution, the nitric acid solution and the ammonia water solution are controlled by a mass flowmeter and a flow regulating valve.
4. The dosing method for integrally producing a calcium ammonium nitrate solution according to claim 1, wherein: the dilute calcium nitrate solution and the nitric acid solution are mixed in a primary mixing section of the multi-tube reactor.
5. The dosing method for integrally producing a calcium ammonium nitrate solution according to claim 1, wherein: the mixed solution of the dilute calcium nitrate solution and the nitric acid solution reacts in the reaction section of the multi-tube reactor.
6. The dosing method for integrally producing a calcium ammonium nitrate solution according to claim 1, wherein: the mass percentage concentration of the ammonia water is 10-20%.
7. The dosing method for integrally producing a calcium ammonium nitrate solution according to claim 1, wherein: and the method also comprises a step S3 of adjusting the pH value of the ammonium calcium nitrate dilute solution, wherein the final pH value is 5-6.
8. The method for integrally preparing the ammonium calcium nitrate solution according to claim 7, wherein the method comprises the following steps: the dilute calcium ammonium nitrate solution is added with acid in the final mixing section of the multi-tube reactor for pH adjustment.
9. The dosing method for integrally producing a calcium ammonium nitrate solution according to claim 1, wherein: the mass percentage concentration of the nitric acid solution is 45-60%.
10. The dosing method for integrally producing a calcium ammonium nitrate solution according to claim 1, wherein: the preparation method of the dilute calcium nitrate solution comprises the steps of reacting limestone and nitric acid through an acidolysis tower to generate a dilute calcium nitrate solution, and removing insoluble substances from the dilute calcium nitrate solution through a filter press to obtain the dilute calcium nitrate solution.
CN202311721825.8A 2023-12-14 2023-12-14 Batching method for integrally producing ammonium calcium nitrate solution Pending CN117800378A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311721825.8A CN117800378A (en) 2023-12-14 2023-12-14 Batching method for integrally producing ammonium calcium nitrate solution

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Application Number Priority Date Filing Date Title
CN202311721825.8A CN117800378A (en) 2023-12-14 2023-12-14 Batching method for integrally producing ammonium calcium nitrate solution

Publications (1)

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CN117800378A true CN117800378A (en) 2024-04-02

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