CN1223511C - Novel process for producing calcium nitrite - Google Patents
Novel process for producing calcium nitrite Download PDFInfo
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- CN1223511C CN1223511C CN 02134123 CN02134123A CN1223511C CN 1223511 C CN1223511 C CN 1223511C CN 02134123 CN02134123 CN 02134123 CN 02134123 A CN02134123 A CN 02134123A CN 1223511 C CN1223511 C CN 1223511C
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Abstract
The demand of calcium nitrite as superior cement additives is large, and the calcium nitrite only can be prepared from nitric acid nitric oxide under the pressure of 0.2MPa at home and abroad, which has the disadvantages of bulky equipment, low production efficiency and high product cost. The new process orderly comprises a primary absorption reaction step of oxidized nitrogen gas and lime cream, a secondary gas-liquid separation step after the reaction, a deposition step of partial mixed solution after the separation, and a neutralization reaction step of Ca(OH)2 remaining in the supernatant liquid of calcium nitrite after the deposition. The present invention is characterized in that before the primary absorption reaction step, the method also comprises a nitric oxide regulation step for regulating the concentration of NO in the oxidized nitrogen gas with high density, and a nitric oxide supplement step for supplementing the required oxidized nitrogen gas for the absorption reaction and the neutralization reaction and regulating the ratio of NO to NOx required by the reactions, and the process flow adopts a forward flow reaction step of the oxidized nitrogen gas and the lime cream. The present invention has the advantages of capability of using high-pressure oxidized nitrogen gas as raw materials, high reaction speed, small equipment volume, short process flow, high production efficiency and low production cost.
Description
Technical Field
The present invention relates to a technological process for industrial production of calcium nitrite and its equipment, in the concrete, it relates to a new technological process for producing calcium nitrite by using high-pressure nitrogen oxide gas and lime milk as raw material and its equipment.
Background
Calcium nitrite is the newly found optimal cement additive, and the demand amount is large. At present, nitric oxide gas with pressure less than 0.2MPa is used for production at home and abroad. Because the pressure is low, the production equipment is huge, the production efficiency is low, and the product cost is high. The pressure of nitric oxide gas of nitric acid produced in China is generally 0.35-0.9 MPa, and manufacturers try to produce sodium nitrite under the condition of 0.35MPa nitric oxide gas, and the failure is ended. The method for producing calcium nitrite by adopting the existing low-pressure nitrogen oxide gas far cannot meet the market demand, and a new method and related production equipment for producing calcium nitrite under the condition of high-pressure nitrogen oxide gas are needed to be found.
Disclosure of Invention
The invention aims to: the invention provides a new process method for producing calcium nitrite to meet market demand by using high-pressure nitrogen oxide gas and lime milk as raw materials by combining the national conditions of enterprises in China for producing nitric oxide gas, and the invention also aims to provide production equipment for implementing the process.
The purpose of the invention is realized by implementing the following technical scheme:
a process for producing calcium nitrite comprises a first-stage absorption reaction process of nitrogen oxide gas and lime milk in sequence; a first stage gas-liquid separation process; a second stage absorption reaction step of separating unreacted gas and partial reaction mixture; a second stage gas-liquid separation process after the reaction is finished; a step of precipitating and extracting calcium nitrate from the separated part of the mixed solution; carrying out neutralization reaction on residual hydro-calcium oxide in the precipitated calcium nitrite supernatant to complete the neutralization reaction process of calcium nitrite solution production; the method is characterized in that: before the first stage absorptionreaction step, the high pressure nitrogen oxide gas of 0.3-0.9 MPa is adjusted to make NO/(NO) of the gas2+ NO) ratio of the nitrogen oxide gas reaches the optimal value of 0.3-0.6; and supplementing nitrogen oxide gas required for the second-stage absorption reaction and neutralization reaction process, and regulating NO/(NO) required by the reaction2A step of replenishing a nitrogen oxide gas having a + NO) ratio; after the first and second two-stage gas-liquid separation processes, a process of pressurizing, cooling and cooling part of the reaction mixed liquid, returning the reaction mixed liquid to the front stage, spraying the reaction mixed liquid by an injector, and carrying out absorption reaction with the front stage high-pressure nitrogen oxide gas with 0.3-0.9 MPa in the tower respectively is provided.
The equipment using the process comprises four main equipment, namely a first-stage absorption reaction tower, a second-stage absorption reaction tower, a precipitation tank and a neutralization tower, which are sequentially arranged; wherein, the bottoms of the first-stage absorption reaction tower and the second-stage absorption reaction tower are respectively provided with a gas-liquid separator; the gas-liquid separator at the bottom of the first-stage absorption reaction tower is connected with the top of the second-stage absorption reaction tower through an upper output pipeline of the first-stage absorption reaction tower, and is connected with the gas-liquid separator at the bottom of the second-stage absorption reaction tower through a lower output pipeline of the second-stage absorption reaction tower, a pressure circulating pump and a liquid flow pipe; the gas-liquid separator at the bottom of the second-stage absorption reaction tower is connected with a tail gas main discharge pipe at the upper part, and a pipeline is connected with a precipitation tank at the lower part; the bottom of the precipitation tank is provided with a calcium nitrate precipitation discharge pipe, the top of the precipitation tank is provided with a supernatant discharge pipe, and the supernatant discharge pipe is connected with the top of the neutralization tower through a pressure pump and a liquid conveying pipeline; one path of the neutralization tower is connected with a tail gas main discharge pipe through a tail gas discharge pipe at the top of the neutralization tower, and the other path of the neutralization tower is a discharge pipe with a calcium nitrite solution at the bottom of the neutralization tower, and the neutralization tower is characterized in that: (a) an oxidizer is arranged in front of the first-stage absorption reaction tower, one path of the oxidizer is connected with the top of the first-stage absorption reaction tower through a gas pipe, the other path of the oxidizer is divided into two branch pipelines through a pipeline, one branch pipeline is connected with the top of the second-stage absorption reaction tower through a switch valve, and the other branch pipeline is connected with the bottom of the neutralization tower through a switch valve; (b) a water cooler for cooling the high-pressure and high-temperature nitrogen oxide gas with the pressure of 0.3-0.9 MPa to 150-250 ℃ is arranged in front of the oxidizer; (c) an input pipeline for returning part of the mixed liquid is arranged on the top of the first-stage absorption reaction tower, the pipeline is connected with a liquid flow pipe connected with a gas-liquid separator at the bottom of the second-stage absorption reaction tower through a water cooler, and the input pipeline for returning part of the mixed liquid is arranged on the top of the second-stage absorption reaction tower and is connected with a liquid flow return pipeline which flows out of the gas-liquid separator at the bottom of the second-stage absorption reaction tower through the water cooler and passes through a pressure circulating pump; (d) and ejectors for ejecting the mixed liquid returned by the pipeline to react with the high-pressure nitrogen oxide gas with the pressure of 0.3-0.9 MPa are respectively arranged at the tops of the first-stage absorption reaction tower and the second-stage absorption reaction tower.
The invention has the advantages that: as the invention uses 0.3-0.9 MPa high-pressure nitrogen oxide gas as raw material, the NO/NO of the nitrogen oxide gas entering the absorption tower is conveniently and accurately regulated by adopting the oxidizerXAnd the circulating return mixed liquid is sprayed by the sprayers at the tops of the first-stage absorption reaction tower and the second-stage absorption reaction tower to react with the nitrogen oxide gas, so that the reaction rate is increased, the process flow is shortened, the production efficiency is greatly improved, and the production cost is greatly reduced to meet the market demand.
Drawings
FIG. 1 is a process flow diagram of the present invention
FIG. 2 is a schematic diagram of the structure of the apparatus of the present invention, labeled: 1 is a first-stage absorption reaction tower, 2 is a second-stage absorption reaction tower, 3 is a neutralization tower, 4, 5 and 6 are water coolers, 7 and 8 are pressure circulating pumps, 9 is a pressure pump, 10 is an oxidizer, 11 is a precipitation tank, 12 and 13 are separators at the bottoms of the first and second-stage absorption reaction towers respectively, 14 and 15 are ejectors at the tops of the first and second-stage absorption reaction towers respectively, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 30, 31, 32, 33 and 34 are pipelines respectively, wherein 18 is a liquid flow pipe, 20 is a tail gas total discharge pipe, 21 is a liquid conveying pipeline, 22 is a supernatant pipe, 23 is a calcium nitrate precipitation discharge pipe, 32 and 33 are input pipelines for returning part of mixed liquid connected with the tops of the first and second-stage absorption reaction towers respectively, and 34 is a liquid flow return pipeline; 28. and 29 is a valve.
Detailed Description
The process equipment comprises four main devices, namely a first-stage absorption reaction tower 1, a second-stage absorption reaction tower 2, a precipitation tank 11 and a neutralization tower 3 which are sequentially arranged; wherein the bottoms of the first-stage absorption reaction tower and the second-stage absorption reaction tower are respectively provided with a gas-liquid separator; the gas-liquid separator 12 at the bottom of the first-stage absorption reaction tower is connected with the top of the second-stage absorption reaction tower 2 through an upper output pipeline 16, and is connected with the gas-liquid separator 13 at the bottom of the second-stage absorption reaction tower through a lower output pipeline 17, a pressure circulating pump 7 and a liquid flow pipe 18; the gas-liquid separator 13 at the bottom of the second-stage absorption reaction tower is connected with a tail gas main discharge pipe 20, and the lower pipeline 19 is connected with the settling tank 11; the bottom of the precipitation tank 11 is provided with a calcium nitrate precipitation discharge pipe 23, the top is provided with a supernatant discharge pipe 22, and the supernatant discharge pipe is connected with the top of the neutralization tower 3 through a pressure pump 9 and a liquid conveying pipeline 21; one path of the neutralization tower 3 is connected with a tail gas main discharge pipe 20 through a tail gas discharge pipe 25 at the top part of the neutralization tower, and the other path is a discharge pipe 24 which is provided with calcium nitrite solution at the bottom partof the neutralization tower, and the neutralization tower is characterized in that: (a) an oxidizer 10 is arranged in front of the first-stage absorption reaction tower 1, one path of the oxidizer is connected with the top of the first-stage absorption reaction tower through a gas pipe 26, the other path of the oxidizer is divided into two branch pipelines through a pipeline 27, one branch pipeline 30 is connected with the top of the second-stage absorption reaction tower through a switch valve 28, and the other branch pipeline 31 is connected with the bottom of the neutralization tower 3 through a switch valve 29; (b) a water cooler 4 for cooling the high-pressure and high-temperature nitrogen oxide gas with the pressure of 0.3-0.9 MPa to 150-250 ℃ is arranged in front of the oxidizer 10; (c) an input pipeline 32 for returning part of the mixed liquid is arranged at the top of the first-stage absorption reaction tower, the pipeline 32 is connected with a liquid flow pipe 18 connected with a gas-liquid separator at the bottom of the second-stage absorption reaction tower through a water cooler 5, an input pipeline 33 for returning part of the mixed liquid is arranged at the top of the second-stage absorption reaction tower, and the pipeline 33 is connected with a liquid flow return pipeline 34 which is discharged from the gas-liquid separator 13 at the bottom of the second-stage absorption reaction tower and passes through a pressure circulating pump 8 through a water cooler 6; (d) ejectors 14 and 15 for ejecting the mixed liquid returned through the pipelines 32 and 33 to react with the high-pressure nitrogen oxide gas with the pressure of 0.3-0.9 MPa are respectively arranged at the top parts in the first-stage absorption reaction tower and the second-stage absorption reaction tower.
The production process of the invention comprises the following steps:
high-temperature nitrogen oxide gas of 0.3-0.9 MPa And the temperature is reduced to 150-250 ℃ through a water cooler 4, and the mixture is conveyed to an oxidizer 10, and the concentration of NO is adjusted, so that the ratio of NO: NOXThe ratio of (A) is 0.3-0.6, then the lime milk is conveyed into a first-stage absorption reaction tower through a pipeline 26, fresh lime milk with the weight ratio concentration of 9-13% is conveyed into the absorption tower from the bottom of the tower 1, absorption reaction is carried out in the tower, and nitrogen oxide gas NO is generatedXNO and NO in (1)2And Ca (OH)2Reacting to generate calcium nitrite and a small amount of calcium nitrate, and separating gas and liquid in a gas-liquid mixture obtained after the reaction in a tower bottom separator 12; unreacted gas enters the absorption reaction tower 2 through the top of the second-stage absorption reaction tower through a pipeline 16; separated from separator 12 via conduit 17 and composed of calcium nitrite, calcium nitrate, unreacted calcium hydroxide and waterPressurizing the mixed solution by a pressure circulating pump 7, feeding a part of the mixed solution into a second-stage absorption reaction tower 2 through a liquid flow pipeline 18, continuing absorption reaction, and returningThe gas-liquid mixture after reaction is subjected to gas-liquid separation in a separator 13 at the bottom of the tower; the separated tail gas is sent to a tail gas treatment system through a main exhaust pipeline 20; a part of the separated mixed solution enters a precipitation tank 11 through a pipeline 19 for precipitation, and precipitated calcium nitrate at the bottom of the tank is discharged through a precipitation discharge pipe 23; the supernatant in the precipitation tank 11 is pressurized by a supernatant discharge pipe 22 through a pressure pump 9 and is sent into a neutralization tower 3 through a liquid conveying pipeline 21, the required nitrogen oxide gas is supplemented intothe neutralization tower through a pipeline 27, a switch valve 29 and a pipeline 31 in an oxidizer 10, the residual calcium hydroxide is neutralized, calcium nitrite neutralization liquid with the pH value of 7-8 is generated, and the calcium nitrite neutralization liquid is sent into a post-processing procedure through a pipeline 24; the tail gas in the neutralization tower is sent into a tail gas main discharge pipe 20 through a pipeline 25 and is discharged; a part of the mixed liquid separated by the separator 12 is pressurized by a pressure circulating pump 7 through a pipeline 17, is cooled to 30-50 ℃ through pipelines 18 and 32 and a water cooler 5, is sent into the first-stage absorption reaction tower through a return input pipeline 32, is sprayed by an injector 14 in the tower, and continuously reacts with the nitrogen oxide gas input into the tower through a pipeline 26; the mixed liquid separated by the separator 13 is pressurized by a pressure circulating pump 8, is cooled to 30-38 ℃ through a liquid flow return pipeline 34 and a water cooler 6, and is sent to a secondary absorption reaction tower through a return input pipeline 33, the returned mixed liquid is sprayed by an injector 15 in the tower for absorption reaction, and insufficient nitrogen oxide gas is supplied to the tower through an oxidizer 10 through a pipeline 27, a switch valve 28 and a pipeline 30.
Claims (2)
1. A process for producing calcium nitrite comprises a first-stage absorption reaction process of nitrogen oxide gas and lime milk in sequence; a first stage gas-liquid separation process; a second stage absorption reaction step of separating unreacted gas and partial reaction mixture; a second stage gas-liquid separation process after the reaction is finished; a step of precipitating and extracting calcium nitrate from the separated part of the mixed solution; carrying out neutralization reaction on residual hydro-calcium oxide in the precipitated calcium nitrite supernatant to complete the neutralization reaction process of calcium nitrite solution production; the method is characterized in that: in the first stage of absorption reaction processBefore, the high-pressure nitrogen oxide gas of 0.3-0.9 MPa is regulated to make NO/(NO) of the gas2+ NO) ratio of the nitrogen oxide gas reaches the optimal value of 0.3-0.6; and supplementing nitrogen oxide gas required for the second-stage absorption reaction and neutralization reaction process, and regulating NO/(NO) required by the reaction2A step of replenishing a nitrogen oxide gas having a + NO) ratio; after the first and second two-stage gas-liquid separation processes, a process of pressurizing, cooling and cooling part of the reaction mixed liquid, returning the reaction mixed liquid to the front stage, spraying the reaction mixed liquid by an injector, and carrying out absorption reaction with the front stage high-pressure nitrogen oxide gas with 0.3-0.9 MPa in the tower respectively is provided.
2. The apparatus for producing calcium nitrite according to claim 1, comprising four main apparatuses, namely a first-stage absorption reaction tower (1), a second-stage absorption reaction tower (2), a precipitation tank (11) and a neutralization tower (3), which are arranged in sequence; wherein the bottoms of the first-stage absorption reaction tower and the second-stage absorption reaction tower are respectively provided with a gas-liquid separator; the gas-liquid separator (12) at the bottom of the first-stage absorption reaction tower is connected with the top of the second-stage absorption reaction tower (2) through an upper output pipeline (16) of the gas-liquid separator, and is connected with the gas-liquid separator (13) at the bottom of the second-stage absorption reaction tower through a lower output pipeline (17)of the gas-liquid separator, a pressure circulating pump (7) and a liquid flow pipe (18); a gas-liquid separator (13) at the bottom of the second-stage absorption reaction tower is connected with a tail gas main discharge pipe (20) in an upper mode, and a pipeline (19) in a lower mode is connected with a settling tank (11); a calcium nitrate precipitation discharge pipe (23) is arranged at the bottom of the precipitation tank (11), a supernatant discharge pipe (22) is arranged at the top of the precipitation tank, and the supernatant discharge pipe is connected with the top of the neutralization tower (3) through a pressure pump (9) and a liquid conveying pipeline (21); one path of the neutralization tower (3) is connected with the tail gas main exhaust pipe (20) through the tail gas exhaust pipe (25) at the top of the neutralization tower, and the other path is the exhaust pipe (24) filled with calcium nitrite solution at the bottom of the neutralization tower, and the neutralization tower is characterized in that: (a) an oxidizer (10) is arranged in front of the first-stage absorption reaction tower (1), one path of the oxidizer is connected with the top of the first-stage absorption reaction tower through a gas pipe (26), the other path of the oxidizer is divided into two branch pipelines through a pipeline (27), one branch pipeline (30) is connected with the top of the second-stage absorption reaction tower through a switch valve (28), and the other branch pipeline (31) is connected with the bottom of the neutralization tower (3) through a switch valve (29); (b) a water cooler (4) which cools and cools the high-pressure and high-temperature nitrogen oxide gas with the pressure of 0.3-0.9 MPa to 150-250 ℃ is arranged in front of the oxidizer (10); (c) an input pipeline (32) for returning part of the mixed liquid is arranged at the top of the first-stage absorption reaction tower, the pipeline (32) is connected with a liquid flow pipe (18) connected with a gas-liquid separator at the bottom of the second-stage absorption reaction tower through a water cooler (5), an input pipeline (33) for returning part of the mixed liquid is arranged at the top of the second-stage absorption reaction tower, and the pipeline (33) is connected with a liquid flow return pipeline (34) which is discharged from a gas-liquid separator (13) at the bottom of the second-stage absorption reaction tower and passes through a pressure circulating pump (8) through a water cooler (6); (d) ejectors (14) (15) for ejecting the mixed liquid returned through the pipes (32) (33) to react with the high-pressure nitrogen oxide gas of 0.3-0.9 MPa are respectively arranged at the top parts in the first-stage absorption reaction tower and the second-stage absorption reaction tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02134123 CN1223511C (en) | 2002-11-21 | 2002-11-21 | Novel process for producing calcium nitrite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02134123 CN1223511C (en) | 2002-11-21 | 2002-11-21 | Novel process for producing calcium nitrite |
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| CN1465528A CN1465528A (en) | 2004-01-07 |
| CN1223511C true CN1223511C (en) | 2005-10-19 |
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| CN 02134123 Expired - Fee Related CN1223511C (en) | 2002-11-21 | 2002-11-21 | Novel process for producing calcium nitrite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102463030A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Method for removing nitric oxide in tail gas for preparing oxalate from CO |
| CN106629805B (en) * | 2016-10-17 | 2017-11-21 | 交城县三喜化工有限公司 | A kind of method and its device for producing calcium nitrate liquid |
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