CN110627077A - Method for preparing sodium silicate by using sodium nitrate - Google Patents
Method for preparing sodium silicate by using sodium nitrate Download PDFInfo
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- CN110627077A CN110627077A CN201911072056.7A CN201911072056A CN110627077A CN 110627077 A CN110627077 A CN 110627077A CN 201911072056 A CN201911072056 A CN 201911072056A CN 110627077 A CN110627077 A CN 110627077A
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- reaction
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- sodium silicate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/38—Nitric acid
- C01B21/40—Preparation by absorption of oxides of nitrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/06—Preparation with gaseous nitric acid or nitrogen oxides
Abstract
The present invention provides a method for preparing sodium silicate, comprising: mixing sodium nitrate and a silicon raw material, reacting under a heating condition, treating a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and treating to obtain nitric acid or a nitrate byproduct. The method can selectively prepare sodium silicate products with different moduli and by-product dilute nitric acid or nitrate by adjusting the proportion of sodium nitrate and quartz sand or other silicon-containing raw materials. The method can also be applied to the production of water glass or white carbon black. The method has the characteristics of low reaction temperature, short reaction time and low energy consumption, and has the advantages of simple process flow, high product purity, capability of completely recycling the generated gas and better industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of chemical production, relates to a method for preparing sodium silicate, and particularly relates to a method for preparing sodium silicate by using sodium nitrate.
Background
Sodium silicate, commonly known as natron, is a water-soluble silicate whose aqueous solution is commonly known as water glass. Sodium silicate is a widely used chemical raw material, is used for manufacturing various silicon compound products such as silica gel, white carbon black, zeolite molecular sieves, silica sol and the like, and is a basic raw material of silicon compounds.
The industrial production method of sodium silicate mainly comprises a dry method and a wet method. The dry production process is that quartz sand and sodium carbonate are mixed in certain proportion and heated in a reverberatory furnace to 1300-1400 deg.c to produce molten sodium silicate, which is water quenched or dry molded to obtain solid sodium silicate. The wet production process is to produce water glass by heating and reacting quartz powder and sodium hydroxide as raw materials in a high-pressure kettle. Both of the two processes have the defects of high energy consumption, large raw material loss and the like.
Because of the high price of sodium carbonate, a process for preparing sodium silicate by replacing sodium carbonate with sodium sulfate has been developed. Because the decomposition temperature of sodium sulfate is high, a certain proportion of reducing agents such as carbon or coal are required to be added to reduce the sodium sulfate into sodium sulfite which is easy to react with silicon dioxide. The sodium silicate is prepared by adopting sodium sulfate, and the problems are that the sodium sulfate (commonly called nitre water) in an unreacted molten state is generated in the production process, the permeability is extremely strong, and the corrosion to equipment is serious; secondly, a large amount of sulfur dioxide gas is generated after sodium sulfate is reduced and decomposed in the production process, and the gas is difficult to recycle and has a large environmental pollution problem.
CN 102092734 a discloses a method for preparing sodium silicate solution and mullite refractory material, in particular to a method for preparing sodium silicate solution and mullite refractory material by using fly ash. The method comprises the steps of taking fly ash subjected to magnetic separation and iron removal as a raw material, carrying out high-temperature and high-pressure NaOH alkali dissolution and desilication on the fly ash to obtain a sodium silicate solution and desilication fly ash, and washing and drying the sodium silicate solution and the desilication fly ash to obtain low-sodium desilication fly ash; and mixing the dried low-sodium-removed fly ash, a powdery aluminum source and kaolin powder with water, pressing and molding, and firing in a high-temperature tunnel kiln to obtain the refractory material. The technical scheme needs to prepare the sodium silicate at high temperature and high pressure, and has high process energy consumption and high cost.
CN 104556080A discloses a method for preparing sodium silicate by using desiliconized alkali liquor, which comprises the following steps; 1) introducing carbon dioxide gas into desiliconized alkali liquor at the temperature of 50-100 ℃ until silicon dioxide is not separated out, and then sequentially filtering, washing, separating and drying to obtain a silicon dioxide filter cake; 2) and mixing and stirring the silicon dioxide filter cake and desiliconized alkali liquor again at 70-100 ℃, and filtering and removing slag to obtain a sodium silicate product with the modulus of 1.5-3.8. The by-products generated by the technical scheme are not fully utilized, and the waste of resources is caused.
Therefore, there is a need to develop a method for preparing sodium silicate with low energy consumption, easy operation and less pollution.
Disclosure of Invention
In order to solve the technical problems in the prior art, the method for preparing the sodium silicate is simple in process, mild in condition, low in energy consumption and environment-friendly, and can be used for preparing sodium silicate products with different moduli.
In order to achieve the technical effect, the invention adopts the following technical scheme:
the invention provides a method for preparing sodium silicate, which is characterized by comprising the following steps:
mixing sodium nitrate and a silicon raw material, reacting under a heating condition, treating a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and treating to obtain nitric acid or a nitrate byproduct.
As a preferred embodiment of the present invention, the silicon raw material comprises any one or a combination of at least two of quartz sand, silicon slag, tailings sand, or waste silicon powder, and the combination is typically but not limited to: a combination of silica sand and silica slag, a combination of silica slag and tailings sand, a combination of tailings sand and waste silica powder, a combination of waste silica powder and silica sand, or a combination of silica slag, tailings sand and waste silica powder, and the like.
In the invention, the source of the sodium nitrate and silicon raw material is not limited, the sodium nitrate and silicon raw material can be obtained by any process, and all sodium silicate and silicon raw materials produced in the field are suitable for the invention.
In a preferred embodiment of the present invention, the molar ratio of the sodium nitrate to the silicon raw material is 3:1 to 1:6, such as 2.5:1, 2:1, 1.5:1, 1:2, 1:3, 1:4, or 1:5, but not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable, and preferably 2:1 to 1: 3.5.
Wherein the molar ratio of the sodium nitrate to the silicon raw material is the molar ratio of the sodium nitrate to the silicon dioxide in the silicon raw material.
In the invention, sodium nitrate with lower decomposition temperature is adopted to replace sodium carbonate and sodium sulfate with higher decomposition temperature, the reaction temperature is obviously reduced, and the generated nitrogen oxides are collected and treated to prepare dilute nitric acid or nitrate byproducts. Sodium nitrate and quartz sand or other silicon-containing raw materials are used as raw materials, and sodium silicate products with different modulus can be selectively prepared by adjusting the proportion of the sodium nitrate and the quartz sand or other silicon-containing raw materials.
In a preferred embodiment of the present invention, the reaction is carried out in an air atmosphere or an oxygen atmosphere.
In a preferred embodiment of the present invention, the temperature of the heating reaction is 600 to 1200 ℃, for example 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃ or 1100 ℃, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned value range are also applicable, and preferably 650 to 900 ℃.
In the present invention, the heating method includes, but is not limited to, one or a combination of at least two of electric heating, gas heating, and coal heating.
Preferably, the heating reaction time is 30-180 min, such as 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, 130min, 140min, 150min, 160min or 170min, but not limited to the enumerated values, and other non-enumerated values in the range of the enumerated values are also applicable, preferably 60-120 min.
As a preferred technical scheme of the invention, the method for treating the solid phase comprises any one or a combination of at least two of cooling, water quenching and leaching, and typical but non-limiting examples of the combination are as follows: a combination of cooling and water quenching, a combination of water quenching and rinsing, a combination of rinsing and cold zone or a combination of cooling, water quenching and rinsing, etc.
As a preferred embodiment of the present invention, the method for treating the gas comprises any one or a combination of at least two of water absorption, alkaline solution absorption, oxidized water absorption, oxidized alkaline solution absorption, or peroxide solution absorption, and the combination is typically but not limited to: a combination of water absorption and alkaline solution absorption, a combination of water absorption after oxidation and alkaline solution absorption after oxidation, a combination of peroxide solution and water absorption, a combination of alkaline solution absorption and peroxide solution absorption, or a combination of water absorption, alkaline solution absorption and peroxide solution absorption, and the like.
Preferably, the alkaline solution comprises any one of, or a combination of at least two of, aqueous sodium hydroxide solution, aqueous potassium hydroxide solution, aqueous sodium carbonate solution, or aqueous potassium carbonate solution, as typical but non-limiting examples: a combination of an aqueous sodium hydroxide solution and an aqueous potassium hydroxide solution, a combination of an aqueous potassium hydroxide solution and an aqueous sodium carbonate solution, a combination of an aqueous sodium carbonate solution and an aqueous potassium carbonate solution, a combination of an aqueous potassium carbonate solution and an aqueous sodium hydroxide solution, a combination of an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution and an aqueous sodium carbonate solution, and the like.
Preferably, the oxidation comprises any one of oxygen oxidation, ozone oxidation or catalytic oxidation or a combination of at least two of the following typical but non-limiting examples: a combination of oxygen oxidation and ozone oxidation, a combination of ozone oxidation and catalytic oxidation, a combination of catalytic oxidation and oxygen oxidation, or a combination of oxygen oxidation, ozone oxidation and catalytic oxidation, and the like.
Preferably, the peroxide solution is a hydrogen peroxide solution.
Preferably, the hydrogen peroxide solution has a concentration of 1 to 30 wt%, such as 2 wt%, 5 wt%, 8 wt%, 10 wt%, 12 wt%, 15 wt%, 18 wt%, 20 wt%, 22 wt%, 25 wt% or 28 wt%, but not limited to the recited values, and other values within the range are equally applicable, preferably 5 to 15 wt%.
In a preferred embodiment of the present invention, the sodium silicate product has a modulus of 1.0 to 3.5, such as 1.2, 1.5, 1.8, 2.0, 2.2, 2.5, 2.8, 3.0, 3.2, or 3.4, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
As a preferred embodiment of the present invention, the method for preparing sodium silicate comprises:
mixing sodium nitrate and a silicon raw material according to a molar ratio of 3: 1-1: 6, reacting for 30-180 min in an oxygen or air atmosphere at 600-1200 ℃, cooling, water quenching and leaching a solid phase after the reaction is finished to obtain a sodium silicate product with a modulus of 1.0-3.5, collecting gas generated by the reaction, and performing water absorption, alkaline solution absorption, water absorption after oxidation, alkaline solution absorption after oxidation or peroxide solution absorption to obtain nitric acid or a nitrate byproduct.
As a preferable technical scheme of the invention, the method is used for producing the water glass or the white carbon black.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the invention provides a method for preparing sodium silicate, which adopts sodium nitrate and quartz sand or other silicon-containing raw materials as raw materials, greatly reduces the reaction temperature, does not need to additionally add a reducing agent and the like, saves the energy consumption and the cost, and has good economic benefit;
(2) the invention provides a method for preparing sodium silicate, the by-product nitrogen oxide gas produced by the method has high purity, the by-product of dilute nitric acid or nitrate can be prepared after collection and treatment, the whole process flow is short, and the operation is simple and convenient;
(3) the invention provides a method for preparing sodium silicate, which can selectively prepare sodium silicate products with different modulus by adjusting the ratio of sodium nitrate to quartz sand or other silicon-containing raw materials, can also be applied to the production of water glass or white carbon black, and has good application prospect.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and quartz sand according to a molar ratio of 2:1, reacting in a reaction furnace at 850 ℃ for 60min in an air atmosphere, cooling a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and absorbing by using a peroxide solution with 12 wt% to obtain a dilute nitric acid byproduct.
Example 2
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and quartz sand according to a molar ratio of 1:1, reacting in an oxygen atmosphere at 650 ℃ for 120min in a reaction furnace, performing water quenching treatment on a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and absorbing the gas with water to obtain a dilute nitric acid byproduct.
Example 3
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and quartz sand according to a molar ratio of 1:2, reacting in a reaction furnace at 800 ℃ in an air atmosphere for 60min, cooling a solid phase after the reaction is finished to obtain a sodium disilicate product, collecting gas generated by the reaction, and absorbing by using a sodium hydroxide solution to obtain a sodium nitrate byproduct.
Example 4
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and quartz sand according to a molar ratio of 1:3, reacting in an oxygen atmosphere at 750 ℃ for 120min in a reaction furnace, performing water quenching treatment on a solid phase after the reaction is finished to obtain a sodium trisilicate product, collecting gas generated by the reaction, and absorbing by using a potassium hydroxide solution to obtain a potassium nitrate byproduct.
Example 5
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and quartz sand according to a molar ratio of 1:3.5, reacting in a reaction furnace in an oxygen atmosphere at 1200 ℃ for 30min, cooling a solid phase after the reaction is finished to obtain a sodium silicate product with a modulus of 3.5, collecting gas generated by the reaction, and absorbing by using a 20 wt% peroxide solution to obtain a dilute nitric acid byproduct.
Example 6
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and quartz sand according to a molar ratio of 2:1, reacting in a reaction furnace at 800 ℃ in an air atmosphere for 60min, cooling a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and absorbing by using a sodium hydroxide solution after catalytic oxidation to obtain a sodium nitrate byproduct.
Example 7
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and silicon ore powder according to a molar ratio of 2:1, reacting in a reaction furnace at 750 ℃ for 90min in an air atmosphere, leaching a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and absorbing by water after ozone oxidation to obtain a dilute nitric acid byproduct.
Example 8
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and waste silicon powder according to a molar ratio of 2:1, reacting in a reaction furnace at 800 ℃ in an air atmosphere for 120min, performing water quenching treatment on a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and absorbing oxygen by using a potassium hydroxide aqueous solution to obtain a potassium nitrate byproduct after the oxygen is oxidized.
Example 9
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and tailing slag according to a molar ratio of 2:1, reacting in a reaction furnace at 850 ℃ for 60min in an air atmosphere, cooling a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and absorbing by using a sodium carbonate aqueous solution after catalytic oxidation to obtain a sodium nitrate byproduct.
Example 10
This example provides a method of preparing sodium silicate, comprising:
mixing sodium nitrate and quartz sand according to a molar ratio of 2:1, reacting in a reaction furnace at 800 ℃ in an air atmosphere for 60min, cooling a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and absorbing with water after ozone oxidation to obtain a dilute nitric acid byproduct.
The sodium silicate products prepared in examples 1-10 were tested for their concentrations as well as their by-products, and the results are shown in table 1.
TABLE 1
| Purity of sodium silicate/%) | By-product concentration/%) | |
| Example 1 | 99.34％ | 33.13 |
| Example 2 | 99.70％ | 31.56 |
| Example 3 | 99.65％ | 52.01 |
| Example 4 | 98.91％ | 51.78 |
| Example 5 | 99.46％ | 30.29 |
| Example 6 | 99.05％ | 53.04 |
| Example 7 | 99.41％ | 33.28 |
| Example 8 | 99.45％ | 52.47 |
| Example 9 | 99.22％ | 53.88 |
| Example 10 | 98.92％ | 33.12 |
According to the test results in table 1, the reaction temperature of the method for preparing sodium silicate provided by the invention is low, the purity of the prepared sodium silicate can reach more than 99.50%, and the concentrations of byproducts such as nitric acid, sodium nitrate, potassium nitrate and the like are high, so that resources are fully utilized.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A process for the preparation of sodium silicate, characterized in that it comprises:
mixing sodium nitrate and a silicon raw material, reacting under a heating condition, treating a solid phase after the reaction is finished to obtain a sodium silicate product, collecting gas generated by the reaction, and treating to obtain nitric acid or a nitrate byproduct.
2. The method according to claim 1, wherein the silicon raw material comprises any one of quartz sand, silicon slag, tailing sand, or waste silicon powder, or a combination of at least two of them.
3. The method according to claim 1 or 2, wherein the molar ratio of the sodium nitrate to the silicon raw material is 3:1 to 1:6, preferably 2:1 to 1: 3.5.
4. The process according to any one of claims 1 to 3, wherein the reaction is carried out in an air atmosphere or an oxygen atmosphere.
5. The method according to any one of claims 1 to 4, wherein the temperature of the heating reaction is 600 to 1200 ℃, preferably 650 to 900 ℃;
preferably, the heating reaction time is 30-180 min, preferably 60-120 min.
6. A method according to any one of claims 1 to 5, wherein the treatment of the solid phase comprises any one or a combination of at least two of cooling, water quenching or rinsing.
7. The method according to any one of claims 1 to 6, wherein the gas is treated by any one or a combination of at least two of water absorption, alkaline solution absorption, post-oxidation water absorption, post-oxidation alkaline solution absorption, or peroxide solution absorption;
preferably, the alkaline solution comprises any one of or a combination of at least two of a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution, a sodium carbonate aqueous solution or a potassium carbonate aqueous solution;
preferably, the oxidation comprises any one or a combination of at least two of oxygen oxidation, ozone oxidation or catalytic oxidation;
preferably, the peroxide solution is a hydrogen peroxide solution;
preferably, the concentration of the hydrogen peroxide solution is 1 to 30 wt%, preferably 5 to 15 wt%.
8. The method according to any one of claims 1 to 7, wherein the sodium silicate product has a modulus of 1.0 to 3.5.
9. The method according to any one of claims 1-8, characterized in that the method comprises:
mixing sodium nitrate and a silicon raw material according to a molar ratio of 3: 1-1: 6, reacting for 30-180 min in an oxygen or air atmosphere at 600-1200 ℃, cooling, water quenching and leaching a solid phase after the reaction is finished to obtain a sodium silicate product with a modulus of 1.0-3.5, collecting gas generated by the reaction, and performing water absorption, alkaline solution absorption, water absorption after oxidation, alkaline solution absorption after oxidation or peroxide solution absorption to obtain nitric acid or a nitrate byproduct.
10. The method according to any one of claims 1 to 9, wherein the method is used for producing water glass or silica.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113120911A (en) * | 2021-04-20 | 2021-07-16 | 昆明理工大学 | Method for separating silicon and iron in copper smelting slag through ultrasonic enhancement and preparing white carbon black by using silicon |
| CN113277524A (en) * | 2021-06-16 | 2021-08-20 | 洛阳市奇航化工有限公司 | Preparation method of industrial sodium silicate adhesive |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113120911A (en) * | 2021-04-20 | 2021-07-16 | 昆明理工大学 | Method for separating silicon and iron in copper smelting slag through ultrasonic enhancement and preparing white carbon black by using silicon |
| CN113120911B (en) * | 2021-04-20 | 2023-09-12 | 昆明理工大学 | Method for ultrasonically reinforcing and separating silicon and iron in copper smelting slag and preparing white carbon black by utilizing silicon |
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