CN112939001A - Preparation method of sodium silicate anhydrous by sodium nitrate - Google Patents
Preparation method of sodium silicate anhydrous by sodium nitrate Download PDFInfo
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- CN112939001A CN112939001A CN202110410827.XA CN202110410827A CN112939001A CN 112939001 A CN112939001 A CN 112939001A CN 202110410827 A CN202110410827 A CN 202110410827A CN 112939001 A CN112939001 A CN 112939001A
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- C01B33/32—Alkali metal silicates
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Abstract
The invention discloses a preparation method of sodium silicate without nitrate, which takes micro silicon powder, sodium sulfate and semi-coke as raw materials, and the micro silicon powder, the sodium sulfate and the semi-coke are subjected to melting reaction to prepare powdery sodium silicate; not only the reasonable utilization of the micro silicon powder is realized, but also the resource waste and the environmental pollution caused by the waste of the micro silicon powder are avoided; the modulus of the prepared sodium silicate is 1.5-3, and the conversion rate of the raw materials reaches more than 90%. The method overcomes the generation of the saltpeter water by optimizing the parameters of the raw material proportion, the heating rate, the reaction temperature, the reaction time, the granularity of the blue carbon powder and the like in the reaction process, and has good application prospect compared with the traditional process.
Description
Technical Field
The invention relates to a preparation method of sodium silicate free of sodium nitrate water, belonging to the technical field of sodium silicate preparation.
Background
Sodium silicate, commonly known as sodium silicate, and its aqueous solution, commonly known as sodium silicate, has the chemical formula of Na2O·nSiO2It is a soluble silicate. In the chemical industry, sodium silicate is used for manufacturing silica gel, zeolite molecular sieves, white carbon black, silica sol and the like; in the petroleum industry, the catalyst is used for manufacturing a silicon-aluminum catalyst for petroleum catalysis and cracking; in the light chemical industry, the materials which are indispensable in soap and washing powder are softener and settling agent of tap water; in agriculture, for the manufacture of siliceous fertilizers; in the building industry, it is used for manufacturing cement, soil curing agents, refractory materials, corrugated boards, etc.
At present, the raw materials for preparing sodium silicate mainly comprise quartz sand, sodium carbonate, sodium sulfate, carbon powder and the like. The invention utilizes solid waste silica fume to replace quartz sand, uses semi-coke to replace carbon powder as raw material to carry out reaction, and prepares solid sodium silicate with different modulus by a melting method. The mechanism of the preparation process shows that the semi-coke powder reduces part of sodium sulfate at 600-1000 ℃ to generate sodium sulfide, and the sodium sulfide further reacts with the sodium sulfate to prepare the sodium silicate. The production of the nitrate water is overcome by optimizing the process parameters such as the raw material proportion, the heating rate, the reaction temperature, the reaction time, the granularity of the blue carbon powder and the like. The method not only realizes the recycling of solid wastes such as the micro silicon powder, the blue carbon powder and the like, but also solves the production safety problem caused by the nitrate water.
Disclosure of Invention
The invention aims to overcome the defect of producing the sodium nitrate water in the preparation process and provide a preparation method of sodium silicate without the sodium nitrate water, which takes micro silicon powder, sodium sulfate and semi-coke as raw materials and prepares powdery sodium silicate by carrying out a melting reaction on the micro silicon powder, the sodium sulfate and the semi-coke; not only the reasonable utilization of the micro silicon powder is realized, but also the resource waste and the environmental pollution caused by the waste of the micro silicon powder are avoided; the modulus of the prepared sodium silicate is 1.5-3, and the conversion rate of the raw materials reaches more than 90%. The method overcomes the generation of the saltpeter water by optimizing the parameters of the raw material proportion, the heating rate, the reaction temperature, the reaction time, the granularity of the blue carbon powder and the like in the reaction process, and has good application prospect compared with the traditional process.
The preparation method of the sodium silicate without sodium nitrate hydrate, disclosed by the invention, is carried out according to the following steps:
a. pulverizing Ramsbottom coke, sieving with 50-300 mesh sieve, and collecting powder to obtain Ramsbottom coke powder with particle size of 50-300 mesh;
b. uniformly mixing the micro silicon powder, the sodium sulfate and the semi-coke powder obtained in the step a according to a molar ratio of 1.5-3:1:2-3.5, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with a heating rate of 8-12 ℃/min, a reaction temperature of 950-1100 ℃ and a reaction time of 30-70min to perform a melting reaction;
c. after the reaction is finished, after the reactant is cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free silicate product with the modulus of 1.5-3.
The invention relates to a preparation method of sodium silicate without sodium nitrate hydrate, which comprises the following chemical reaction formula: 2Na2SO4+nSiO2+C→2Na2O·nSiO2+2SO2(g)+CO2(g)。
The invention has the beneficial effects that: the sodium silicate is prepared by taking the solid wastes such as the micro silicon powder, the sodium sulfate, the blue carbon powder and the like as raw materials through a melting reaction, so that the reasonable utilization of the micro silicon powder is realized, and the resource waste and the environmental pollution caused by the waste of the micro silicon powder are avoided; the modulus of the prepared sodium silicate is 1.5-3, and the conversion rate of the raw materials reaches more than 90%. The method overcomes the generation of the saltpeter water by analyzing the mechanism of the reaction process and optimizing the process parameters such as the proportion of raw materials, the heating rate, the reaction temperature, the reaction time, the granularity of the blue carbon powder and the like, and has good application prospect compared with the traditional process.
Detailed Description
Example 1
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 200 meshes and 250 meshes, and collecting powder to obtain semi-coke powder with the particle size of 200 meshes and 250 meshes;
b. uniformly mixing 3.17g of silica fume, 5g of sodium sulfate and 1.06g of semi-coke powder obtained in the step a, conveying the mixture into a high-temperature furnace, heating to 1000 ℃ at a heating rate of 10 ℃/min in an air atmosphere, and reacting for 60min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 1.66 and the conversion rate of the raw material of 90.67%.
Example 2
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 200 meshes and 250 meshes, and collecting powder to obtain semi-coke powder with the particle size of 200 meshes and 250 meshes;
b. uniformly mixing 4.23g of silica fume, 5g of sodium sulfate and 1.06g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 8 ℃/min, the reaction temperature of 950 ℃ and the reaction time of 30min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.25 and the conversion rate of raw materials of 90.18%.
Example 3
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 200 meshes and 250 meshes, and collecting powder to obtain semi-coke powder with the particle size of 200 meshes and 250 meshes;
b. uniformly mixing 5.28g of silica fume, 5g of sodium sulfate and 1.06g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 10 ℃/min, the reaction temperature of 1000 ℃ and the reaction time of 50min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.43 and the conversion rate of raw materials of 94.57%.
Example 4
Preparation of sodium silicate:
a. pulverizing Ramsbottom coke, sieving with 50-100 mesh sieve, and collecting powder to obtain Ramsbottom coke powder with particle size of 50-100 mesh;
b. uniformly mixing 6.34g of silica fume, 5g of sodium sulfate and 1.06g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 9 ℃/min, the reaction temperature of 1100 ℃ and the reaction time of 60min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.96 and the conversion rate of the raw material of 90.95%.
Example 5
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 150-200 meshes, and collecting powder to obtain semi-coke powder with the particle size of 150-200 meshes;
b. uniformly mixing 5.28g of silica fume, 5g of sodium sulfate and 0.85g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 10 ℃/min, the reaction temperature of 1050 ℃ and the reaction time of 70min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.58 and the conversion rate of the raw material of 92.64 percent.
Example 6
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 250-300 meshes, and collecting powder to obtain semi-coke powder with the particle size of 250-300 meshes;
b. uniformly mixing 5.28g of silica fume, 5g of sodium sulfate and 1.27g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 11 ℃/min, the reaction temperature of 1100 ℃ and the reaction time of 70min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.45 and the conversion rate of the raw material of 94.83 percent.
Example 7
Preparation of sodium silicate:
a. crushing semi-coke, sieving with a 300-mesh sieve, and collecting powder to obtain semi-coke powder with the particle size of 300 meshes;
b. uniformly mixing 5.28g of silica fume, 5g of sodium sulfate and 1.48g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 12 ℃/min, the reaction temperature of 1100 ℃ and the reaction time of 65min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.41 and the conversion rate of the raw material of 94.41 percent.
Example 8
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 100-150 meshes, and collecting powder to obtain semi-coke powder with the particle size of 100-150 meshes;
b. uniformly mixing 3.17g of silica fume, 5g of sodium sulfate and 1.06g of semi-coke powder obtained in the step a, conveying the mixture into a high-temperature furnace, heating to 1000 ℃ at a heating rate of 8 ℃/min in an air atmosphere, and reacting for 60min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 1.71 and the conversion rate of raw materials of 90.43%.
Example 9
Preparation of sodium silicate:
a. pulverizing Ramsbottom coke, sieving with 50-100 mesh sieve, and collecting powder to obtain Ramsbottom coke powder with particle size of 50-100 mesh;
b. uniformly mixing 4.23g of silica fume, 5g of sodium sulfate and 1.06g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 10 ℃/min, the reaction temperature of 950 ℃ and the reaction time of 40min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.13 and the conversion rate of raw materials of 90.44%.
Example 10
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 150-200 meshes, and collecting powder to obtain semi-coke powder with the particle size of 150-200 meshes;
b. uniformly mixing 5.28g of silica fume, 5g of sodium sulfate and 1.06g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 11 ℃/min, the reaction temperature of 1050 ℃ and the reaction time of 60min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.39 and the conversion rate of the raw material of 94.05 percent.
Example 11
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 150-200 meshes, and collecting powder to obtain semi-coke powder with the particle size of 150-200 meshes;
b. uniformly mixing 6.34g of silica fume, 5g of sodium sulfate and 1.06g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 12 ℃/min, the reaction temperature of 1000 ℃ and the reaction time of 50min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.89 and the conversion rate of raw materials of 94.30%.
Example 12
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 150-200 meshes, and collecting powder to obtain semi-coke powder with the particle size of 150-200 meshes;
b. uniformly mixing 5.28g of silica fume, 5g of sodium sulfate and 0.85g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 10 ℃/min, the reaction temperature of 950 ℃ and the reaction time of 70min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate anhydrous sodium silicate product with the modulus of 2.65 and the conversion rate of the raw material of 91.53 percent.
Example 13
Preparation of sodium silicate:
a. crushing the semi-coke, sieving the crushed semi-coke with a sieve of 250-300 meshes, and collecting powder to obtain semi-coke powder with the particle size of 250-300 meshes;
b. uniformly mixing 5.28g of silica fume, 5g of sodium sulfate and 1.27g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 10 ℃/min, the reaction temperature of 1000 ℃ and the reaction time of 50min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.47 and the conversion rate of the raw material of 95.34%.
Example 14
Preparation of sodium silicate:
a. crushing semi-coke, sieving with a 300-mesh sieve, and collecting powder to obtain semi-coke powder with the particle size of 300 meshes;
b. uniformly mixing 5.28g of silica fume, 5g of sodium sulfate and 1.48g of semi-coke powder obtained in the step a, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with the heating rate of 9 ℃/min, the reaction temperature of 1100 ℃ and the reaction time of 55min to perform a melting reaction;
c. after the reaction is finished, after the reactants are cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free water silicate product with the modulus of 2.34 and the conversion rate of the raw material of 93.24%.
Claims (1)
1. The preparation method of sodium silicate without sodium nitrate hydrate is characterized by comprising the following steps:
a. pulverizing Ramsbottom coke, sieving with 50-300 mesh sieve, and collecting powder to obtain Ramsbottom coke powder with particle size of 50-300 mesh;
b. uniformly mixing the micro silicon powder, the sodium sulfate and the semi-coke powder obtained in the step a according to a molar ratio of 1.5-3:1:2-3.5, then sending the mixture into a high-temperature furnace, and calcining the mixture in an air atmosphere with a heating rate of 8-12 ℃/min, a reaction temperature of 950-1100 ℃ and a reaction time of 30-70min to perform a melting reaction;
c. after the reaction is finished, after the reactant is cooled to room temperature, taking out the product, and grinding to obtain a powdery sodium nitrate-free silicate product with the modulus of 1.5-3.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003070636A1 (en) * | 2001-12-21 | 2003-08-28 | Tianrun Ye | Method of producing a silica aerogel and a sodium carbonate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003070636A1 (en) * | 2001-12-21 | 2003-08-28 | Tianrun Ye | Method of producing a silica aerogel and a sodium carbonate |
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| 谢刚等, 冶金工业出版社 * |
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