CN114408885B - Reducing agent for producing yellow phosphorus by thermal method and preparation method thereof - Google Patents
Reducing agent for producing yellow phosphorus by thermal method and preparation method thereof Download PDFInfo
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- CN114408885B CN114408885B CN202111635840.1A CN202111635840A CN114408885B CN 114408885 B CN114408885 B CN 114408885B CN 202111635840 A CN202111635840 A CN 202111635840A CN 114408885 B CN114408885 B CN 114408885B
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
- C01B25/027—Preparation of phosphorus of yellow phosphorus
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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Abstract
The invention discloses a reducing agent for producing yellow phosphorus by a thermal method, which comprises the following components in percentage by mass: 40-80% of solid waste, 10-50% of fixed carbon regulator, 1-5% of activator and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%. The invention discloses a preparation method of the reducing agent for producing yellow phosphorus by a thermal method. The reducing agent for producing yellow phosphorus by a thermal method and the preparation method thereof solve the problems of high raw material cost, high tar content and influence on the normal operation of a furnace gas-solid-gas separation device of the existing reducing agent.
Description
Technical Field
The invention belongs to the technical field of phosphorus chemical technology, and particularly relates to a reducing agent for producing yellow phosphorus by a thermal method. The invention also relates to a preparation method of the reducing agent for producing yellow phosphorus by a thermal method.
Background
At present, the reducing agent used in yellow phosphorus industry is coke, and in order to reduce the cost of raw materials for production, part of enterprises adopt anthracite to replace the coke. The main indexes are as follows:
the problems existing in the reducing agent used in yellow phosphorus industry at present are as follows:
1. coke is favorable for production, but the resources are pretty, the price is high, and the cost per ton of yellow phosphorus is increased by 1500 yuan.
2. Anthracite has lower price than coke, but has high volatile content, and volatile matters generate a large amount of tar in a yellow phosphorus electric furnace and enter the subsequent process along with the yellow phosphorus furnace gas, so that the normal operation of a gas-solid separation device of the yellow phosphorus furnace gas is seriously influenced, dust in the furnace gas can not be separated, a large amount of phosphorus mud (0.3 ton of phosphorus mud/yellow phosphorus) is generated, and the yield of phosphorus is reduced while the environment-friendly pressure is brought;
3. tar and yellow phosphorus are mixed together and cannot be separated, so that the purity of the yellow phosphorus is reduced.
Disclosure of Invention
The invention aims to provide a reducing agent for producing yellow phosphorus by a thermal method, which solves the problems of high raw material cost, high tar content and influence on the normal operation of a furnace gas-solid-gas separation device of the existing reducing agent.
The invention further aims at providing a preparation method of the reducing agent for producing yellow phosphorus by a thermal method.
The first technical scheme adopted by the invention is as follows: the reducing agent for producing yellow phosphorus by a thermal method comprises the following components in percentage by mass: 40-80% of solid waste, 10-50% of fixed carbon regulator, 1-5% of activator and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%.
The first technical solution of the invention is also characterized in that,
the solid waste is carbon residue ash with a fixed carbon mass ratio of 30-80% and a volatile matter mass ratio of 0.1-1.5%.
The fixed carbon regulator is coke breeze with the fixed carbon mass ratio of 40-88% and the volatile matter mass ratio of not more than 4%.
The activator is calcium sulfate.
The molding agent is sodium silicate.
The second technical scheme adopted by the invention is as follows: the preparation method of the reducing agent for producing yellow phosphorus by a thermal method comprises the following steps:
step 1, weighing the following components in percentage by mass: 40-80% of solid waste, 10-50% of fixed carbon regulator, 1-5% of activator and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%;
step 2, adding water into the solid waste weighed in the step 1 and stirring to obtain wet solid waste with the water content of 5-10% by mass;
step 3, mixing 50-80% of the wet solid waste prepared in the step 2 with the fixed carbon regulator, the activating agent and the molding agent weighed in the step 1 uniformly, heating, humidifying and activating to obtain a mixed material with the temperature of 25-65 ℃, the humidity of 15-26 and the activity of S50-S95;
step 4, extruding and forming the mixed material prepared in the step 3 to obtain material particles;
step 5, adding the rest of the wet solid waste prepared in the step 2 to the material particles prepared in the step 4 for strength enhancement;
step 6, drying the reinforced material particles in the step 5;
and 7, screening the material particles dried in the step 6 to obtain the product.
The second technical proposal of the invention is also characterized in that,
the granularity and the strength of the material particles obtained by screening in the step 7 are respectively 3-15 mm and 30-45N.
The solid waste is carbon residue ash with a fixed carbon mass ratio of 30-80% and a volatile matter mass ratio of 0.1-1.5%.
The fixed carbon regulator is coke breeze with the fixed carbon mass ratio of 40-88% and the volatile matter mass ratio of not more than 4%.
The activator is calcium sulfate and the molding agent is sodium silicate.
The beneficial effects of the invention are as follows:
1. waste utilization and energy utilization rate improvement by 2 percent.
2. Compared with coke, the reducing agent is expected to reduce the production cost of yellow phosphorus by 10-13%.
3. Greatly reduces the tar and dust content in the yellow phosphorus furnace gas, and is expected to improve the purity of the yellow phosphorus by 0.3 to 0.7 percent.
4. Thoroughly eliminates tar blocking micropores of gas-solid separation equipment, provides guarantee for long-term stable operation of a follow-up furnace gas-solid separation device, creates conditions for realizing anhydrous phosphorus recovery, thereby solving the problem that the yellow phosphorus industry pollutes the environment with sludge phosphorus and phosphorus recovery wastewater for many years, and preliminarily estimating that ton yellow phosphorus reduces the discharge of the sludge phosphorus by 0.3 ton and ton yellow phosphorus reduces the phosphorus recovery water by 5 ton.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of the reducing agent for producing yellow phosphorus by a thermal method.
Detailed Description
The invention will be described in detail with reference to the accompanying drawings and detailed description.
The invention provides a reducing agent for producing yellow phosphorus by a thermal method, which comprises the following components in percentage by mass: 40-80% of solid waste, 10-50% of fixed carbon regulator, 1-5% of activator and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%.
Wherein, the solid waste is carbon residue ash with the mass ratio of fixed carbon of 30-80% and the mass ratio of volatile matters of 0.1-1.5% preferably; the fixed carbon regulator is preferably coke breeze with the fixed carbon mass ratio of 40-88% and the volatile matter mass ratio of not more than 4%; the activator is preferably calcium sulfate; the molding agent is preferably sodium silicate.
The invention also provides a preparation method of the reducing agent for producing yellow phosphorus by a thermal method, which is shown in figure 1 and comprises the following steps:
step 1, weighing the following components in percentage by mass: 40-80% of carbon residue ash, 10-50% of coke breeze, 1-5% of activating agent and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%;
step 2, adding water into the carbon residue ash weighed in the step 1 and stirring to obtain wet carbon residue ash with the water content of 5-10% by mass;
step 3, mixing 50-80% of the wet carbon residue ash prepared in the step 2 with the powdered coke, the activating agent and the molding agent weighed in the step 1 uniformly, heating, humidifying and activating to obtain a mixed material with the temperature of 25-65 ℃, the humidity of 15-26 and the activity of S50-S95;
step 4, extruding and forming the mixed material prepared in the step 3 to obtain material particles;
step 5, adding the rest of the wet solid waste prepared in the step 2 to the material particles prepared in the step 4 to enhance the strength, namely, reacting the excited active substances, the modeling agent and the like in the particles to achieve the purpose of enhancing the strength of the particles;
step 6, drying the reinforced material particles in the step 5;
and 7, screening the dried material particles in the step 6 to obtain finished product particles with the granularity and the strength of 3-15 mm and 30-45N, and conveying the finished product particles to a yellow phosphorus electric furnace to prepare yellow phosphorus, wherein the screened fine powder can be conveyed to the step 2 for recycling.
Example 1
Weighing the following components in percentage by mass: 40% of carbon residue ash, 50% of coke breeze, 5% of calcium sulfate and 5% of sodium silicate; adding water into the weighed carbon residue ash and stirring to obtain wet carbon residue ash with the water content of 5 percent; mixing 50% of wet carbon residue ash by mass with powdered coke, an activating agent and a molding agent uniformly, heating, humidifying and activating to obtain a mixed material with the temperature of 25 ℃, the humidity of 15% and the activity of S80; extruding and forming the mixed material to obtain material particles; adding the rest 50% wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the granularity and strength of 86% (the particle size is 3-15 mm and the particle ratio is 38N).
Example 2
Weighing the following components in percentage by mass: 80% of carbon residue ash, 10% of coke breeze, 5% of calcium sulfate and 5% of sodium silicate; adding water into the weighed carbon residue ash and stirring to obtain wet carbon residue ash with the water content of 10 percent; mixing 80% of wet carbon residue ash by mass with powdered coke, an activating agent and a molding agent uniformly, heating, humidifying and activating to obtain a mixed material with the temperature of 65 ℃, the humidity of 20% and the activity of S95; extruding and forming the mixed material to obtain material particles; adding the rest 20% wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the particle size and strength of 93% (the particle size is 3-15 mm and the particle ratio is 45N).
Example 3
Weighing the following components in percentage by mass: 80% of carbon residue ash, 18% of coke breeze, 1% of calcium sulfate and 1% of sodium silicate; adding water into the weighed carbon residue ash and stirring to obtain wet carbon residue ash with the water content of 8 percent; mixing wet carbon residue ash 60% by weight with coke breeze, activator and molding agent uniformly, heating, humidifying and activating to obtain mixed material with temperature of 50deg.C, humidity of 26% and activity of S50; extruding and forming the mixed material to obtain material particles; adding the rest 40% wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the granularity and strength of 80% (the particle size is 3-15 mm and the particle ratio is 30N).
Example 4
Weighing the following components in percentage by mass: 60% of carbon residue ash, 35% of coke breeze, 2% of calcium sulfate and 3% of sodium silicate; adding water into the weighed carbon residue ash and stirring to obtain wet carbon residue ash with the water content of 6 percent; mixing wet carbon residue ash 70% by weight with coke breeze, activator and molding agent uniformly, heating, humidifying and activating to obtain mixed material with temperature of 40deg.C, humidity of 22% and activity of S78; extruding and forming the mixed material to obtain material particles; adding the rest 30% wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the granularity and strength of 85% (the particle size is 3-15 mm and the particle ratio is 37N).
Example 5
Weighing the following components in percentage by mass: 55% of carbon residue ash, 40% of coke breeze, 3% of calcium sulfate and 2% of sodium silicate; adding water into the weighed carbon residue ash and stirring to obtain wet carbon residue ash with the water content of 7 percent; mixing 80% of wet carbon residue ash by mass with powdered coke, an activating agent and a molding agent uniformly, heating, humidifying and activating to obtain a mixed material with the temperature of 35 ℃, the humidity of 20% and the activity of S75; extruding and forming the mixed material to obtain material particles; adding the rest 20% wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the particle size and strength of 83% (the particle size is 3-15 mm and the particle ratio is 35N).
Through the mode, the invention has the beneficial effects that:
1. waste utilization and energy utilization rate improvement by 2 percent. According to industry data, in the running process of the coal-based conversion and utilization device, the yield of the carbon residue ash accounts for 3% of the coal feeding amount, the calorific value of the coal is 6083kcal/kg, the calorific value of the carbon residue ash is 4590kcal/kg, and the energy utilization rate of the carbon residue ash is 90%, so that the energy utilization rate improved by the invention can be calculated according to the following formula: (4590 x 3% x 90%)/6083=2.04%.
2. Compared with coke, the reducing agent is expected to reduce the production cost of yellow phosphorus by 10-13%. The yellow phosphorus cost (raw material+electricity) can be reduced (13000-11600)/13000=10.8% if the yellow phosphorus cost per ton (coke) is estimated to be 11600 yuan by the reducing agent of the invention according to the average price of the yellow phosphorus plant (raw material+electricity) in Guizhou province in 2020.
3. Greatly reduces the tar and dust content in the yellow phosphorus furnace gas, and is expected to improve the purity of the yellow phosphorus by 0.3 to 0.7 percent. About 10.5 kg of tar byproduct per ton of yellow phosphorus calculated by using white coal (anthracite), 30-60% of tar is mixed with the yellow phosphorus finished product, and the purity of the yellow phosphorus is affected by 10.5 x 0.6/1000=0.63%.
4. Thoroughly eliminates tar blocking micropores of gas-solid separation equipment, provides guarantee for long-term stable operation of a subsequent furnace gas-solid separation device, creates conditions for realizing anhydrous phosphorus recovery, thereby solving the problem that the yellow phosphorus industry pollutes the environment with phosphorus recovery wastewater for years, and primarily estimates that ton yellow phosphorus reduces the discharge of 0.3 ton (yellow phosphorus industry data, ton yellow phosphorus by-product sludge phosphorus is 0.1-0.3 ton) and ton yellow phosphorus reduces the phosphorus recovery water by 5 ton (yellow phosphorus industry data, ton yellow phosphorus water consumption is 5-10 ton).
Claims (3)
1. The reducing agent for producing yellow phosphorus by a thermal method is characterized by comprising the following components in percentage by mass: 40-80% of solid waste, 10-50% of fixed carbon regulator, 1-5% of activator and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%;
the solid waste is carbon residue ash with the mass ratio of fixed carbon of 30-80% and the mass ratio of volatile matters of 0.1-1.5%; the fixed carbon regulator is coke breeze with the fixed carbon mass ratio of 40-88% and the volatile matter mass ratio of not more than 4%; the activator is calcium sulfate; the molding agent is sodium silicate.
2. The method for preparing the reducing agent for producing the yellow phosphorus by the thermal method as claimed in claim 1, which is characterized by comprising the following steps:
step 1, weighing the following components in percentage by mass: 40-80% of solid waste, 10-50% of fixed carbon regulator, 1-5% of activator and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%;
the solid waste is carbon residue ash with the mass ratio of fixed carbon of 30-80% and the mass ratio of volatile matters of 0.1-1.5%; the fixed carbon regulator is coke breeze with the fixed carbon mass ratio of 40-88% and the volatile matter mass ratio of not more than 4%; the activator is calcium sulfate, and the molding agent is sodium silicate;
step 2, adding water into the solid waste weighed in the step 1 and stirring to obtain wet solid waste with the water content of 5-10% by mass;
step 3, mixing 50-80% of the wet solid waste prepared in the step 2 with the fixed carbon regulator, the activating agent and the molding agent weighed in the step 1 uniformly, heating, humidifying and activating to obtain a mixed material with the temperature of 25-65 ℃, the humidity of 15-26 and the activity of S50-S95;
step 4, extruding and forming the mixed material prepared in the step 3 to obtain material particles;
step 5, adding the rest of the wet solid waste prepared in the step 2 to the material particles prepared in the step 4 for strength enhancement;
step 6, drying the reinforced material particles in the step 5;
and 7, screening the material particles dried in the step 6 to obtain the product.
3. The method for preparing the reducing agent for producing the yellow phosphorus by the thermal method according to claim 2, wherein the granularity and the strength of the material particles obtained by screening in the step 7 are respectively 3-15 mm and 30-45N.
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