CN114408885A - 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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- CN114408885A CN114408885A CN202111635840.1A CN202111635840A CN114408885A CN 114408885 A CN114408885 A CN 114408885A CN 202111635840 A CN202111635840 A CN 202111635840A CN 114408885 A CN114408885 A CN 114408885A
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- 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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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 activating agent 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 provided by the invention 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 processes, 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
The reducing agent used in the yellow phosphorus industry at present is coke, and anthracite is adopted to replace the coke in order to reduce the production raw material cost for part of enterprises. The main indexes are as follows:
the prior yellow phosphorus industry has the problems of using a reducing agent:
1. the coke is beneficial to production but has high resource and price, which causes the cost of per ton yellow phosphorus to rise by more than 1500 yuan.
2. The anthracite is lower in price than coke, but has high volatile matter content, the volatile matter generates a large amount of tar in a yellow phosphorus electric furnace and enters a subsequent process along with yellow phosphorus furnace gas, the normal operation of a yellow phosphorus furnace gas-solid separation device is seriously influenced, and dust in the furnace gas cannot be separated, so that a large amount of phosphorus sludge (0.3 ton phosphorus sludge/yellow phosphorus) is generated, the phosphorus yield is reduced, and meanwhile, the environmental protection pressure is brought;
3. the tar and the yellow phosphorus are mixed together and can not 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 also aims to provide a preparation method of the reducing agent for producing the yellow phosphorus by the 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 activating agent and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%.
The first technical solution of the present invention is also characterized in that,
the solid waste is residual carbon ash with the mass ratio of fixed carbon being 30-80% and the mass ratio of volatile matter being 0.1-1.5%.
The fixed carbon regulator is coke breeze with the mass ratio of fixed carbon of 40-88% and the mass ratio of volatile components 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 the yellow phosphorus by the 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 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 solid waste weighed in the step 1 and stirring to prepare wet solid waste with the water mass content of 5-10%;
step 3, taking 50-80% of the mass of the wet solid waste prepared in the step 2, uniformly mixing the wet solid waste with the fixed carbon regulator, the activator and the molding agent weighed in the step 1, 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, carrying out extrusion forming on 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 material particles reinforced in the step 5;
and 7, screening the material particles dried in the step 6 to obtain the material.
The second technical solution of the present 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 residual carbon ash with the mass ratio of fixed carbon being 30-80% and the mass ratio of volatile matter being 0.1-1.5%.
The fixed carbon regulator is coke breeze with the mass ratio of fixed carbon of 40-88% and the mass ratio of volatile components of not more than 4%.
The activating agent is calcium sulfate and the molding agent is sodium silicate.
The invention has the beneficial effects that:
1. the waste utilization is realized, and the energy utilization rate is improved by 2 percent.
2. Compared with the coke, the reducing agent is expected to reduce the production cost of yellow phosphorus by 10-13%.
3. The tar and dust content in the yellow phosphorus furnace gas is greatly reduced, and the purity of the yellow phosphorus is expected to be improved by 0.3-0.7%.
4. The tar blocking the micropores of the gas-solid separation equipment is thoroughly eliminated, the guarantee is provided for the long-term stable operation of the subsequent furnace gas-solid separation equipment, the condition is created for realizing anhydrous phosphorus recovery, the chronic disease that the environment is polluted by phosphorus sludge and phosphorus recovery wastewater puzzling the yellow phosphorus industry for many years can be solved, and the emission of 0.3 ton of phosphorus sludge is reduced by one ton of yellow phosphorus through preliminary estimation, and the emission of 5 tons of phosphorus recovery water is reduced by one ton of yellow phosphorus.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the reducing agent for producing yellow phosphorus by a thermal method.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
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 activating agent and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%.
Wherein, the solid waste is preferably fixed with carbon residue ash with the mass ratio of 30-80% and the mass ratio of volatile matter of 0.1-1.5%; the fixed carbon regulator is preferably powdered coke with the mass ratio of fixed carbon of 40-88% and the mass ratio of volatile components of not more than 4%; the activator is preferably calcium sulfate; sodium silicate is preferred as the styling agent.
The invention also provides a preparation method of the reducing agent for producing yellow phosphorus by a thermal method, which comprises the following steps as shown in figure 1:
step 1, weighing the following components in percentage by mass: 40-80% of residual carbon 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 mass content of 5-10%;
step 3, uniformly mixing 50-80% of the wet carbon residue ash content prepared in the step 2 with the coke breeze, the activating agent and the molding agent weighed in the step 1, 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, carrying out extrusion forming on 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, namely, reacting activated active substances, a molding agent and the like in the particles to achieve the purpose of increasing the particle strength;
step 6, drying the material particles reinforced in the step 5;
and 7, screening the material particles dried in the step 6 to obtain finished product particles with the particle size and the strength of 3-15 mm and 30-45N respectively, sending the finished product particles to a yellow phosphorus electric furnace to prepare yellow phosphorus, and sending fine powder under the screen to the step 2 for recycling.
Example 1
Weighing the following components in percentage by mass: 40% of residual carbon ash, 50% of coke breeze, 5% of calcium sulfate and 5% of sodium silicate; adding water into the weighed residual carbon ash, and stirring to prepare wet residual carbon ash with the water mass content of 5%; uniformly mixing 50% of wet carbon residue ash content with coke breeze, an activating agent and a molding agent, heating, humidifying and activating to obtain a mixed material with the temperature of 25 ℃, the humidity of 15% and the activity of S80; carrying out extrusion forming on the mixed material to obtain material particles; adding the remaining 50% of wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the granularity and the strength of 86% (the particle size is 3-15 mm) and 38N respectively.
Example 2
Weighing the following components in percentage by mass: 80% of residual carbon ash, 10% of coke breeze, 5% of calcium sulfate and 5% of sodium silicate; adding water into the weighed residual carbon ash, and stirring to prepare wet residual carbon ash with the water mass content of 10%; uniformly mixing 80% of wet carbon residue ash content with coke breeze, an activating agent and a molding agent, heating, humidifying and activating to obtain a mixed material with the temperature of 65 ℃, the humidity of 20% and the activity of S95; carrying out extrusion forming on the mixed material to obtain material particles; adding the remaining 20% of wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the granularity and the strength of 93 percent (the particle size is 3-15 mm) and 45N respectively.
Example 3
Weighing the following components in percentage by mass: 80% of residual carbon ash, 18% of coke breeze, 1% of calcium sulfate and 1% of sodium silicate; adding water into the weighed residual carbon ash, and stirring to prepare wet residual carbon ash with the water mass content of 8%; uniformly mixing 60% of wet carbon residue ash content with coke breeze, an activating agent and a molding agent, heating, humidifying and activating to obtain a mixed material with the temperature of 50 ℃, the humidity of 26% and the activity of S50; carrying out extrusion forming on the mixed material to obtain material particles; adding the remaining 40% of wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the granularity and the strength of 80% (the particle size is 3-15 mm) and 30N respectively.
Example 4
Weighing the following components in percentage by mass: 60% of residual carbon ash, 35% of coke breeze, 2% of calcium sulfate and 3% of sodium silicate; adding water into the weighed residual carbon ash, and stirring to prepare wet residual carbon ash with the water mass content of 6%; uniformly mixing 70% of wet carbon residue ash content with coke breeze, an activating agent and a molding agent, heating, humidifying and activating to obtain a mixed material with the temperature of 40 ℃, the humidity of 22% and the activity of S78; carrying out extrusion forming on the mixed material to obtain material particles; adding the remaining 30% of wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the granularity and the strength of 85% (the particle size is 3-15 mm) and 37N respectively.
Example 5
Weighing the following components in percentage by mass: 55% of residual carbon ash, 40% of coke breeze, 3% of calcium sulfate and 2% of sodium silicate; adding water into the weighed residual carbon ash, and stirring to prepare wet residual carbon ash with the water mass content of 7%; uniformly mixing 80% of wet carbon residue ash content with coke breeze, an activating agent and a molding agent, heating, humidifying and activating to obtain a mixed material with the temperature of 35 ℃, the humidity of 20% and the activity of S75; carrying out extrusion forming on the mixed material to obtain material particles; adding the remaining 20% of wet solid waste into the material particles for strength enhancement; drying and screening to obtain finished product particles with the granularity and the strength of 83 percent (the particle size is 3-15 mm) and 35N respectively.
Through the mode, the beneficial effects of the invention are as follows:
1. the waste utilization is realized, and the energy utilization rate is improved by 2 percent. According to industrial data, in the operation process of the coal-based conversion utilization device, the yield of the carbon residue ash accounts for 3% of the coal charging amount, the coal heat value is 6083kcal/kg, the heat value of the carbon residue ash is 4590kcal/kg, and the energy utilization rate of the carbon residue ash is 90%, so that the improved energy utilization rate can be calculated according to the following formula: (4590 x 3% 90%)/6083 ═ 2.04%.
2. Compared with the coke, the reducing agent is expected to reduce the production cost of yellow phosphorus by 10-13%. According to the average cost of yellow phosphorus factory (raw material + electricity) in Guizhou province in 2020, and 13000 Yuan per ton of yellow phosphorus (using coke), if the cost of yellow phosphorus per ton is estimated to be 11600 Yuan by using the reducing agent of the present invention, the cost (raw material + electricity) (13000 + 11600)/13000 is estimated to be 10.8 percent lower.
3. The tar and dust content in the yellow phosphorus furnace gas is greatly reduced, and the purity of the yellow phosphorus is expected to be improved by 0.3-0.7%. According to the calculation of white coal (anthracite), about 10.5 kg of tar as a byproduct of each ton of yellow phosphorus is mixed with 30-60% of tar and a yellow phosphorus finished product, and the purity of the yellow phosphorus is influenced by 10.5 x 0.6/1000 to 0.63%.
4. The tar blocking the micropores of the gas-solid separation equipment is thoroughly eliminated, the guarantee is provided for the long-term stable operation of a subsequent furnace gas-solid separation device, and the condition is created for realizing anhydrous phosphorus recovery, so that the problem that the environment is polluted by phosphorus recovery wastewater and mud phosphorus which puzzles the yellow phosphorus industry for many years can be solved, the emission of the mud phosphorus is reduced by 0.3 ton (the data of the yellow phosphorus industry and the byproduct of the mud phosphorus is 0.1-0.3 ton) for one ton of yellow phosphorus through preliminary estimation, and the emission of the mud phosphorus is reduced by 5 ton (the data of the yellow phosphorus industry and the consumption of the yellow phosphorus water is 5-10 ton) for one ton of yellow phosphorus.
Claims (10)
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 activating agent and 1-5% of molding agent, wherein the sum of the mass percentages of the components is 100%.
2. The reducing agent for producing yellow phosphorus by a thermal method according to claim 1, wherein the solid waste is residual carbon ash containing 30 to 80% by mass of fixed carbon and 0.1 to 1.5% by mass of volatile matter.
3. The reducing agent for producing yellow phosphorus by a thermal process according to claim 1, wherein the fixed carbon regulator is coke breeze containing 40-88% by mass of fixed carbon and no more than 4% by mass of volatile matter.
4. The reducing agent for thermal yellow phosphorus production according to claim 1, wherein the activator is calcium sulfate.
5. The reducing agent for producing yellow phosphorus by a thermal process according to claim 1, wherein the forming agent is sodium silicate.
6. The method of claim 1, comprising the steps of:
step 1, weighing the following components in percentage by mass: 40-80% of solid waste, 10-50% of fixed carbon regulator, 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 solid waste weighed in the step 1 and stirring to prepare wet solid waste with the water mass content of 5-10%;
step 3, taking 50-80% of the mass of the wet solid waste prepared in the step 2, uniformly mixing the wet solid waste with the fixed carbon regulator, the activator and the molding agent weighed in the step 1, 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, carrying out extrusion forming on 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 material particles reinforced in the step 5;
and 7, screening the material particles dried in the step 6 to obtain the material.
7. The method for preparing a reducing agent for producing yellow phosphorus by a thermal method according to claim 6, wherein the particle size and strength of the material particles obtained by screening in the step 7 are respectively 3-15 mm and 30-45N.
8. The method of claim 6, wherein the solid waste is carbon residue ash containing 30-80% by mass of fixed carbon and 0.1-1.5% by mass of volatile components.
9. The method for preparing a reducing agent for producing yellow phosphorus by a thermal process according to claim 6, wherein the fixed carbon regulator is coke breeze containing 40-88% by mass of fixed carbon and no more than 4% by mass of volatile matter.
10. The method of claim 6, wherein the activator is calcium sulfate and the forming agent is sodium silicate.
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