CN111394133A - Gasification reduction device and method for co-producing yellow phosphorus and synthesis gas - Google Patents

Gasification reduction device and method for co-producing yellow phosphorus and synthesis gas Download PDF

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CN111394133A
CN111394133A CN202010330541.6A CN202010330541A CN111394133A CN 111394133 A CN111394133 A CN 111394133A CN 202010330541 A CN202010330541 A CN 202010330541A CN 111394133 A CN111394133 A CN 111394133A
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phosphorus
slag
coal
unit
gasification reduction
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许洋
毛炜
赵静一
王明坤
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Guizhou Aerospace Maiwei Technology Co ltd
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Guizhou Aerospace Maiwei Technology Co ltd
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    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
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    • C01B2203/06—Integration with other chemical processes
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    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0903—Feed preparation
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    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0953—Gasifying agents
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    • C10J2300/00—Details of gasification processes
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    • C10J2300/00—Details of gasification processes
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    • C10J2300/00—Details of gasification processes
    • C10J2300/16—Integration of gasification processes with another plant or parts within the plant
    • C10J2300/1625—Integration of gasification processes with another plant or parts within the plant with solids treatment
    • C10J2300/1628—Ash post-treatment
    • 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 provides a gasification reduction device for co-producing yellow phosphorus and synthesis gas, which comprises a phosphorus coal gasification reduction unit and a chilling unit, wherein the phosphorus coal gasification reduction unit is communicated with the chilling unit from top to bottom, and the phosphorus coal gasification reduction unit: the gasification reduction reaction of all materials in the phosphorus coal gasification reduction unit is realized to obtain phosphorus-containing furnace gas; the quench unit: used for cooling slag formed in the process of the coal gasification reduction reaction of the phosphorus to be solid and discharging the solid. The invention also provides a method for co-producing yellow phosphorus and synthesis gas by using the gasification reduction device. The invention is a technology with high energy utilization rate, optimized process, energy conservation, environmental protection and lower cost.

Description

Gasification reduction device and method for co-producing yellow phosphorus and synthesis gas
Technical Field
The invention relates to the field of chemical industry, in particular to a gasification reduction device and a gasification reduction method for co-producing yellow phosphorus and synthesis gas.
Background
Yellow phosphorus is one of important basic chemical raw materials, is an important parent raw material for producing thermal phosphoric acid and phosphide, and is an important raw material for preparing fine phosphate and fine organic phosphorus chemical industry. At present, only two methods can be used for industrialized yellow phosphorus production: the blast furnace method for preparing phosphorus and the electric furnace method for preparing phosphorus.
The technological process of blast furnace phosphorus preparation is that lump phosphate rock is used as material, silica is used as flux, coke and anthracite are used as reductant and fuel, and they are added into blast furnace in certain proportion and order. The coke is combusted by hot air in the furnace to provide heat, simultaneously, the residual coke and the molten phosphate rock are subjected to chemical reduction reaction under the high-temperature condition, furnace gas escapes from the top of the blast furnace, and a phosphorus product is obtained by a dust removal device and a condensation refining device.
The blast furnace method for preparing phosphorus has two problems which are not solved: first, the reduction rate is low. The pilot plant conducted in the last 30 th century abroad showed that the minimum residual phosphorus in the slag can reach 1.5% (P)2O5Content), the reduction rate of the corresponding phosphorus is more than 90%, but the highest reduction rate actually achieved by the domestic test device is 73.9%. Secondly, it is not economical. The main reason why the technology of making phosphorus by blast furnace method in the last century abroad can be developed is that the electric power resource is in shortage, the electricity price is relatively high, and the coke price is relatively cheap. With the development of the power generation industry, the power supply is abundant, the electricity price is reduced, the blast furnace method has no cost advantage compared with the electric furnace method, and the blast furnace method gradually loses the market. The production of yellow phosphorus by electric furnace method is that the mixed charging material of phosphorus ore, silica and coke is added into an electric furnace, and the electric energy is introduced into the electric furnace and converted into heat energy to melt the material and generate chemical reduction reaction, so that the material therein is subjected to chemical reduction reactionThe phosphorus is sublimated, and the phosphorus-containing furnace gas is subjected to condensation washing, refining and separation to obtain the finished product phosphorus. However, the electric furnace method has high energy consumption and heavy pollution, can not realize long-period continuous production, and requires high grade of phosphate ore. The current yellow phosphorus production technology cannot meet the new requirements of low carbon and environmental protection.
Coal gasification refers to the process of converting solid fuels such as coal, coke, semi-coke, etc. into gas products and a small amount of residues by reacting with a gasification agent under the conditions of high temperature, normal pressure or pressurization. The coal gasification process can be used for producing fuel gas, as industrial gas and city gas, and also for producing synthesis gas, as raw material for synthesizing ammonia, methanol and liquid fuel.
CN103897737A discloses a method for co-producing synthetic gas by phosphorus smelting in a total oxygen shaft furnace and a device for co-producing synthetic gas by phosphorus smelting, wherein the device continues the smelting idea of preparing phosphorus by a blast furnace method, and the total oxygen shaft furnace comprises a preheating zone, a reaction zone, a combustion zone, a furnace cylinder, a feed inlet, a coal gas outlet, a seal and a slag outlet. During specific operation, apatite carbo-pellets and fuel coal are mixed to obtain furnace burden, the furnace burden is added from a charging opening at the top of the shaft furnace, and pure oxygen and steam are introduced from a tuyere at the lower part of the shaft furnace; high-temperature flue gas generated by burning fuel coal at the lower part of the shaft furnace reversely heats descending furnace burden; in the middle of the shaft furnace, reducing agent carbon in the apatite and carbon pellets reduces phosphorus pentoxide in the apatite into elemental phosphorus, meanwhile, fuel coal is subjected to gasification reaction, and generated phosphorus-containing coal gas is discharged from a coal gas outlet at the top of the shaft furnace. However, the reaction zone of the shaft furnace is configured only, so that the heat generated by the coal gasification reaction is not utilized efficiently, a slag discharge method of the shaft furnace is not described in detail, and the smooth discharge of the discharged slag is a key factor influencing the normal operation of the shaft furnace.
Therefore, a gasification reduction device for co-producing yellow phosphorus and synthesis gas, which has the advantages of high energy utilization rate, optimized process, energy conservation, environmental protection and lower cost, is developed.
Disclosure of Invention
In order to solve the defects, the invention provides a gasification reduction device for co-producing yellow phosphorus and synthesis gas.
The technical scheme of the invention is as follows:
a gasification reduction device for co-producing yellow phosphorus and synthesis gas comprises a phosphorus coal gasification reduction unit and a chilling unit, wherein the phosphorus coal gasification reduction unit is communicated with the chilling unit from top to bottom;
the phosphorus coal gasification reduction unit: the gasification reduction reaction of all materials in the phosphorus coal gasification reduction unit is realized to obtain phosphorus-containing furnace gas;
the quench unit: used for cooling slag formed in the process of the coal gasification reduction reaction of the phosphorus to be solid and discharging the solid.
Further, the phosphorus coal gasification reduction unit comprises a feed inlet, a reaction chamber and a slag pool which are sequentially arranged from top to bottom;
the feeding hole is positioned above the reaction chamber and used for providing solid materials for the coal gasification reduction reaction of the phosphorus;
an air inlet is formed in the lateral lower part of the reaction chamber and used for providing gas materials for the phosphorus coal gasification reduction reaction;
an air outlet is arranged at the lateral upper part of the reaction chamber and used for leading out the phosphorus-containing furnace gas;
and the slag pool is positioned right below the reaction chamber and used for receiving slag formed in the phosphorus coal gasification reduction reaction and discharging the slag to the chilling unit positioned below the slag pool.
Further, the solid material comprises phosphorus pellet and raw coal and/or coke, wherein the phosphorus pellet can be prepared by crushing, grinding and mixing phosphate ore, anthracite and silica according to a certain proportion.
Further, the gas material comprises oxygen and water vapor, and the proportion of the oxygen and the water vapor can be controlled to be 1.05-1.1 Nm3And/kg, which is beneficial to the stable operation of the gasification reduction device.
Furthermore, the gas inlet can comprise a plurality of gasifying agent nozzles, the gasifying agent nozzles are positioned above the slag pool and are uniformly distributed along the circumferential direction at an included angle of 0-30 degrees with the horizontal plane, so that the gas material is sprayed into the reaction chamber at a high speed through the gasifying agent nozzles to perform coal gasification reaction with raw material coal and/or coke, local high temperature is formed inside the reaction chamber, and meanwhile, the reduction reaction temperature of the phosphorus pellet can be adjusted.
Furthermore, at least one coal material layer and at least one phosphorus material layer can be arranged in the reaction chamber, the coal material layer comprises raw material coal and/or coke, the phosphorus material layer comprises phosphorus pellet balls, the coal material layer and the phosphorus material layer can be arranged in a spaced laying mode, and the coal material layer positioned at the lower part of the reaction chamber is contacted with oxygen at the bottom of the reaction chamber and is combusted to generate high-temperature furnace gas to flow upwards; along with the upward flow of the high-temperature furnace gas, the materials of the upper phosphorus layer are fully mixed and contacted, so that the phosphorus ore in the phosphorus pellet is reduced into elemental phosphorus. Therefore, the coal material layer and the phosphorus material layer are arranged in the reaction chamber in a layered mode, high-temperature furnace gas generated by coal gasification reaction below is fully utilized to directly provide reduction reaction heat for the phosphorus ball pellets above, heat loss of the furnace gas is reduced, and higher heat utilization rate is achieved.
Further, in order to realize the maximum energy utilization rate, the height of the coal bed and the material bed of the phosphorus bed is set skillfully, the material bed is too low, which can cause the defects of insufficient reaction, raw material waste and low product yield, the material bed is too high, which can cause insufficient mixing of materials in the reaction process, insufficient fluidity and contact efficiency of the materials in the reaction chamber, still can not ensure the best reaction state, and cause the great waste of cost and energy. Therefore, the high-temperature heat generated by gasification reaction on the lower coal bed is equal to the required heat generated by reduction reaction on the upper phosphorus bed, the quality of the phosphorus pellet and the raw material coal and/or coke is calculated through heat balance, the material volume is calculated according to the stacking density of the materials in the phosphorus pellet and the coal bed, and then a proper bed height ratio is obtained, and the proper bed height ratio of the phosphorus bed and the coal bed is set as follows:
Figure BDA0002464801290000031
Figure BDA0002464801290000032
wherein: h1-the height of the phosphorus layer consumed per hour, in m;
H2-the height of the coal bed consumed per hour in m;
q is the heat required for producing the yellow phosphorus product of unit mass, and the unit is J/kg;
q is the heat released by the reaction of unit mass of the raw material coal and/or coke and oxygen, and the unit is J/kg;
m is the mass of the product yellow phosphorus, and the unit is kg;
a-carbon content in the feed coal and/or coke,%;
b-conversion of carbon in feed coal and/or coke,%;
rho-bulk density of the feed coal and/or coke in kg/m3；
d-the diameter of the reaction chamber in m.
Further, the phosphorus coal gasification reduction unit also comprises a feeding conduit and a manhole;
the feeding conduit is positioned right below the feeding hole and used for vertically guiding the solid materials into the gasification chamber to prevent a small amount of solid materials from entering the manhole or the gas outlet, so that the mechanical scouring and abrasion to the inner wall of the phosphorus coal gasification reduction unit are reduced;
the manhole is positioned above the side of the reaction chamber and used for entering the reaction chamber during maintenance.
Furthermore, the phosphorus coal gasification reduction unit also comprises a phosphorus coal gasification reduction unit shell which can adopt a water jacket structure or a coil pipe water-cooled wall structure, and a lining refractory material is used for protecting the shell from over-temperature, and water in the water jacket or the coil pipe water-cooled wall structure can absorb heat generated by coal gasification reaction to generate steam for realizing heat recovery.
Furthermore, the slag pool can be of an inverted cone structure, the upper part of the slag pool is used for receiving slag from the reaction chamber, the lower part of the slag pool is provided with a slag outlet, and the slag outlet is communicated with the chilling unit and used for discharging the slag. The outer wall of the slag pool is a metal casting, the inner wall of the slag pool is made of refractory materials, and a cooling water pipe is arranged between the outer wall and the inner wall. The temperature of the cooling water pipe can be 30-60 ℃, the temperature difference between an inlet and an outlet can be 10-20 ℃, and through the cooling treatment of the cooling water pipe, part of the slag can form a layer of solid slag on the boundary of the inner wall of the slag pool and adhere to the inner wall, so that a layer of solid slag formed between the cooling water pipe and the slag keeps dynamic balance and can play a role in protecting the metal casting on the outer wall. In particular, the diameter of the slag outlet may be 30-70mm, the metal casting is a pure copper casting, and the refractory material is refractory brick.
Further, the chilling unit is located below the phosphorus coal gasification reduction unit and connected with the phosphorus coal gasification reduction unit through a flange, and the slag outlet penetrates through the flange to directly pass through the chilling unit, so that the slag is discharged to the chilling unit.
Further, the quench unit comprises a combustion chamber and a quench chamber from top to bottom;
the upper part of the combustion chamber is provided with an annular air passage, an annular burner positioned on the annular air passage, an ignition gun, a flue gas cover and a flue gas cooling coil;
the annular air passage is used for introducing mixed gas of fuel and air into the annular burner;
the annular burner is used for spraying the mixed gas to the slag outlet;
the ignition gun is used for igniting the mixed gas sprayed out by the annular burner and carrying out secondary gasification on slag at the molten slag outlet in a combustion state, so that the molten slag outlet is always kept in a non-blocking state;
the flue gas hood is used for forming a gasification space, and flue gas generated by secondary gasification is sealed in the flue gas hood through the liquid seal effect of the lower chilling water;
and the flue gas cooling coil is connected above the flue gas hood and used for discharging flue gas generated by secondary gasification out of the chilling unit. Specifically, the flue gas cooling coil further comprises an exhaust inlet and an exhaust outlet, the exhaust inlet can be arranged in the flue gas cover, and the exhaust outlet is arranged outside the chilling unit.
Furthermore, the chilling chamber is located below the combustion chamber, chilling water is filled in the chilling chamber, a solid slag charge outlet is formed in the bottom of the chilling chamber and used for cooling and discharging slag charges which are not completely combusted in secondary gasification, and meanwhile, the chilling chamber is also used for cooling smoke in the smoke cooling coil pipe. Specifically, the temperature of the chilling water may be 50 to 60 ℃.
Further, when the phosphorus coal gasification reduction unit normally works, the solid slag outlet is in a closed state; when the amount of the solid slag reaches the discharge standard, connecting a slag collecting component with the solid slag outlet, boosting the pressure until the pressure condition in the slag collecting component and the pressure condition in the chilling unit reach balance, opening the solid slag outlet, allowing the solid slag to fall into the slag collecting component under the action of gravity, sealing the solid slag outlet, and continuing to perform subsequent operation.
Further, cooling water is filled in the slag collecting assembly and used for preventing the chilling water in the chilling chamber from falling into the slag collecting assembly.
Further, the quench unit also includes a quench unit enclosure that is not provided with a water jacket and a refractory material.
The invention also provides a method for co-producing yellow phosphorus and synthesis gas by using the gasification reduction device for co-producing yellow phosphorus and synthesis gas, which comprises a phosphorus gasification reduction reaction process and a slag discharge process;
the phosphorus coal gasification reduction reaction process comprises the following steps:
a1: crushing and grinding the phosphate ore, anthracite and silica into powder, and mixing the powder with the phosphate ore: anthracite coal: the mass ratio of silica is (30-80): (10-30): (10-20) mixing the phosphorus pellets to prepare phosphorus pellet pellets, and feeding the prepared phosphorus pellet pellets and the raw material coal and/or coke into the reaction chamber through the feeding holes respectively, wherein the phosphorus pellet is placed on the phosphorus material layer, and the raw material coal and/or coke is placed on the coal material layer;
a2: introducing water vapor and high-purity oxygen into the reaction chamber through the air inlet respectively, wherein the coal bed positioned at the lower part of the reaction chamber is contacted with the oxygen at the bottom of the reaction chamber and is combusted to generate high-temperature furnace gas which flows upwards;
a3: and driving the whole heat flow and circulation inside the reaction chamber along with the upward flow of the furnace gas, simultaneously promoting the materials in the reaction chamber to be fully mixed and contacted, wherein the pressure in the reaction chamber is 1-10MPa, the temperature is 1200-1600 ℃, the phosphate ore in the phosphorus pellet is reduced into simple substance phosphorus, and the phosphorus-containing furnace gas generated in the reaction process is discharged from the gas outlet.
The slag discharging process comprises the following steps:
s1: when the phosphorus coal gasification reduction unit normally operates, the ignition gun ignites mixed gas of fuel and air sprayed by the annular burner, secondary gasification is carried out on slag at a slag outlet in a combustion state, flue gas generated by secondary gasification is sealed in a gasification space formed by the flue gas cover and the quenching water and is discharged out of the chilling unit through the flue gas cooling coil, and the difference value of the pressure P1 in the flue gas cover being greater than the pressure P2 in the slag pool is kept to be 5-15Kpa by controlling the amount of the mixed gas introduced into the annular burner, wherein the pressure P1-P2 is rhoSlag chargeg(h0-h)，h0Is the height of the slag bath, and h is the height of the slag charge, so as to prevent the slag charge in the slag bath from falling into the chilling unit;
s2: and gradually reducing the pressure difference P1-P2 between the flue gas cover and the slag bath along with the increase of slag materials borne in the slag bath, stopping introducing mixed gas into the annular burner when the pressure difference is lower than 5Kpa, discharging the slag materials which are not completely combusted in secondary gasification through the slag outlet, falling into chilled water, cooling to form solid slag materials, discharging the solid slag materials through the solid slag material outlet, and repeating the steps S1 and S2 after the slag discharge process is finished.
Further, in a1, the preparation process of the phosphorus ball pellet comprises: grinding phosphate ore, anthracite and silica into fine powder of 60-100 meshes, and mixing the fine powder with the following components in percentage by weight: anthracite coal: silica 13: 4: 3, adding any one or more of refractory cement, sodium humate, pergolide, water glass and bentonite, pressing into pellets with the particle size of 10-30 mm, and drying to prepare the phosphorus pellet with the compressive strength of 1800N/pellet.
Further, in a2 and A3, the chemical reaction formula in the reaction chamber is as follows:
(1) coal gasification reaction:
C+O2＝CO2
2C+O2＝2CO
C+CO2＝2CO
C+H2O＝H2+CO
C+2H2O＝2H2+CO2
CO+H2O＝H2+CO2
wherein the temperature of the generated high-temperature furnace gas is 1400-1600 ℃;
(2) reduction reaction of phosphorus pellet: the reaction starts to occur in the temperature range of 1152-1177 ℃, and when the temperature reaches about 1227 ℃, the reaction is almost completely carried out, and the reaction formula is as follows:
Ca3(PO4)2+5C+3SiO2＝3CaSiO2+5CO+P2
when the temperature reaches over 1352 ℃, the reaction formula is as follows:
Ca3(PO4)2+5C＝3CaO+5CO+P2
the reduction reaction can proceed spontaneously, with the equilibrium direction of the reaction tending to form P2The yield (more than 95%) of the yellow phosphorus of the product is far higher than that of the existing yellow phosphorus production technology (not more than 90%).
Further, in S1 and S2, the pressure difference P1-P2 between the flue gas hood and the slag pool can be judged by monitoring the pressure gauges of the slag pool and the flue gas hood;
when the phosphorus coal gasification reduction unit normally operates, before slag generated by phosphorus coal gasification reduction reaction falls into the slag pool, controlling the amount of mixed gas introduced into the annular burner so that the pressure difference P1-P2 between the flue gas cover and the slag pool is rhoSlag chargegh0Wherein h is0Is the height of the slag bath;
as the slag received in the slag pool increases, the pressure difference between the flue gas cover and the slag pool is P1-P2 ═ rhoSlag chargeg(h0-h) progressively decreasing, said pressure difference P1-P2 being 0 when said slag bath is filled with slag; in general, when the pressure difference value is reduced to be below 5kPa, the mixed gas is stopped from being introduced into the flue gas burner, and the slag is prepared to be discharged.
The technical scheme provided by the invention can have the following beneficial effects:
1. according to the gasification reduction device for co-producing yellow phosphorus and synthesis gas, the phosphorus coal gasification reduction unit and the chilling unit are connected into a whole up and down, and slag formed in the phosphorus coal gasification reduction reaction process is intermittently discharged into the chilling unit for cooling treatment, so that the continuous and stable operation of the whole gasification reduction device is promoted, and the environment-friendly and green discharge of the slag is facilitated.
2. The slag pool and the chilling unit are matched for use to carry out cooling slag discharge treatment on the slag, wherein the slag formed in the process of the phosphorus coal gasification reduction reaction is discharged into the slag pool provided with cooling water, and the annular burner in the chilling unit is utilized to carry out secondary gasification on the slag at the slag outlet, so that the problem that the slag is easy to block the slag outlet in the prior art is solved, and the reliability and the stability of the gasification reduction device are ensured.
3. The chilling unit is further provided with a smoke cover, a smoke cooling coil pipe and other components, smoke generated by secondary gasification of slag materials is sealed in the smoke cover and then is cooled and discharged outside the gasification reduction device, and independent discharge of gas-solid waste materials in the chilling unit is realized; in addition, the arrangement of the flue gas hood can prevent slag from splashing to the inner wall of the chilling unit when the slag is combusted, a certain flow guide space is provided for the slag to fall into chilling water, and meanwhile, an exhaust inlet can be arranged in the flue gas hood, so that the surface stress on the inner wall of the chilling unit is reduced, and the safe operation of the whole device is facilitated;
4. the phosphorus coal gasification reduction unit combines the advantages of high gasification efficiency and high gasification strength of pressurized coal gasification and the advantage of direct treatment of middle-low grade phosphorus ore by preparing phosphorus by a blast furnace method, and realizes the co-production of yellow phosphorus and synthesis gas.
5. According to the phosphorus coal gasification reduction unit, the phosphorus material layer and the coal material layer are arranged at intervals in a layered mode, high-temperature furnace gas generated by the pressurized gasification reaction of the lower coal material layer is fully utilized to directly provide reduction reaction heat for the upper phosphorus material layer, and heat loss of the furnace gas is reduced. Compared with the total oxygen shaft furnace in the prior art, the phosphorus coal gasification reduction unit has the advantages that the heat utilization rate can reach 80-85 percent, and the yield of yellow phosphorus can reach more than 95 percent.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
FIG. 1 is a schematic diagram of a gasification reduction plant for co-producing yellow phosphorus and syngas according to an exemplary embodiment, wherein FIG. 1(a) is a schematic diagram of the overall structure and FIG. 1(b) is a schematic diagram of a partial enlargement;
FIG. 2 is a schematic structural view of a slag bath shown in accordance with an exemplary embodiment.
The reference numbers are as follows:
1-a phosphorus coal gasification reduction unit,
11-reaction chamber
12-feed inlet
13-air intake
14-air outlet
15-slag bath
151-slag outlet
152-outer wall of slag bath
153-Cooling Water pipe
154-inner wall of slag bath
16-feed conduit
17-manhole
18-phosphorus coal gasification reduction unit casing
19-refractory material
2-quench chamber Unit
21-annular air flue
211-ring burner
22-chilled liquid level
23-ignition gun
24-solid slag discharge
25-flue gas hood
26-flue gas cooling coil
261-exhaust gas inlet
262-exhaust outlet
27-quench chamber Unit Enclosure
3-Flange
Detailed Description
The following description and the drawings sufficiently illustrate specific embodiments of the invention to enable those skilled in the art to practice them. The examples merely typify possible variations. Individual components and functions are optional unless explicitly required, and the sequence of operations may vary. Portions and features of some embodiments may be included in or substituted for those of others. The scope of embodiments of the invention encompasses the full ambit of the claims, as well as all available equivalents of the claims. Embodiments may be referred to herein, individually or collectively, by the term "invention" merely for convenience and without intending to voluntarily limit the scope of this application to any single invention or inventive concept if more than one is in fact disclosed. Herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed. The embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the structures, products and the like disclosed by the embodiments, the description is relatively simple because the structures, the products and the like correspond to the parts disclosed by the embodiments, and the relevant parts can be just described by referring to the method part.
The invention is further described with reference to the following figures and examples:
as shown in fig. 1(a) and 1(b), a gasification reduction apparatus for co-producing yellow phosphorus and syngas includes a phosphorus coal gasification reduction unit 1 and a chilling unit 2, wherein the phosphorus coal gasification reduction unit 1 and the chilling unit 2 are connected and integrated by a flange 3. The coal gasification reduction unit 1 is mainly used for realizing the gasification reduction reaction of phosphorus pellet, raw material coal and/or coke, oxygen and water vapor to obtain phosphorus-containing furnace gas; the chilling unit 2 is mainly used for cooling slag formed in the process of the coal gasification reduction reaction of phosphorus into a solid state and discharging the solid state.
The phosphorus coal gasification reduction unit 1 comprises a reaction chamber 11, a feed inlet 12, a gas inlet 13, a gas outlet 14, a slag pool 15, a feed conduit 16, a manhole 17, a phosphorus coal gasification reduction unit shell 18 and refractory materials 19;
wherein, the feed inlet 12 is positioned right above the reaction chamber 11 and is used for providing solid materials, namely phosphorus pellet and raw coal, for the phosphorus coal gasification reduction reaction;
the gas inlet 13 is positioned below the side of the reaction chamber 11 and above the slag pool 15 and is used for providing gas materials, namely oxygen and water vapor, for the phosphorus coal gasification reduction reaction, wherein the gas inlet 13 comprises a plurality of gasification agent nozzles which form an included angle of 20 degrees with the horizontal plane and are circumferentially arranged, and the gas materials are sprayed into the reaction chamber 11 at a high speed through the gasification agent nozzles to perform the coal gasification reaction with raw material coal, so that local high temperature is formed inside the reaction chamber 11, and meanwhile, the reduction reaction temperature of phosphorus pellet pellets can be adjusted;
the gas outlet 14 is positioned above the side of the reaction chamber 11 and used for leading out phosphorus-containing furnace gas;
the slag pool 15 is positioned under the reaction chamber 11 and has an inverted cone structure, the upper part of the slag pool is used for receiving slag from the reaction chamber 11, the lower part of the slag pool is provided with a slag outlet 151, and the slag outlet 151 penetrates through the flange 3 to be directly communicated with the chilling unit 2 and is used for discharging slag materials into the chilling unit 2;
at least one coal material layer 111 and at least one phosphorus material layer 112 are arranged in the reaction chamber 11, the coal material layer 111 comprises raw coal and/or coke, the phosphorus material layer 112 comprises phosphorus pellet, the coal material layer 111 and the phosphorus material layer 112 are arranged in a layered mode in an interval laying mode, and the material layer height ratio of the coal material layer 111 to the phosphorus material layer 112 is H1/H21.4; when the phosphorus coal gasification reduction reaction is carried out, the coal bed 111 at the lower part of the reaction chamber 11 is contacted with oxygen at the bottom of the reaction chamber 11 and is combusted to generate high-temperature furnace gas which flows upwards, and the materials of the upper phosphorus bed 112 are fully mixed and contacted with the high-temperature furnace gas flowing upwards, so that the phosphorus ore in the phosphorus pellet is reduced into elemental phosphorus;
a feeding conduit 16 is positioned right below the feeding hole 12 and used for vertically guiding solid materials into the gasification chamber 11 and preventing a small amount of solid materials from entering a manhole 17 or an air outlet 14, so that the mechanical scouring and abrasion to the inner wall of the phosphorus coal gasification reduction unit 1 are reduced; the manhole 17 is positioned above the side of the reaction chamber and is used for entering the reaction chamber 11 during maintenance;
the outer shell 18 of the phosphorus coal gasification reduction unit can adopt a water jacket structure or a coil pipe water-cooled wall structure, and is lined with a refractory material 19 for reducing the heat radiation from inside to outside of the reaction chamber 11, protecting the outer shell 18 from over temperature, and simultaneously generating steam to realize heat recovery.
The chilling unit 2 is positioned below the phosphorus coal gasification reduction unit 1, is connected with the phosphorus coal gasification reduction unit 1 through a flange 3, and comprises a combustion chamber, a chilling chamber and a chilling unit shell 27;
the combustion chamber comprises an annular air flue 21, an annular burner 211 positioned on the annular air flue, an ignition gun 23, a solid slag charge outlet 24, a flue gas cover 25 and a flue gas cooling coil 26;
the annular air flue 21 is positioned below the slag outlet 151 and used for introducing mixed gas of natural gas and air into the annular burner 211, the annular air flue 21 is an annular multi-channel metal component, and air holes are uniformly distributed on the inner side of the annular channel;
the annular burner 211 is used for injecting mixed gas of natural gas and air into the slag outlet 151;
the ignition gun 23 is positioned below the annular air passage 21 and used for igniting the mixed gas sprayed by the annular burner 211, and performing secondary gasification on slag at the slag outlet 151 in a combustion state, so that the slag outlet 151 is always kept in an unblocked state;
the flue gas cover 25 is used for forming a gasification space, and flue gas generated by secondary gasification is sealed in the flue gas cover 25 through the liquid seal effect of the lower quenching water 22;
the flue gas cooling coil 26 is used for discharging flue gas generated by secondary gasification out of the chilling unit, and comprises an exhaust inlet 261 and an exhaust outlet 262, wherein the exhaust inlet is connected to the upper part of the flue gas cover 25, and the exhaust outlet is arranged outside the chilling unit 2;
the chilling chamber is positioned below the combustion chamber, and is internally provided with chilling water 22, the bottom of the chilling chamber is provided with a solid slag charge outlet 24 which is used for discharging slag charge which is not completely combusted in secondary gasification and cooling the flue gas in a flue gas cooling coil 26, and the temperature of the chilling water can be 50-60 ℃;
when the phosphorus coal gasification reduction unit 1 normally works, the solid slag outlet 24 is in a closed state; when the amount of the solid slag reaches the discharge standard, connecting a slag collecting component (not shown in the figure) with a solid slag outlet 24, raising the temperature and the pressure until the pressure condition in the slag collecting component and the pressure condition in the chilling unit reach balance, opening the solid slag outlet 24, enabling the solid slag to fall into the slag collecting component under the action of gravity, sealing the solid slag outlet 24, and continuing to perform subsequent operation, wherein cooling water is filled in the slag collecting component and used for preventing chilling water 22 in the chilling chamber from falling into the slag collecting component;
the quench unit enclosure is not provided with a water jacket and refractory material.
As shown in FIG. 2, the slag bath 15 has an inverted cone-shaped structure and a height h0667mm, the lower part is provided with a slag outlet 151, the slag outlet 151 is communicated with a chilling unit and is used for discharging slag, and the density of the slag is 2500kg/m3(ii) a The diameter of the slag outlet 151 is 50mm, the outer wall of the slag pool 15 is a pure steel casting 152, the inner wall of the slag pool 15 is a refractory brick 154, a cooling water pipe 153 is arranged between the outer wall 152 and the inner wall 154, the temperature of the cooling water pipe 153 is 30-60 ℃, the temperature difference between an inlet and an outlet is 10-20 ℃, part of slag can form a layer of solid slag on the boundary 154 of the inner wall of the slag pool 15 through the cooling treatment of the cooling water pipe 153, the layer of solid slag is attached to the inner wall 154, and thus a layer of solid slag formed between the cooling water pipe 153 and the slag keeps dynamic balance and can play a role in protecting the pure steel casting on the outer wall 152.
The invention discloses a gasification reduction method for co-producing yellow phosphorus and synthesis gas by using a gasification reduction device shown in figures 1 and 2, which comprises the following specific steps:
a1: the phosphorus coal gasification reduction reaction process: crushing and grinding phosphate ore, anthracite and silica into fine powder of 80 meshes, and mixing the raw materials according to the weight ratio of the phosphate ore: anthracite coal: the mass ratio of silica is 13: 4: 3, uniformly mixing, adding bentonite as a binder, pressing into phosphorus pellet with the particle size of 20mm, and drying to prepare the phosphorus pellet with the compressive strength of 1800N/pellet. Feeding the prepared phosphorus ball groups and the raw material coal into a reaction chamber 11 of a phosphorus coal gasification reduction unit 1 through a feeding hole 12 respectively, wherein the phosphorus ball groups are placed on a phosphorus material layer 111, and the raw material coal is placed on a coal material layer 112;
a2: mixing water vapor and high purity oxygen (oxygen-vapor ratio of 1.1 Nm)3Kg), respectively leading the raw materials into the reaction chamber 11 through the air inlet 13, and enabling the raw materials positioned on the coal bed 111 to be subjected to coal gasification reaction with oxygen and water vapor and to be combusted to generate 1500 ℃ high-temperature furnace gas to flow upwards;
a3: the furnace gas flows upwards to drive the whole heat in the reaction chamber 11 to flow and circulate, and simultaneously promote the materials in the reaction chamber 11 to be fully mixed and contacted, the high-temperature furnace gas heats the adjacent upper-layer phosphorus pellet to 1300 ℃, and the reaction time is kept for 30 minutes, so that the phosphorus pentoxide in the phosphorus pellet is reduced into elemental phosphorus. At this time, the pressure in the reaction chamber is about 4MPa, the temperature is about 1400 ℃, and the phosphorus-containing furnace gas generated in the reaction process is discharged from the gas outlet 14. The heat utilization rate is 85 percent, and the yield of yellow phosphorus is 95 percent.
The slag discharging process is as follows:
s1: when the phosphorus coal gasification reduction unit 1 normally operates, the ignition gun 23 is used for igniting mixed gas of fuel and air sprayed by the annular burner 211, when the phosphorus coal gasification reduction unit is in a combustion state, secondary gasification is carried out on slag at a slag outlet 151, flue gas generated by the secondary gasification is sealed in a gasification space formed by a flue gas cover 25 and chilling water 22 and is discharged out of the chilling unit through a flue gas cooling coil 26, the difference value P1-P2 that the pressure P1 in the flue gas cover is greater than the pressure P2 in the slag pool is kept to be 5-16.3kpa by controlling the amount of the mixed gas introduced into the annular burner 211, and at the moment, the solid slag outlet is in a closed state;
s2: as the slag materials in the slag pool 15 are increased, the pressure difference P1-P2 is gradually reduced, when the pressure P1-P2 is monitored to be lower than 5Kpa through a flue gas cover and a slag pool pressure gauge, the mixed gas is stopped to be introduced into the annular burner 211, the slag materials which are not completely combusted in the secondary gasification are discharged through a slag outlet 151 and fall into the quenching water 22 to be cooled to form solid slag materials; when the amount of the solid slag reaches the discharge standard, the slag collecting assembly is connected with the solid slag outlet 24, the pressure is increased until the pressure condition in the slag collecting assembly and the pressure condition in the chilling unit 2 reach balance, namely 4Mpa, the solid slag outlet 24 is opened, the solid slag falls into the slag collecting assembly filled with cooling water based on the gravity effect, then the solid slag outlet 24 is closed, and S1 and S2 are continuously repeated.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, but any modifications or equivalent variations made according to the technical spirit of the present invention are within the scope of the present invention as claimed.

Claims (9)

1. A gasification reduction device for co-producing yellow phosphorus and synthesis gas is characterized by comprising a phosphorus coal gasification reduction unit and a chilling unit, wherein the phosphorus coal gasification reduction unit is communicated with the chilling unit from top to bottom;
the phosphorus coal gasification reduction unit: the gasification reduction reaction of all materials in the phosphorus coal gasification reduction unit is realized to obtain phosphorus-containing furnace gas;
the quench unit: used for cooling slag formed in the process of the coal gasification reduction reaction of the phosphorus to be solid and discharging the solid.
2. A gasification reduction apparatus according to claim 1, wherein the phosphorus coal gasification reduction unit comprises a feed inlet (12), a reaction chamber (11) and a slag bath (15) arranged in sequence from top to bottom;
the feeding hole (12) is positioned above the reaction chamber (11) and is used for providing solid materials for the phosphorus coal gasification reduction reaction;
an air inlet (13) is formed in the lateral lower part of the reaction chamber (11) and is used for providing gas materials for the coal gasification reduction reaction of the phosphorus;
an air outlet (14) is arranged above the side of the reaction chamber (11) and used for leading out the phosphorus-containing furnace gas;
the slag pool (15) is located right below the reaction chamber (11) and used for receiving slag formed in the phosphorus coal gasification reduction reaction and discharging the slag to the chilling unit located below the slag pool (15).
3. A gasification reduction apparatus according to claim 2, characterized in that at least one coal layer (111) and at least one phosphorus layer (112) are provided in the reaction chamber (11), the coal layer (111) and the phosphorus layer (112) are arranged in a spaced-apart manner, the coal layer (111) comprises raw coal and/or coke, the phosphorus layer (112) comprises phosphorus pellet, wherein the layer height ratio of the phosphorus layer (112) and the coal layer (111) is set as follows:
Figure FDA0002464801280000011
Figure FDA0002464801280000012
wherein: h1-the height of the phosphorus layer consumed per hour, in m;
H2-the height of the coal bed consumed per hour in m;
q is the heat required for producing the yellow phosphorus product of unit mass, and the unit is J/kg;
q is the heat released by the reaction of unit mass of the raw material coal and/or coke and oxygen, and the unit is J/kg;
m is the mass of the product yellow phosphorus, and the unit is kg;
a-carbon content in the feed coal and/or coke,%;
b-conversion of carbon in feed coal and/or coke,%;
rho-bulk density of the feed coal and/or coke in kg/m3；
d-diameter of the reaction unit in m.
4. A gasification reduction apparatus according to claim 2, characterized in that the phosphorus coal gasification reduction unit further comprises a feed conduit (16);
the feed conduit (16) is located directly below the feed inlet (12) for vertically introducing the solid material into the reaction chamber (11).
5. A gasification reduction apparatus according to claim 2, wherein the slag bath (15) is of an inverted cone-shaped configuration, the upper portion being adapted to receive slag from the reaction chamber (11), and the lower portion being provided with a slag outlet (151), the slag outlet (151) being in communication with the quench unit for discharging the slag charge.
6. A gasification reduction apparatus according to claim 5, wherein the quench unit is located below the P-coal gasification reduction unit and connected thereto by a flange, and the slag outlet (151) leads directly to the quench unit through the flange, discharging the slag to the quench unit.
7. The gasification reduction apparatus of claim 6, wherein the quench unit comprises, from top to bottom, a combustion chamber and a quench chamber;
the upper part of the combustion chamber is provided with an annular air passage (21), an annular burner (211) positioned on the annular air passage, an ignition gun (23), a flue gas cover (25) and a flue gas cooling coil (26);
the annular air channel (21) is used for introducing mixed gas of fuel and air into the annular burner (211);
the annular burner (211) is used for spraying the mixed gas to the slag outlet (151);
the ignition gun (23) is used for igniting the mixed gas sprayed out by the annular burner (211), and performing secondary gasification on slag at the slag outlet (151) in a combustion state, so that the slag outlet (151) is kept in an unblocked state all the time;
the flue gas cover (25) is used for forming a gasification space, and flue gas generated by secondary gasification is sealed in the flue gas cover (25) through the liquid seal effect of the lower chilling water (22);
and the flue gas cooling coil (26) is connected above the flue gas hood (25) and is used for discharging flue gas generated by secondary gasification out of the chilling unit.
8. A gasification reduction apparatus according to claim 7, characterized in that the chilling chamber is located below the combustion chamber and contains chilling water (22) inside, and the bottom of the chilling chamber is provided with a solid slag outlet (24) for cooling and discharging the slag which is not completely burned in the secondary gasification and cooling the flue gas in the flue gas cooling coil (26).
9. A method for co-producing yellow phosphorus and synthesis gas by using the gasification reduction plant according to any one of claims 1 to 8, wherein the method comprises a phosphorus coal gasification reduction process and a slag discharge process;
the phosphorus coal gasification reduction reaction process comprises the following steps:
a1: crushing and grinding the phosphate ore, anthracite and silica into powder, and mixing the powder with the phosphate ore: anthracite coal: the mass ratio of silica is (30-80): (10-30): (10-20) mixing the phosphorus pellets to prepare phosphorus pellet pellets, and feeding the prepared phosphorus pellet pellets and the raw material coal and/or coke into the reaction chamber (11) through the feeding hole (12) respectively, wherein the phosphorus pellet is placed on the phosphorus layer (112), and the raw material coal and/or coke is placed on the coal layer (111);
a2: introducing water vapor and high-purity oxygen into the reaction chamber (11) through the air inlet (13), wherein the coal bed (111) positioned at the lower part of the reaction chamber (11) is contacted with the oxygen at the bottom of the reaction chamber (11) and is combusted to generate high-temperature furnace gas to flow upwards;
a3: the furnace gas flows upwards to drive the heat of the whole interior of the reaction chamber (11) to flow and circulate, and simultaneously promote the materials in the reaction chamber (11) to be fully mixed and contacted, the pressure in the reaction chamber (11) is 1-10MPa, the temperature is 1200-1600 ℃, phosphate ore in the phosphorus pellet is reduced into elemental phosphorus, and the phosphorus-containing furnace gas generated in the reaction process is discharged from the gas outlet (14);
the slag discharging process comprises the following steps:
s1: when the phosphorus coal gasification reduction unit normally operates, the ignition gun (23) ignites mixed gas of fuel and air sprayed by the annular burner (211), when the phosphorus coal gasification reduction unit is in a combustion state, slag at the slag outlet (151) is secondarily gasified, flue gas generated by secondary gasification is sealed in a gasification space formed by the flue gas cover (25) and the quenching water (22) and is discharged out of the chilling unit through the flue gas cooling coil (26), and the difference P1-P2 that the pressure P1 in the flue gas cover (25) is greater than the pressure P2 in the slag pool (15) is kept to be 5-20Kpa by controlling the amount of the mixed gas introduced into the annular burner (211), wherein P1-P2 ═ PSlag chargeg(h0-h)，h0The height h of the slag pool is the height of the slag charge, so that the slag charge in the slag pool (15) is prevented from falling into the chilling unit;
s2: with the increase of slag materials borne in the slag pool (15), the pressure difference P1-P2 between the flue gas cover (25) and the slag pool (15) is gradually reduced, when the pressure difference is lower than 5Kpa, mixed gas is stopped to be introduced into the annular burner (211), the slag materials which are not completely combusted in the secondary gasification are discharged through the slag outlet (151), fall into the quenching water (22) to be cooled to form solid slag materials, and then are discharged through the solid slag material outlet (24), and after the slag discharging process is finished, the steps S1 and S2 are repeated.
CN202010330541.6A 2020-04-24 2020-04-24 Gasification reduction device and method for co-producing yellow phosphorus and synthesis gas Pending CN111394133A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112430478A (en) * 2020-11-03 2021-03-02 哈尔滨工业大学 U-shaped coal gasification waste heat boiler with spraying cooling device and cooling method
CN113336207A (en) * 2021-06-30 2021-09-03 昆明理工大学 Combined production system of yellow phosphorus and synthesis gas

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112430478A (en) * 2020-11-03 2021-03-02 哈尔滨工业大学 U-shaped coal gasification waste heat boiler with spraying cooling device and cooling method
CN112430478B (en) * 2020-11-03 2022-03-11 哈尔滨工业大学 U-shaped coal gasification waste heat boiler with spraying cooling device and cooling method
CN113336207A (en) * 2021-06-30 2021-09-03 昆明理工大学 Combined production system of yellow phosphorus and synthesis gas
EP4112538A1 (en) * 2021-06-30 2023-01-04 Kunming University Of Science And Technology System for combined production of yellow phosphorus and syngas

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