CN109336066B - Process and system for jointly preparing acid by recycling sulfur and waste gas from viscose waste gas TRS - Google Patents
Process and system for jointly preparing acid by recycling sulfur and waste gas from viscose waste gas TRS Download PDFInfo
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- CN109336066B CN109336066B CN201811433117.3A CN201811433117A CN109336066B CN 109336066 B CN109336066 B CN 109336066B CN 201811433117 A CN201811433117 A CN 201811433117A CN 109336066 B CN109336066 B CN 109336066B
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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
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
- C01B17/765—Multi-stage SO3-conversion
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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
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
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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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Abstract
The invention relates to a process for jointly producing acid by recovering sulfur from viscose waste gas TRS and waste gas, which overcomes the defects that the stable operation of a system is influenced and the cost is overhigh due to the defects of raw material posts of the conventional waste gas acid production system, effectively utilizes sulfur generated by the viscose waste gas TRS recovery technology, solves the problem that the TRS cannot be treated by the conventional technology due to more complex iron impurities, and realizes the development of the circular economy technology of a company.
Description
Technical Field
The invention relates to the field of sulfuric acid manufacture, in particular to a process and a system for jointly preparing acid by recovering sulfur from viscose waste gas TRS and waste gas.
Background
At the present stage, the mainstream sulfuric acid production process in international society includes the production of acid by sulfur, the production of acid by waste gas (hydrogen sulfide), the production of acid by pyrite, the production of sulfuric acid by smelting flue gas, the production of sulfuric acid by gypsum and phosphogypsum, and the like.
The acid making system by using waste gas produced in production is built in 2014 of my company, belongs to an environmental protection project, and mainly adopts viscose waste gas (H) in the current system2S) carrying out incineration to produce sulfuric acid, wherein the actual load of a system only accounts for 50% of the design load.
2016, develops a TRS recycling project on viscose waste gas, and utilizes a complexing iron auxiliary agent to recycle the viscose waste gas H2S is oxidized to generate elemental sulfur. At the present stage, TRS sulfur (elemental sulfur) cannot be combusted by a sulfur acid-making system due to the fact that the content of the complex iron additive is up to 40%. Can use a newly designed TRS sulfur melting tank to melt TRS sulfur, and burn the TRS sulfur after primary impurity removal, wherein the burning S02Flue gas and H2Mixing S waste gas, feeding the mixed S waste gas into a waste gas incinerator for secondary combustion, and adjusting SO2The concentration is washed and cooled for 3 times by a purification system to form pure S02And finally, converting and absorbing the flue gas to produce qualified sulfuric acid.
Chinese patent publication No.: "CN 104401947A" discloses a method for preparing acid by combining sulfur and waste gas, which comprises the following steps: the method mainly solves the problems that when the acid making method in the prior art is used alone, the utilization rate of equipment is low, the system load is insufficient due to insufficient waste gas, an electric furnace needs to be started for adding, heat is compensated, and the power consumption cost is increased.
However, the patent still has defects in the practical use process: (1) the concentration of the used sulfur reaches 99 percent, but the concentration of the sulfur produced by industrial waste gas is only 79 percent, and the impurity content is too large, so that the sulfur cannot be directly melted, filtered and put into use; (2) the sulfur produced by the industrial waste gas cannot be used due to excessive impurity content, only high-purity sulfur can be purchased, and the production structure is single, so that the production cost is increased; (3) when the waste gas acid-making system is driven in a cold state, water and SO generated by combustion of hydrogen sulfide due to too low temperature of a hearth2And a small amount of SO3Can generate condensed acid to cause corrosion of system equipment and reduce the service life of the system equipment. Therefore, liquefied gas is needed to be used for baking the hearth to above 400 ℃ during driving, normal production can be put into operation, and the time for putting the system into normal operation is prolonged.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a process and a system for preparing acid by combining recovered sulfur from viscose waste gas TRS and waste gas. The invention makes up the defects of instability and overhigh cost of the existing waste gas acid making system, effectively utilizes the sulfur generated by the viscose waste gas TRS recovery technology, solves the problem that the TRS sulfur contains more complex iron impurities and cannot be treated by the conventional technology, and realizes the development of the circular economy technology of the company.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a process for preparing acid by recovering sulfur and waste gas from viscose waste gas TRS is characterized by comprising the following steps:
(1) in a TRS reactor, carrying out oxidation reaction on waste gas generated in the viscose production process and a complex iron auxiliary agent, standing, separating supernatant, and allowing bottom sediment to enter a primary separation tank;
(2) standing in a primary separation tank, sending supernatant into a reactor, and allowing bottom precipitate to enter a primary centrifuge for primary dehydration separation;
(3) the precipitate after primary dehydration separation enters a primary washing tank, clear water is added, and the primary washing is completed after stirring;
(4) the sediment after the primary washing enters a secondary separation tank, standing is carried out, the supernatant is sent to a primary separation tank, and the sediment at the bottom enters a secondary centrifuge for secondary dehydration and separation;
(5) the precipitate after the secondary dehydration separation enters a secondary washing tank, clear water is added, and the secondary washing is completed after stirring;
(6) the sediment after the secondary washing enters a third-stage separation tank, standing is carried out, the supernatant is sent to a second-stage separation tank, and the sediment at the bottom enters a third-stage centrifugal machine for carrying out third dehydration separation;
(7) the precipitate after the third dewatering separation enters a third washing tank, clear water is added, and the three times of washing are completed after stirring;
(8) the precipitate after the third washing enters a filter press to obtain TRS sulfur;
(9) introducing TRS sulfur into a sulfur melting tank, heating, stirring and melting, wherein the complex iron additive is denatured and is increased from 2-valent iron to 3-valent iron;
(10) delivering the liquid sulfur at the lower layer of the sulfur melting tank to a sulfur incinerator for incineration to obtain SO2A gas;
(11) SO is added2The gas is sent to an incinerator for incineration, and simultaneously, waste gas, the waste gas and the combusted SO are introduced into the incinerator2Fully mixing the gas, and adjusting the SO after combustion2The concentration of the gas is 6%;
(12) SO in step (11)2Cooling the gas to 260 ℃ through a waste heat boiler;
(13) SO in the step (12)2Gas is sprayed and washed by a washing barrel, secondarily cooled and washed by a venturi type washing barrel and thirdly cooled and washed by a packed tower in sequence;
(14) finally, the acid mist is removed by an electric demister, and the dried product enters a converter after being dried by a drying tower to produce pure S03；
(15) And finally, producing sulfuric acid through an absorption tower.
Further, the heating temperature in the step (9) is up to 135-145 ℃.
Further, in the step (9), the density of the complex iron additive after denaturation is smaller than that of liquid sulfur, impurities of the complex iron additive float on the surface, and a layer of stainless steel wire mesh is horizontally arranged above the sulfur melting tank to capture the complex iron additive.
Further, the SO after the combustion in the step (10)2The temperature of the gas is 950-1050 ℃, SO2The concentration of the gas was 10%.
Further, the waste gas in the step (11) is H2S。
The utility model provides a system for sour is united with waste gas to viscose waste gas TRS recovery sulphur which characterized in that: comprises a sulfur melting tank, a sulfur burner, a boiler, a spraying device, a washing barrel, a Venturi barrel, a packed tower, an electric demister, a drying tower, a converter and an absorption tower which are connected in sequence.
And a layer of stainless steel wire mesh is horizontally arranged above the sulfur melting tank.
The invention has the advantages that:
the invention overcomes the defects of instability and overhigh cost of the existing waste gas acid making system, effectively utilizes the sulfur generated by the viscose waste gas TRS recovery technology, solves the problem that the TRS sulfur contains more complex iron impurities and cannot be treated by the conventional technology, and realizes the development of the circular economy technology of the company.
And secondly, the residual complex iron auxiliary agent in the TRS sulfur is purified by 3 times of water washing, so that continuous normal production can be realized.
A layer of stainless steel wire mesh is horizontally arranged above a sulfur melting tank, and in the melting process of TRS sulfur, complex iron is heated at high temperature to form iron-containing impurities, the density of the complex iron is lower than that of liquid sulfur, an impurity layer is formed on the liquid sulfur, and after the iron-containing impurities are trapped by the stainless steel wire mesh, the iron-containing impurities are precooled in air to form solid impurities, and the impurities can be removed by replacing the wire mesh.
Fourthly, the waste gas incinerator for producing acid by waste gas adopts the incinerator rich in H2S waste gas is combusted, and in the normal production process, H is generated2S combustion can generate water and SO2And a small amount of SO3When the temperature of the hearth is lower, strong corrosive condensed acid can be formed, so that the corrosion of a flue and a boiler is caused, and the service life is influenced. Therefore, when the system is started each time, liquefied gas is needed to heat the hearth, and waste gas can be put into the furnace to produce when the temperature is above 400 ℃. SO after combustion2The temperature of the gas is 950-1050 ℃, and the normal operation time of the system is prolonged. Melting waste gas sulfur, collecting impurities through a stainless steel wire net, burning the waste gas in a sulfur burning furnace, delivering the burned flue gas with the temperature of 950-1050 ℃ to a waste gas acid-making waste gas burning furnace, continuously heating a hearth through the flue gas, and carrying out H treatment on the flue gas2After S stops burning, the waste gas incinerator can still be continuously ensured to keep normal process temperature, the generation of condensed acid is prevented, meanwhile, the furnace baking time is reduced for the next waste gas input burning, and the waste gas incinerator can be put into normal production more quickly.
Fifthly, adding SO2The gas is sent to an incinerator for incineration, and simultaneously, waste gas, the waste gas and the combusted SO are introduced into the incinerator2Fully mixing the gas, and adjusting SO after combustion2The concentration of the gas was 6%. Due to H2S then proceeds in a two-step reaction, H in the case of oxygen deficiency2After S is combusted, H2O and elemental S are generated, and H is sufficient in oxygen2S combustion for producing H2O and SO2. According to the catalyst configuration in the converter, to ensure the reaction heat balance in the converter, pair S02There are related requirements for concentration. Too low a gas concentration may result in insufficient conversion heat, failure to achieve system heat balance, need to supplement external heat source, and increase system cost. Increasing SO if required2Too high a gas concentration requires a reduction in furnace air to produce H2S can not be fully combusted to produce sublimed sulfur, and the sublimed sulfur can be sublimed into elemental sulfur due to rapid temperature reduction during rear-end purification and washing, so that system blockage is caused. Therefore S02The gas concentration is controlled at 6Percent, can ensure the normal operation of the conversion system and also ensure H2And S is fully combusted.
Sixth, H2S and S02After the waste gas is burnt, the total temperature of an outlet is controlled to be 950-1050 ℃, the waste heat boiler exchanges heat with desalted water in a furnace tube to produce 3.6Mpa medium-pressure steam, and the medium-pressure steam is finally produced into 0.5Mpa low-pressure saturated steam through a pressure reduction system, so that the waste heat recovery and utilization are realized, and the benefit is generated. The temperature of the flue gas cooled by the boiler is 260 ℃, and the liquid medium in the purification post is dilute sulfurous acid, so that the corrosion to metal materials is serious, and all standing equipment and pipelines of the purification post are made of glass fiber reinforced plastics and cannot bear overhigh temperature. Cooling to 60 deg.C by water spray of washing barrel, spraying with venturi spray and packed tower, removing acid mist by electric demister, and making into subsequent system for producing H2SO4. Controlling the outlet S0 of the waste heat boiler2The gas temperature is 260 ℃, heat can be effectively recovered to produce steam, and meanwhile, the gas temperature at a purification post can not damage equipment.
And seventhly, the invention produces acid by using sulfur produced by waste gas in the viscose production process, thereby not only reducing the production cost, but also reducing the emission of the waste gas, and being scientific and environment-friendly.
Compared with the prior art, the invention has the advantages that: (1) the prior art is used for TRS sulfur containing high impurity content waste gas, and the TRS sulfur is trapped on a sulfur melting post through a trapping net, so that a large amount of impurities are removed, the generation of ash in a waste gas acid making system is reduced, and the TRS sulfur is more beneficial to production; (2) the original patent can only be used for preparing acid by combining high-purity sulfur and waste gas, and the existing process is suitable for preparing acid by combining waste gas TRS sulfur and high-purity sulfur and has comprehensiveness; (3) the original patent access point directly accesses the flue gas with the temperature of 360 ℃ into a purification post and reduces the temperature by purification, washing and cooling, while the prior art directly accesses the flue gas with the temperature of 950 ℃ to 1050 ℃ and H2The flue gas formed after the S mixed combustion needs to be cooled to 260 ℃ through a waste heat boiler, so that the heat of the flue gas at 100 ℃ can be recovered more, the operation load of a purification post is reduced, and steam can be produced more by pairs, thereby generating benefits.
Drawings
FIG. 1 is a system diagram of the present invention;
the reference numbers in the figures are: 1. a sulfur melting tank, 2, a sulfur burning furnace, 3, an incinerator, 4, a boiler, 5, a spraying device, 6, a washing barrel, 7, a Venturi barrel, 8, a packed tower, 9, an electric demister, 10, a drying tower, 11, a converter, 12, an absorption tower, 13 and a stainless steel wire net.
Detailed Description
And (3) introducing the viscose waste gas into a TRS reactor to generate slurry rich in the complex iron auxiliary agent and sulfur, entering a primary separation tank through a lower discharge port, and realizing separation of the slurry and the supernatant by a standing separation mode. And (3) conveying the bottom sauce to a primary centrifuge for dehydration and separation through a slurry pump, and recovering the clear liquid above the primary separation tank to the TRS reactor through a pump.
After the primary centrifuge is dehydrated, TRS sulfur enters a primary washing tank, clear water is added, and primary washing is realized under the combined action of stirring. And (4) the mixed slurry enters a secondary separation tank, and the slurry is separated from the supernatant in a standing separation mode. And the bottom sauce is conveyed to a secondary centrifuge by a sauce pump for dehydration and separation. And the clear liquid above the secondary separation tank is recycled to the primary separation tank through a pump.
And (3) after the secondary centrifuge is dehydrated, allowing the TRS sulfur to enter a secondary washing tank, adding clear water, and under the combined action of stirring, realizing secondary washing. And (4) the mixed slurry enters a third-stage separation tank, and the slurry is separated from the supernatant in a standing separation mode. And (4) conveying the bottom sauce to a three-time centrifuge through a sauce pump for dehydration and separation. And the clear liquid above the third-stage separation tank is recycled to the second-stage separation tank through a pump.
Introducing TRS sulfur into a sulfur melting tank 1, melting under the combined action of steam and stirring, controlling the process temperature at 135-145 ℃, wherein the contained complexing iron auxiliary agent is denatured under the action of high temperature, and the temperature is increased from 2-valent iron to 3-valent iron.
Because the density of the complex iron additive is less than that of liquid sulfur after the complex iron additive is denatured, impurities of the complex iron additive float on the surface, and a layer of stainless steel wire mesh 13 is horizontally arranged above the novel sulfur melting tank 1 and used for trapping the complex iron additive.
The clean liquid sulfur at the lower layer is sent to a sulfur incinerator 2 by a pump for incinerationThe superheated flue gas after burning is about 950 ℃ to 1050 ℃ and SO2The concentration is 10 percent, the mixture is sent to a waste gas incinerator 3 for acid preparation by waste gas, and simultaneously enters the waste gas incinerator 3 for full mixing, and SO after combustion is adjusted2Gas concentration of 6%, mixed SO2The temperature of the gas is reduced to 260 ℃ through the waste heat boiler 4, and the waste heat boiler 4 produces steam as a byproduct.
The temperature of the SO is reduced to 260 ℃ by the waste heat boiler 42Spraying and washing the gas by a washing barrel 6, cooling and washing for the second time by a venturi type washing barrel 6, cooling and washing for the third time by a packed tower 8, removing acid mist by an electric demister 9, drying by a drying tower 10, and then converting to produce pure S03And finally sulfuric acid is produced through the absorption tower 12. And the residual complex iron auxiliary agent in the TRS sulfur is purified by 3 times of water washing, so that continuous normal production can be realized.
Claims (4)
1. A process for preparing acid by recovering sulfur and waste gas from viscose waste gas TRS is characterized by comprising the following steps:
(1) in the reactor, carrying out oxidation reaction on waste gas generated in the viscose production process and the complex iron auxiliary agent, standing, separating supernatant, and allowing bottom sediment to enter a primary separation tank;
(2) standing in a primary separation tank, sending supernatant into a reactor, and allowing bottom precipitate to enter a primary centrifuge for primary dehydration separation;
(3) the precipitate after primary dehydration separation enters a primary washing tank, clear water is added, and the primary washing is completed after stirring;
(4) the sediment after the primary washing enters a secondary separation tank, standing is carried out, the supernatant is sent to a primary separation tank, and the sediment at the bottom enters a secondary centrifuge for secondary dehydration and separation;
(5) the precipitate after the secondary dehydration separation enters a secondary washing tank, clear water is added, and the secondary washing is completed after stirring;
(6) the sediment after the secondary washing enters a third-stage separation tank, standing is carried out, the supernatant is sent to a second-stage separation tank, and the sediment at the bottom enters a third-stage centrifugal machine for carrying out third dehydration separation;
(7) the precipitate after the third dehydration separation enters a third washing tank, and clear water is added and stirred to finish the third washing;
(8) the precipitate after the third washing enters a filter press to obtain TRS sulfur;
(9) introducing TRS sulfur into a sulfur melting tank (1), heating, stirring and melting, wherein the complex iron additive is denatured and is increased from 2-valent iron to 3-valent iron;
(10) delivering the liquid sulfur at the lower layer of the sulfur melting tank (1) to a sulfur incinerator (2) for incineration to obtain SO2A gas;
(11) adding SO2The gas is sent to an incinerator (3) for incineration, and simultaneously, waste gas, the waste gas and the combusted SO are introduced into the incinerator (3)2Fully mixing the gas, and adjusting SO after combustion2The concentration of the gas is 6%;
(12) SO in step (11)2The gas is cooled to 260 ℃ through a waste heat boiler (4);
(13) SO in the step (12)2Gas is sprayed and washed by a washing barrel (6), cooled and washed for the second time by a Venturi washing barrel (6) and cooled and washed for the third time by a packed tower (8) in sequence;
(14) finally, acid mist is removed through an electric demister (9), and the dried SO enters a converter (11) after being dried by a drying tower (10) to produce pure SO3 ；
(15) Finally, sulfuric acid is produced through an absorption tower (12);
in the step (9), the density of the complex iron additive is lower than that of liquid sulfur after the complex iron additive is denatured, impurities of the complex iron additive float on the surface, and a layer of stainless steel wire mesh (13) is horizontally arranged above the sulfur melting tank (1) and used for trapping the complex iron additive; SO combusted in the step (10)2The temperature of the gas is 950-1050 ℃, SO2The concentration of the gas is 10%; the waste gas in the step (11) is H2S。
2. The process of claim 1, wherein the recovery of sulfur from the viscose waste gas TRS and the combined production of acid from the waste gas comprise: the heating temperature in the step (9) is 135-145 ℃.
3. The system for the combined acid making process of recovering sulfur and waste gas by the viscose waste gas TRS as claimed in claim 1, wherein: comprises a sulfur melting tank (1), a sulfur incinerator (2), a boiler (4), a spraying device (5), a washing barrel (6), a Venturi barrel (7), a packed tower (8), an electric demister (9), a drying tower (10), a converter (11) and an absorption tower (12) which are connected in sequence.
4. The system for the combined acid making process by recovering sulfur and waste gas from the viscose waste gas TRS as claimed in claim 3, wherein the system comprises: a layer of stainless steel wire mesh (13) is horizontally arranged above the sulfur melting tank (1).
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