CN106315520A - Waste sulfuric acid cracking technology - Google Patents
Waste sulfuric acid cracking technology Download PDFInfo
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- CN106315520A CN106315520A CN201510346801.8A CN201510346801A CN106315520A CN 106315520 A CN106315520 A CN 106315520A CN 201510346801 A CN201510346801 A CN 201510346801A CN 106315520 A CN106315520 A CN 106315520A
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Abstract
The invention relates to an improved waste sulfuric acid cracking technology, which takes waste sulfuric acid, air and fuel for providing heat required by cracking as the raw materials, the waste sulfuric acid is subjected to a cracking reaction in a cracking furnace to generate the mixing furnace gas containing sulfur dioxide, sulfur trioxide, carbon dioxide, water vapour, nitrogen and flue dust, and the furnace gas is subjected to heat exchange and then is introduced into a subsequent acid making system to prepare the finished product sulfuric acid. The waste acid cracking technology has a complete automatic control system and a plurality of linkage means for guaranteeing safety operation, and all the instrument signal can be accessed to a DCS control system of an acid making apparatus. The waste sulfuric acid cracking technology has the advantages of large waste acid processing amount, environmental protection, high efficiency, safety and stabilization. The temperature in the cracking furnace is more than 600 DEG C, an equipped waste acid spray gun has excellent atomization effect, long stay time is kept for furnace gas, so that the cracking rate of the waste sulfuric acid is close to 100%.
Description
Technical field
The invention belongs to technical field of environmental protection in chemical industry, be specifically related to the cracking technology of a kind of Waste Sulfuric Acid.
Background technology
All kinds of relevant chemical plant installations of China, such as relating to esterification, sulfonation, alkylation, hydration hydrolysis, purify and the technique such as dehydration, annual the most all can a large amount of Waste Sulfuric Acid of by-product, especially the alkyl plant of numerous domestic refinery is during producing isobutyltrimethylmethane., often produces 1 ton of alkylate oil and will produce the Waste Sulfuric Acid of 80～100kg, and this Waste Sulfuric Acid viscosity is big, chromaticness is poor, difficult, in addition to the sulphuric acid containing 80～90%, also containing large amount of organic and water.The processing method of Waste Sulfuric Acid mainly has following several at present: 1. alkali neutralisation, allows sulphuric acid be neutralized reaction, extracting sulfuric acid ammonium, magnesium sulfate, calcium sulfate etc. with various inorganic bases.2. concentrate after imurity-removal, by adsorbing, filter, aoxidize, distilling, air stripping, the mode such as the extraction organic and inorganic impurity that removes in Waste Sulfuric Acid, then the dilute sulfuric acid after remove impurity is concentrated to give industrial concentrated sulphuric acid.3. support by the arm burning, be in the fluidized bed furnace or rotary kiln of sulfuric acid production plant, to spray into Waste Sulfuric Acid produce.All there is the problems such as technique is complicated, processing cost is high, product quality is uneven, process is the most thorough in these processing methods.Compared with above processing method, this Technology: list can process alkylation spent acid, other can also be utilized to contain the Waste Sulfuric Acid of organic impurities as raw material, its concentration of the sulfuric acid product produced can reach more than 98%, its product quality has reached national high-class product standard, can return alkyl plant and reuse；Apply this process to process Waste Sulfuric Acid thorough, do not produce secondary pollution；Spent acid treating capacity is big, and single set pyrolysis furnace can accomplish the treating capacity of 40,000 tons/year；Technological operation is simple, is all controlled by DCS；The required fuel of cracking is in addition to natural gas or liquefied petroleum gas, the by-products such as the sulfide hydrogen sour gas of Petrochemical Enterprises by-product, various organic exhaust gas and heavy oil can also be utilized, both alleviate the processing pressure of enterprise's organic liquid waste and waste gas, make use of again the heat that its burning produces；Plant construction cost is substantially reduced, far below external same device.There is good economic and social benefit.
Summary of the invention
The present invention be directed to above-mentioned present situation, and a kind of Waste Sulfuric Acid cracking technology proposed, the Waste Sulfuric Acid of suitable treatment various chemical plant installations by-product, it is particularly suited for a large amount of high concentrations, the Waste Sulfuric Acid of high content of organics that petroleum refinery alkylation device produces, by making Waste Sulfuric Acid cracking flue gas containing sulfur dioxide in pyrolysis furnace, subsequently into follow-up acid making system preparing finished articles sulphuric acid.
The cracking technology of the Waste Sulfuric Acid of the present invention, it is characterized in that cracking the fuel of institute's calorific requirement as raw material with Waste Sulfuric Acid, air, offer Waste Sulfuric Acid, make Waste Sulfuric Acid that cracking reaction to occur in pyrolysis furnace, generate containing sulfur dioxide, sulfur trioxide, carbon dioxide, water, nitrogen, the mixing furnace gas of flue dust, furnace gas enters follow-up acid making system preparing finished articles sulphuric acid after heat exchange, concrete technology is: fuel and air is sprayed in pyrolysis furnace by burner and burns, it is provided that the heat needed for cracking；After reaching the furnace temperature set, by spent acid spray gun, Waste Sulfuric Acid atomization being sprayed into pyrolysis furnace and carry out Pintsch process, the furnace gas containing finite concentration sulfur dioxide that Waste Sulfuric Acid produces after fully cracking enters follow-up acid making system after heat exchange；Described Waste Sulfuric Acid cracking technology includes complete automatic control system and the interlocking run that ensures safety, and all instrument signals all access the DCS control system of sulphuric acid plant.
Usually, one of primary raw material of described spent acid cracking technology is the Waste Sulfuric Acid containing multiple organic or inorganic impurity, and sulfuric acid content palpus >=30% in Waste Sulfuric Acid, preferred concentration is >=80%；Waste Sulfuric Acid needs the spent acid spray gun through burner to be atomized before entering pyrolysis furnace, and the method for atomization can be mechanical means or be completed by atomizing medium.Atomizing medium uses compressed gas, preferably compressed air；The Waste Sulfuric Acid of spent acid spray gun import and compressed-air actuated pressure palpus >=0.1MPa；Temperature when spent acid enters stove must be more than its freezing point, and preferred temperature is room temperature；The treating capacity of Waste Sulfuric Acid is determined by unit scale, and the spent acid treating capacity of single covering device can reach 625～18750kg/h.
One of primary raw material of described spent acid cracking technology is to provide Waste Sulfuric Acid and cracks the fuel of institute's calorific requirement.Fuel enters pyrolysis furnace by burner, and state when entering stove can be liquid or gaseous state, preferably gaseous state；The composition of fuel is the compound containing elements such as carbon, hydrogen, oxygen, sulfur, nitrogen, preferably has Hydrocarbon (including alkane, alkene, alkynes, aromatic hydrocarbons etc.), alcohol, ether, esters and hydrogen, hydrogen sulfide and the sulfur etc. of different carbon chain lengths；Gaseous state or liquid fuel enter pressure palpus >=0.1Mpa during stove；The consumption of fuel is determined by many factors such as the character of the burst size of Waste Sulfuric Acid, air capacity, furnace temperature and fuel and calorific values, is regulated by DCS control system.
One of primary raw material of described spent acid cracking technology is air.Combustion-supporting gas be sufficiently mixed with fuel in burner after enter pyrolysis furnace, the charging temperature of air be room temperature and more than；The consumption of air is regulated by DCS control system
In described technique, cracking temperature >=600 DEG C；Cracking pressure is normal pressure or tiny structure.
Described technique includes that perfect automatic control system DCS, cracking temperature realize self-regulated with the furnace entering volume of fuel, and when furnace temperature is less than design temperature, fuel input will increase；Furnace temperature will reduce higher than setting value fuel input；In the gas that cracking produces, oxygen content and the furnace entering volume self-regulated of air, will reduce when the oxygen concentration of pyrolysis furnace outlet furnace gas is higher than setting value then air addition；When the oxygen concentration of pyrolysis furnace outlet furnace gas will increase less than setting value then air addition；The operation pressure of spent acid cracking realizes self-regulated with the centrifugal blower of follow-up acid making system, operates pressure in ensureing pyrolysis furnace by Fan Regulation；Waste Sulfuric Acid furnace entering volume and air supply realize self-regulated, and when spent acid straying quatity is increased or decreased, compressed-air actuated amount is also scaling up or reduces.
Described technique includes perfect safety and protection system, and burner is chain with air blower, only blower fan normally start or blower fan power fault-free time, burner just can be started working；Burner is chain with spent sulfuric acid spray gun, and only when burner startup or fault-free, opening of spent sulfuric acid spray gun allows spent acid spray in stove；Burner in normal work is if there is accident extinguishing, and flame eye can't detect flame, burner and spent acid spray gun and also will turn off；When accident power-off occur in air blower, burner, fuel and Waste Sulfuric Acid will automatically cut off；System is furnished with excess temperature alarm device, if pyrolysis furnace temperature exceedes setting value, can send alarm signal to control room immediately.
The maximum feature of the present invention is that spent acid treating capacity is big, environmental protection, efficiently and safety and stability.Cracking in-furnace temperature is more than 600 DEG C, and the spent acid spray gun of outfit has the atomizing effect of excellence, and furnace gas also ensure that the sufficiently long time of staying so that Waste Sulfuric Acid cleavage rate is close to 100%.
Detailed description of the invention
Being described principle and the feature of the present invention below in conjunction with embodiment, example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Following example, respectively with Waste Sulfuric Acid, fuel and air etc. as raw material, spray into after first fuel and air being sufficiently mixed in the burner in stove and burn, and maintain furnace temperature more than 600 DEG C；By the regulation of centrifugal blower, operation pressure suitable in maintaining stove；Then use compressed air that Waste Sulfuric Acid carries out in spent acid spray gun atomization and form acid mist, be then sprayed in pyrolysis furnace carrying out Pintsch process；Ultimately generating the mixing furnace gas containing sulfur dioxide, sulfur trioxide, carbon dioxide, water, nitrogen, flue dust etc., furnace gas enters follow-up system after heat exchange and prepares finished product sulfuric acid.
The automatic control of embodiment spent acid cracking technology is achieved in that
1. igniting: after pressing the button ignition switch on burner, system proceeds by purging, then by electrion firing point firelock, detect that flame post fuel electromagnetic valve is opened, burner is ignited, and after flame eye detects burner flame, burner enters normal operating conditions；If flame eye is not detected by burner flame, within 7 seconds, post fuel electromagnetic valve will turn off, and after pressing the SR on burner, purging could be lighted a fire after three minutes again again；If furnace temperature reaches setting value after igniting, spent acid spray gun electromagnetic valve will be opened, and crack in the spent acid spray people's stove after atomization.
The most properly functioning: (1) furnace temperature and burner electromagnetic valve realize automatic control, furnace temperature will be opened greatly less than setting value burner electromagnetic valve；Furnace temperature will be opened little higher than setting value burner electromagnetic valve.(2) the oxygen table at furnace gas export realizes automatic control with the electromagnetic valve of air line, and the oxygen concentration of outlet furnace gas then turns down air line electromagnetic valve higher than setting value；The oxygen concentration of outlet furnace gas then drives big air line electromagnetic valve less than setting value.(3) furnace pressure realizes automatic control, by air-blower control furnace pressure with the sulphur dioxide blower of conversion section.(4) spent acid spray gun electromagnetic valve and compressed air blower fan electromagnetic valve realize automatic control, and when spent acid straying quatity increases or reduces, the air quantity of compression fan is also scaling up or reduces.
The most operating safety with protection system: (1) combustion controller is chain with aerator, after only blower fan normally starts or blower fan power fault-free time, burner just can be started working.(2) burner is chain with the electromagnetic valve of spent acid spray gun, and after only burner control starts or during fault-free, the electromagnetic valve of spent acid spray gun just can be opened and allow spent acid spray in stove.(3) the burner in normal work is if there is accident extinguishing, and flame eye can't detect flame, fuel solenoid valve and spent acid electromagnetic valve and also will turn off.(4), when accident power-off occur in aerator, burner control, automatically cut off fuel and spent acid electromagnetic valve.(5) it is furnished with excess temperature alarm device, if fire box temperature exceedes setting value, alarm signal can be sent to control room immediately.
Embodiment 1
With natural gas for the technique of fuel-pyrolysis Waste Sulfuric Acid, comprise the following steps:
Step one: after the natural gas after voltage stabilizing and the air being preheating to 300 DEG C are sufficiently mixed in burner, spray into after burning torch is lighted in stove, form fusiform flame region；
Step 2: treat that furnace temperature is raised to 800 DEG C and uses high-pressure pump conveying machinery to be atomized the mode combined with compressed air assisted atomization the Waste Sulfuric Acid that concentration is 50% so that the atomization of described Waste Sulfuric Acid sprays in pyrolysis furnace after forming acid mist.Waste Sulfuric Acid after atomization, under furnace high-temperature environment, is cracked to form the flue gas containing sulfur dioxide, sulfur trioxide, carbon dioxide, shredded tobacco for water pipes dirt etc., laggard such as follow-up acid making system through waste heat recovery.
Embodiment 2
With liquefied petroleum gas for the technique of fuel-pyrolysis Waste Sulfuric Acid, comprise the following steps:
Step one: after the liquefied petroleum gas after voltage stabilizing and the air being preheating to 400 DEG C are sufficiently mixed in burner, spray into after burning torch is lighted in stove, form fusiform flame region；
Step 2: treat that furnace temperature is raised to 1000 DEG C and uses high-pressure pump conveying machinery to be atomized the mode combined with compressed air assisted atomization the Waste Sulfuric Acid that concentration is 60% so that the atomization of described Waste Sulfuric Acid sprays in pyrolysis furnace after forming acid mist.Waste Sulfuric Acid after atomization, under furnace high-temperature environment, is cracked to form the flue gas containing sulfur dioxide, sulfur trioxide, carbon dioxide, shredded tobacco for water pipes dirt etc., laggard such as follow-up acid making system through waste heat recovery.
Embodiment 3
With hydrogen sulfide gas for the technique of fuel-pyrolysis Waste Sulfuric Acid, comprise the following steps:
Step one: after the hydrogen sulfide gas after voltage stabilizing and the air being preheating to 500 DEG C are sufficiently mixed in burner, spray into after burning torch is lighted in stove, form fusiform flame region；
Step 2: treat that furnace temperature is raised to 1100 DEG C and uses high-pressure pump conveying machinery to be atomized the mode combined with compressed air assisted atomization the Waste Sulfuric Acid that concentration is 70% so that the atomization of described Waste Sulfuric Acid sprays in pyrolysis furnace after forming acid mist.Waste Sulfuric Acid after atomization, under furnace high-temperature environment, is cracked to form the flue gas containing sulfur dioxide, sulfur trioxide, carbon dioxide, shredded tobacco for water pipes dirt etc., laggard such as follow-up acid making system through waste heat recovery.
Embodiment 4
With sulfur for the technique of fuel-pyrolysis Waste Sulfuric Acid, comprise the following steps:
Step one: after the sulfur after liquefaction or vaporization is sufficiently mixed with the air being preheating to 600 DEG C in burner, sprays into after burning torch is lighted in stove, form fusiform flame region；
Step 2: treat that furnace temperature is raised to 1200 DEG C and uses high-pressure pump conveying machinery to be atomized the mode combined with compressed air assisted atomization the Waste Sulfuric Acid that concentration is 80% so that the atomization of described Waste Sulfuric Acid sprays in pyrolysis furnace after forming acid mist.Waste Sulfuric Acid after atomization, under furnace high-temperature environment, is cracked to form the flue gas containing sulfur dioxide, sulfur trioxide, carbon dioxide, shredded tobacco for water pipes dirt etc., laggard such as follow-up acid making system through waste heat recovery.
Embodiment 5
With hydro carbons that carbon atoms is 5～8 for the technique of fuel-pyrolysis Waste Sulfuric Acid, comprise the following steps:
Step one: after hydro carbons and the air being preheating to 700 DEG C are sufficiently mixed in burner, spray into after burning torch is lighted in stove, form fusiform flame region；
Step 2: treat that furnace temperature is raised to 1400 DEG C and uses high-pressure pump conveying machinery to be atomized the mode combined with compressed air assisted atomization the Waste Sulfuric Acid that concentration is 90% so that the atomization of described Waste Sulfuric Acid sprays in pyrolysis furnace after forming acid mist.Waste Sulfuric Acid after atomization, under furnace high-temperature environment, is cracked to form the flue gas containing sulfur dioxide, sulfur trioxide, carbon dioxide, shredded tobacco for water pipes dirt etc., laggard such as follow-up acid making system through waste heat recovery.
Claims (7)
1. the cracking technology of a Waste Sulfuric Acid, it is characterized in that cracking the fuel of institute's calorific requirement as raw material with Waste Sulfuric Acid, air, offer Waste Sulfuric Acid, make Waste Sulfuric Acid that cracking reaction to occur in pyrolysis furnace, generate containing sulfur dioxide, sulfur trioxide, carbon dioxide, water, nitrogen, the mixing furnace gas of flue dust, furnace gas enters follow-up acid making system preparing finished articles sulphuric acid after heat exchange, concrete technology is: fuel and air is sprayed in pyrolysis furnace by burner and burns, it is provided that the heat needed for cracking；After reaching the furnace temperature set, by spent acid spray gun, Waste Sulfuric Acid atomization being sprayed into pyrolysis furnace and carry out Pintsch process, the furnace gas containing finite concentration sulfur dioxide that Waste Sulfuric Acid produces after fully cracking enters follow-up acid making system after heat exchange；Described Waste Sulfuric Acid cracking technology includes complete automatic control system and the interlocking run that ensures safety, and all instrument signals all access the DCS control system of sulphuric acid plant.
Technique the most according to claim 1, it is characterised in that one of described raw material is the Waste Sulfuric Acid containing multiple organic or inorganic impurity, sulfuric acid content >=30% in Waste Sulfuric Acid；Before Waste Sulfuric Acid entrance pyrolysis furnace, the spent acid spray gun through burner is atomized, and the method for atomization is mechanical means or is completed by atomizing medium, and atomizing medium uses compressed gas；The Waste Sulfuric Acid of spent acid spray gun import and compressed-air actuated pressure >=0.1MPa；Temperature when spent acid enters stove is more than its freezing point.
The most according to claim 1, technique, it is characterised in that one of described raw material is to provide Waste Sulfuric Acid and cracks the fuel of institute's calorific requirement, fuel enters pyrolysis furnace by burner, and state when entering stove is liquid or gaseous state；The composition of fuel is containing carbon, hydrogen, oxygen, sulfur, the compound of nitrogen element, including such as hydrogen, hydrogen sulfide, sulfur and hydro carbons, alcohol ethers, carboxylic acids, esters and high molecular weight compounds etc.；Gaseous state or liquid fuel enter pressure >=0.1Mpa during stove；The consumption of fuel is determined by character and the calorific value many factors of the burst size of Waste Sulfuric Acid, air capacity, furnace temperature and fuel, is regulated by DCS control system.
Technique the most according to claim 1, it is characterised in that one of described raw material is air, combustion-supporting gas be sufficiently mixed with fuel in burner after enter pyrolysis furnace, the charging temperature of air be room temperature and more than；The consumption of air is regulated by DCS control system.
Technique the most according to claim 1, it is characterised in that cracking temperature >=600 DEG C；Cracking pressure is normal pressure or tiny structure.
The most according to claim 1, technique, it is characterised in that include that perfect automatic control system DCS, cracking temperature realize self-regulated with the furnace entering volume of fuel, when furnace temperature is less than design temperature, fuel input will increase；Furnace temperature will reduce higher than setting value fuel input；In the gas that cracking produces, oxygen content and the furnace entering volume self-regulated of air, will reduce when the oxygen concentration of pyrolysis furnace outlet furnace gas is higher than setting value then air addition；When the oxygen concentration of pyrolysis furnace outlet furnace gas will increase less than setting value then air addition；The operation pressure of spent acid cracking realizes self-regulated with the centrifugal blower of follow-up acid making system, operates pressure in ensureing pyrolysis furnace by Fan Regulation；Waste Sulfuric Acid furnace entering volume and air supply realize self-regulated, and when spent acid straying quatity is increased or decreased, compressed-air actuated amount is also scaling up or reduces.
During fault-free that technique the most according to claim 1, it is characterised in that including perfect safety and protection system, burner is chain with air blower, only blower fan normally start or blower fan is powered, burner just can be started working；Burner is chain with spent sulfuric acid spray gun, and only when burner startup or fault-free, opening of spent sulfuric acid spray gun allows spent acid spray in stove；Burner in normal work is if there is accident extinguishing, and flame eye can't detect flame, burner and spent acid spray gun and also will turn off；When accident power-off occur in air blower, burner, fuel and Waste Sulfuric Acid will automatically cut off；System is furnished with excess temperature alarm device, if pyrolysis furnace temperature exceedes setting value, can send alarm signal to control room immediately.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946685A (en) * | 2018-08-22 | 2018-12-07 | 戴国梁 | A kind of sulfuric acid preparation facilities preparing regenerated liquid using Waste Sulfuric Acid |
| CN109052335A (en) * | 2018-07-24 | 2018-12-21 | 上海三夫工程技术有限公司 | A kind of method of sulfur gas reduction Waste Sulfuric Acid sulfur dioxide liquid and sulfuric acid |
| CN110155956A (en) * | 2019-04-18 | 2019-08-23 | 南京汇仁化工设备有限公司 | Fluoride Waste acid treating device and its processing method |
| CN111099564A (en) * | 2018-10-29 | 2020-05-05 | 中国石油化工股份有限公司 | Method for recovering waste sulfuric acid by using high-sulfur coal as fuel |
| CN112815353A (en) * | 2021-01-12 | 2021-05-18 | 桂林理工大学 | Industrial furnace combustion air supply system and control method thereof |
| CN113237065A (en) * | 2021-01-13 | 2021-08-10 | 姚燕 | Intelligent control waste acid cracking furnace and waste sulfuric acid cracking process |
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| CN102050430A (en) * | 2009-11-09 | 2011-05-11 | 中国石油化工股份有限公司 | Method for preparing high concentration sulfuric acid by cracking low concentration sulfuric acid |
| CN102951616A (en) * | 2012-11-21 | 2013-03-06 | 中国寰球工程公司辽宁分公司 | Cracking furnace for waste acid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052335A (en) * | 2018-07-24 | 2018-12-21 | 上海三夫工程技术有限公司 | A kind of method of sulfur gas reduction Waste Sulfuric Acid sulfur dioxide liquid and sulfuric acid |
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| CN108946685A (en) * | 2018-08-22 | 2018-12-07 | 戴国梁 | A kind of sulfuric acid preparation facilities preparing regenerated liquid using Waste Sulfuric Acid |
| CN111099564A (en) * | 2018-10-29 | 2020-05-05 | 中国石油化工股份有限公司 | Method for recovering waste sulfuric acid by using high-sulfur coal as fuel |
| CN110155956A (en) * | 2019-04-18 | 2019-08-23 | 南京汇仁化工设备有限公司 | Fluoride Waste acid treating device and its processing method |
| CN112815353A (en) * | 2021-01-12 | 2021-05-18 | 桂林理工大学 | Industrial furnace combustion air supply system and control method thereof |
| CN113237065A (en) * | 2021-01-13 | 2021-08-10 | 姚燕 | Intelligent control waste acid cracking furnace and waste sulfuric acid cracking process |
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