CN104524714A - Gas phase passivation and desensitization method for easy self-ignition and self-heating material in production equipment - Google Patents
Gas phase passivation and desensitization method for easy self-ignition and self-heating material in production equipment Download PDFInfo
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Abstract
The invention relates to a gas phase passivation and desensitization method for an easy self-ignition and self-heating material in production equipment. The gas phase passivation and desensitization method includes the concrete steps that nitrogen generated by an air separator or nitrogen in a nitrogen steel bottle is used for being mixed with air to form mixed gas with the oxygen volume concentration of 0.5-5%; the mixed gas is injected into the equipment to be treated through a gas inlet to carry out gas phase passivation and desensitization and then escapes out of a gas outlet of the equipment; the oxygen content of the escaping gas is determined through a detection device, and when the oxygen content of the escaping gas is close to the oxygen content of the input gas, treatment is completed. Compared with the prior art, the gas phase passivation and desensitization method has the advantages that in the process of treating the production equipment containing the small amount of easy self-ignition and self-heating material, large-scale modification works for original production equipment are not needed, only part of gas mixing, analyzing and conveying devices need to be additionally arranged and used, investment is small, and operation is convenient; cleaning solvent is not involved in the treating process, and it is avoided that waste gas, waste water and other hazardous substances are generated to pollute the environment.
Description
Technical field
The invention belongs to inflammable easy hot material post-processing technology field, specifically, relate to easy spontaneous combustion in a kind of production equipment and cause the blunt quick method that disappears from the gas phase of hot material.
Background technology
In process of production, because of some material, there is easy spontaneous combustion or from heat sensitivity, if contact with air, with oxygen generation redox reaction wherein, a large amount of heats can be produced, finally causing system temperature to raise and the accident such as initiation fire, blast.Such as, when we directly open include strong reducing property ultra-fine powder materials or other water-tight equipments of meeting oxygen easy self-heating spontaneous combustible substances overhaul time, the air of access arrangement probably has the oxidation reaction of remarkable Fast exothermic effect with the easy self-heating spontaneous combustible substance remaining in device interior or be attached to equipment inner wall, brings out fire even explosion accident.The safe practice of these materials in production, storage, use procedure has report more.
The safeguard technology related in maintenance or waste treatment process is the key link in safety in production.Such as, the production process of super-fine metal powder powder material is normally carried out in the airtight process units completely cut off with oxygen, under the normal working condition completely cut off with oxygen, super-fine metal powder powder material is stability and safety, when equipment needs maintenance, having a small amount of super-fine metal powder powder material unavoidably remains in the equipment of Awaiting Overhaul, overhaul if now directly opened, being there is violent exothermic reaction by the oxygen in the air of access arrangement inside in the super-fine metal powder powder material residual with those, and then may bring out fire, explosion accident.Again such as, often FeS is had at the oil pipeline inwall of the oil storage tank inner-wall and conveying sour crude that store sour crude
xdeposit generates, FeS
xit is the easy self-heating spontaneous combustible substance typically with very high chemical reactivity, more stable when completely cutting off with oxygen, but when the Kaifeng maintenance that stops production contacts with the oxygen in air, easy generation Quick Oxidation reaction self-heating spontaneous combustion initiation fire, occurred both at home and abroad a lot of because of petrochemical equipment sulfur corrosion produce the spontaneous combustion of sulphur iron compound caused by major industrial accident.So, for including the airtight process units of easy self-heating spontaneous combustible substance, corresponding safe handling measure must be taked before overhaul of the equipments Kaifeng.
At present, the primary safety measures taked for the airtight production equipment including the stopping production Awaiting Overhaul of easy self-heating spontaneous combustible substance is before the maintenance of water-tight equipment Kaifeng, first adopt liquid phase cleaning agent to carry out cleaning or foam cleaning.Such as Japan and Korean Patent (as: Unexamined Patent 8-9257, KR20010092131) all adopt liquid phase cleaning agent to clean the storage technology and equipment that internal corrosion product eliminates safe hidden trouble.Because the general volume of above-mentioned production equipment is comparatively large, liquid phase cleaning process needs to use a large amount of cleaning agents, and needs emptying Residual oil before cleaning, and cleaning cost is high, workload large, and has a large amount of cleaning waste liquid to produce, and brings environmental pollution pressure.Particularly, entering of air is caused if dealt with improperly in cleaning process, fire, explosion accident.In addition, adopting during acidic cleaning solution cleaning also easily brings equipment corrosion and harmful acid mist to generate.Patent WO2014108137 discloses or oil plant import department inner at oil tank and sets up device for isolated air, and this device can protect the security of oil tank under deficient oil condition, but can not eliminate its potential safety hazard.For the production equipment including easy spontaneous combustion active matter that non-maintenance temporarily stops production, also there is the safety measure adopting the spontaneous combustion of filling inertia non-combustible gas prevention device, but can not eliminate or the dangerous substance of easy self-heating spontaneous combustion that deactivation has wherein existed.
Summary of the invention
For solving the problems of the technologies described above, the invention provides easy spontaneous combustion in a kind of easy, safe production equipment and causing the blunt quick method that disappears from the gas phase of hot material.
In a kind of production equipment of the present invention, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, described method concrete steps mix with air for the nitrogen in: the nitrogen 1) utilizing deaerator to produce or nitrogen cylinder, and forming carrier of oxygen volume concentrations is the mist of 0.5%-5%; 2) mist is passed into pending equipment from air inlet, carry out gas phase and cause and bluntly disappear quick, then overflow from the gas outlet of equipment; 3) with the oxygen content of detection means measure emergent gas, when its with oxygen content in input gas close to time, process completes.
In a kind of production equipment of the present invention, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and the degree of accuracy of described carrier of oxygen volume concentrations is within ± 0.05%.
In a kind of production equipment of the present invention, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, described gas outlet and air inlet are when same position, adopt different conduit respectively as air inlet and gas outlet, wherein the length of air induction conduit is greater than the length of outtake tube.
In a kind of production equipment of the present invention, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and it is 10-60min that described gas phase causes the blunt quick time that disappears.
In a kind of production equipment of the present invention, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and the maximum of described carrier of oxygen volume concentrations is C × (t
1-t
0)/Q; Described C is the thermal capacitance of all substances in reaction system, and Q is the mist of unit volume oxygen content and the redox reaction heat of pending material, t
0for reaction temperature during desensitization deactivation, t
1for the burning-point of material and oil gas.
In a kind of production equipment of the present invention, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and described checkout gear is tunable diode laser oxygen measurement system.
In a kind of production equipment of the present invention, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and the humidity of described mist is 70-90%.
In a kind of production equipment of the present invention, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and described mist contains nitrogen oxide as catalyst.
The invention provides a kind of can the degree of depth reduce gas molecule effective collision reaction probabilities, extremely promote equivalent reaction thermal capacitance, regulation and control can be designed, abundant eliminative reaction fuel factor effect, essential safety gas phase cause the blunt quick technical method that disappears.Specifically, by controlling the concentration of oxygen, the kind of catalyst and quantity in gas phase blending ingredients, the oxygen-sensitive material in production equipment is made to realize controllable oxidization under comparatively low oxygen concentration, the oxide-film that oxidation product is formed at these material surfaces, the reactivity of sensitive material and air can be reduced further, avoid them because Quick Oxidation causes temperature to raise rapidly, dieseling to occur.Wherein, the essential safety condition needed for eliminative reaction sensitiveness can be carried out calculating by all substances raised temperature institute calorific requirement in the thermal discharge of the oxidation heat liberation process of material and participation course of reaction and be obtained.By controlling oxygen concentration, the temperature that the heat produced in oxidizing process is caused raises the burning-point being no more than this material, reaches the target of essential safety.
Compared with prior art, in production equipment of the present invention, easy spontaneous combustion causes the blunt advantage disappearing quick method from the gas phase of hot material and is: to containing a small amount of easily spontaneous combustion, in the production equipment processing procedure of hot material, do not need to carry out fairly large improvement project to original production equipment, only need use and increase portion gas mixing, analysis and conveying device, invest little, easy to operate; In processing procedure, do not relate to cleaning solvent, the harmful substance such as waste gas, waste liquid contaminated environment can not be produced.After desensitization process, in equipment, the limited oxygen index of material is greater than 21%, is safe disposal result.
Accompanying drawing explanation
Fig. 1: the differential thermal analysis collection of illustrative plates of embodiment 1 sample after gaseous passivation process; Fig. 2: the differential thermal analysis collection of illustrative plates of embodiment 2 sample after gaseous passivation process; Fig. 3: petroleum storage container sulfur corrosion product gas phase passivation simulation test device figure.
Detailed description of the invention
Cause blunt disappear quick method to spontaneous combustion easy in production equipment of the present invention from the gas phase of hot material below in conjunction with specific embodiment to be described further, but protection scope of the present invention is not limited to this.
Embodiment 1
Reduced iron powder 10g being removed surface oxide layer adds in tube furnace, after the air in removal system, under the protection of nitrogen and a small amount of hydrogen, passes into H
2s gas, reacts 4 hours at 1100 DEG C, cooling.Be prepared into active ferrous sulphide.This active ferrous sulphide activity is high, at room temperature meets air and namely spontaneous combustion occurs.Limited oxygen index is less than 13%.
At room temperature, mixed by air with nitrogen, obtained oxygen content is the mist of 1-5%, passes in the ferrous sulfide system of above-mentioned preparation, and flow is 50mL/min, and reaction 20min, the limited oxygen index of gained sample is 24.3-26.5%.Known with differential thermal analysis, its autoignition temperature is greater than 250-270 DEG C.Accompanying drawing 1 (it is result after 1%, 2%, 3%, 4%, 5% atmosphere process that curve 1,2,3,4,5 is respectively oxygen content) is shown in by differential thermal analysis collection of illustrative plates, show in figure, repair after-combustion temperature through gaseous passivation to raise, within the scope of 230-330 DEG C with oxygen concentration increase.
Embodiment 2
In 500mL there-necked flask, add 300mL deionized water, pass into high pure nitrogen and get rid of oxygen.Make cushioning liquid with sodium hydrogen phosphate and sodium dihydrogen phosphate, the pH value controlling solution is 7.5-8.0.Under High Purity Nitrogen protection, add 20g ferrous sulfate and dissolve.6g thioacetamide is dissolved in 50mL to remove in the water of oxygen, adds and be dissolved with in the there-necked flask of ferrous sulfate, react 3 hours under 80 DEG C of conditions in nitrogen protection atmosphere, filter and wash, finally with natural drying after absolute ethanol washing.All operations is all at N
2carry out in the glove box of atmosphere.Gained ferrous sulfide has very high activity, meets air spontaneous combustion.Oxygen index (OI) is less than 13%.
The ferrous sulfide of above-mentioned preparation is put into N
2add in the quartz ampoule of Passivation Treatment under protection.Pass into the mist that oxygen content is 1-2%, flow is 50mL/min, and reaction 15min, the oxygen index (OI) of gained treated sample is 25.4-27.6%.Known with differential thermal analysis, large 250 DEG C of its autoignition temperature.Accompanying drawing 2 (it is result after 1%, 2% atmosphere process that curve 1,2 is respectively oxygen content) is shown in by differential thermal analysis collection of illustrative plates, shows, repair after-combustion temperature and be respectively: at 214-286 DEG C through gaseous passivation in figure.
Embodiment 3
In two homemade No. 45 steel containers (see accompanying drawing 3), container capacity is 1 liter.Filling it up with crude oil respectively, for increasing sulfur corrosion effect, adding 20g thiophene in crude oil, sealing is also reacted 1 month under 40 DEG C of conditions.With oxygen, crude oil is wherein discharged.One of them is directly opened, and on inwall, black sulfur corrosion product to meet after air rapid oxidation in 1 minute, is converted into bronzing, and occurs with Mars.Another passes into nitrogen, oxygen gas mixture that oxygen content is 2%, and flow is 100mL/min, and reaction 20min, open container, the sulfur corrosion product of inwall presents brown.By analysis, the auto-ignition combustion temperature of the sulfur corrosion product of inwall is 230-250 DEG C.In this test, the quantity not sufficient of corrosion product is to measure oxygen index (OI).
Embodiment 4
By 10g metallic aluminium powder at N
2add in the quartz ampoule of Passivation Treatment under protection.Under room temperature condition, mixed by air with nitrogen, be mixed with the mist that oxygen content is 2%, pass in quartz ampoule, flow is 50mL/min, and reaction 30min, the oxygen index (OI) of gained treated sample is 17.4%.
By 10g metallic aluminium powder at N
2add in the quartz ampoule of Passivation Treatment under protection.The humidity improving Passivation Treatment gas is 80%, and keeps oxygen content to be 2%, and pass in quartz ampoule, flow is 50mL/min, and reaction 20min, the oxygen index (OI) of gained treated sample is 23.2%.
As can be seen here, for metallic aluminium powder powder material, improve the relative humidity disposing gas, can passivation efficiency be increased, when being conducive to preventing aluminium powder ingress of air, dieseling occurs.
Case study on implementation 5
Cobalt protoxide is the material making novel perceptual battery, and its autoignition temperature is about 40 DEG C.By 10gCoO at N
2add in the quartz ampoule of Passivation Treatment under protection.Under room temperature condition, mixed by air with nitrogen, be mixed with the mist that oxygen content is 3%, pass in quartz ampoule, flow is 40mL/min, and reaction 30min, the oxygen index (OI) of gained treated sample is 19.6%.
By similarity condition, the humidity regulating Passivation Treatment gas is 80%, and keeps oxygen content to be 3%, adds NO
20.5% makes catalyst, passes in quartz ampoule, and flow is 40mL/min, and reaction 20min, the oxygen index (OI) of gained treated sample is 26.5%.
As can be seen here, when passivation disposal is carried out to cobalt protoxide dusty material, improve the relative humidity disposing gas, add nitrogen oxide as catalytic agent, can passivation efficiency be increased, when effectively reduction material contacts with air, dieseling occurs.
Compared with prior art, in production equipment of the present invention, easy spontaneous combustion causes the blunt advantage disappearing quick method from the gas phase of hot material and is: to containing a small amount of easily spontaneous combustion, in the production equipment processing procedure of hot material, do not need to carry out fairly large improvement project to original production equipment, only need use and increase portion gas mixing, analysis and conveying device, invest little, easy to operate; In processing procedure, do not relate to cleaning solvent, the harmful substance such as waste gas, waste liquid contaminated environment can not be produced.
Claims (8)
1. in a production equipment, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, it is characterized in that, described method concrete steps mix with air for the nitrogen in: the nitrogen 1) utilizing deaerator to produce or nitrogen cylinder, and forming carrier of oxygen volume concentrations is the mist of 0.5%-5%; 2) mist is passed into pending equipment from air inlet, carry out gas phase and cause and bluntly disappear quick, then overflow from the gas outlet of equipment; 3) with the oxygen content of detection means measure emergent gas, when its with oxygen content in input gas close to time, process completes.
2. in a kind of production equipment according to claim 1, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and it is characterized in that, the degree of accuracy of described carrier of oxygen volume concentrations is within ± 0.05%.
3. in a kind of production equipment according to claim 1, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, it is characterized in that, gas outlet and air inlet are when same position, and adopt different conduit respectively as air inlet and gas outlet, wherein the length of air induction conduit is greater than the length of outtake tube.
4. in a kind of production equipment according to claim 1, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and it is characterized in that, it is 10-60min that described gas phase causes the blunt quick time that disappears.
5. in a kind of production equipment according to claim 1, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and it is characterized in that, the maximum of described carrier of oxygen volume concentrations is C × (t
1-t
0)/Q; Described C is the thermal capacitance of all substances in reaction system, and Q is the mist of unit volume oxygen content and the redox reaction heat of pending material, t
0for reaction temperature during desensitization deactivation, t
1for the burning-point of material and oil gas.
6. in a kind of production equipment according to claim 1, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and it is characterized in that, described checkout gear is tunable diode laser oxygen measurement system.
7. in a kind of production equipment according to claim 1, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and it is characterized in that, the humidity of described mist is 70-90%.
8. in a kind of production equipment according to claim 1, easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material, and it is characterized in that, described mist contains nitrogen oxide as catalyst.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463365A (en) * | 2015-11-19 | 2016-04-06 | 北京石油化工学院 | Spontaneous-combustion active ferrous sulfide gaseous phase passivation device and method |
| CN109522668A (en) * | 2018-11-28 | 2019-03-26 | 南京工业大学 | A kind of gas phase protection method inhibiting the iron compound spontaneous combustion of petrochemical equipment inner wall sulphur |
| CN113092401A (en) * | 2021-03-31 | 2021-07-09 | 重庆文理学院 | Gas-sensitive analysis system for laboratory |
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| CN1431027A (en) * | 2002-01-11 | 2003-07-23 | 廖赤虹 | Method and system for putting out fire happened in unopened space |
| CN102181818A (en) * | 2011-04-19 | 2011-09-14 | 潘伦桃 | Method and device for surface passivation of tantalum metal |
| CN202063985U (en) * | 2011-04-19 | 2011-12-07 | 潘伦桃 | Tantalum surface passivation device with refrigerating device |
| CN202072755U (en) * | 2011-03-23 | 2011-12-14 | 宁夏东方钽业股份有限公司 | Tantalum metal surface passivation device |
| CN103429782A (en) * | 2011-03-23 | 2013-12-04 | 宁夏东方钽业股份有限公司 | Method for passivating tantalum metal surface and apparatus thereof |
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2014
- 2014-12-30 CN CN201410844215.1A patent/CN104524714B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| AU4093000A (en) * | 1999-04-28 | 2000-11-10 | Cast Centre Pty Ltd | Cover gases |
| CN1431027A (en) * | 2002-01-11 | 2003-07-23 | 廖赤虹 | Method and system for putting out fire happened in unopened space |
| CN202072755U (en) * | 2011-03-23 | 2011-12-14 | 宁夏东方钽业股份有限公司 | Tantalum metal surface passivation device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463365A (en) * | 2015-11-19 | 2016-04-06 | 北京石油化工学院 | Spontaneous-combustion active ferrous sulfide gaseous phase passivation device and method |
| CN109522668A (en) * | 2018-11-28 | 2019-03-26 | 南京工业大学 | A kind of gas phase protection method inhibiting the iron compound spontaneous combustion of petrochemical equipment inner wall sulphur |
| CN113092401A (en) * | 2021-03-31 | 2021-07-09 | 重庆文理学院 | Gas-sensitive analysis system for laboratory |
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