CN104498744B - Environmental-protection type magnesium alloy melting protection gas and its preparation method and application - Google Patents
Environmental-protection type magnesium alloy melting protection gas and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of environmental-protection type magnesium alloy melting protection gas and its preparation method and application; protection gas bag includes suppression gas and the carrier gas that can suppress magnesium and magnesium alloy that oxidizing fire occurs in fusion process, and particularly, described suppression gas comprises 2; 2,2 trifluoro ethyl mercaptans.The melting protective gas that the present invention uses uses 2,2,2 trifluoro ethyl mercaptans or 2; 2; the mixture that 2 trifluoro ethyl mercaptans and R134a, R125, R32 etc. are formed is inhibitor, and dry air, nitrogen, carbon dioxide, argon etc., as carrier gas, carry out surface protection to melted magnesium alloy.In protection gas, contained fluoro-gas does not all have destruction to ozone layer, and greenhouse effect value is much smaller than SF6, it is possible to meet the requirement of environmental conservation.
Description
Technical field
The present invention relates to a kind of magnesium alloy smelting protection gas and its preparation method and application.
Background technology
The essence of magnesium alloy smelting protection is to reduce the oxidizing fire of magnesium during magnesium alloy smelting, and its method is the most permissible
It is divided into three kinds: flux protection, gas shield, alloying ignition-proof.Flux protection is the guarantor used the earliest during magnesium alloy smelting
Maintaining method.The protection mechanism of magnesium alloy flux is mainly by the inorganic compound of low melting point so that it is melt at a lower temperature
For liquid, and spread out at magnesium alloy liquid level, stop magnesium liquid and air contact, thus play a protective role.Although flux protection exists
In production easy to use, cost is relatively low, and protected effect is obvious, but there is also a lot of problem, as flux exists simultaneously
Fusion process can discharge the harmful gass such as C12, HC1；Fusion process then can gradually sink or be blended in magnesium alloy
In melt, thus pollute Serum Magnesium；In addition, there is also flux protection makes magnesium alloy liquation be lost relatively in fusion process
The problem such as big.Melt alloying fire-retardant method is through adding some alloying element in magnesium alloy thus improves Serum Magnesium surface
The method of oxide-film consistency realizes fire-resisting protection.Although alloying ignition-proof Protection Code is favorably improved magnesium alloy parts
Corrosion resisting property and heat resistance: but the addition of flame-retardant alloy element not only significantly improves the production cost of magnesium alloy, and change
The chemical composition of magnesium alloy, phase composition and tissue morphology, often ultimately result in magnesium alloy mechanical property and decline.Gas protection method
It is to react, by protective gas and magnesium alloy, the high-compactness surface embrane method generated to realize fire-retardant.Gas protection method has guarantor
Protect effective, do not pollute in Serum Magnesium, fusion process the advantages such as loss is few, these be additive method incomparable.Therefore,
Gas protection method has become most popular smelting flame-proof protection method for magnesium alloy, be widely used in magnesium alloy liquid forming,
Among remelting refining and heat treatment.
On magnesium alloy gas shield is applied, the past has had much gas to apply, such as use noble gas such as argon,
Nitrogen, active gases such as carbon dioxide, sulfur dioxide etc., wherein sulfur dioxide owing to it is cheap, be readily available and relatively
Be widely used in the long time, yet with it, there is bigger stink, metal protection and toxicity, receive equipment with
And the restriction of environment.Alternatively, now widely available low toxicity and tasteless sulfur hexafluoride (SF6), it mainly has as follows
Feature: nontoxic, tasteless, protected effect is good, consumption is few, do not pollute, and the corrosion rate of Mg alloy castings can be effectively reduced, carry
High corrosion resistance.Although SF6 has lot of advantages, but in recent years through the experimental demonstration of some researchers, SF6 is a kind of energy
The strong gas producing greenhouse effect.SF6 is strong due to its ability absorbing long wave, and the time retained in an atmosphere is long, belongs to
Highly produce the gas of greenhouse effect.According to the estimation of climate change committee of government department of the United Nations (IPCC), SF6 is a kind of
Have the gas of the highest GWP global warming potential, i.e. greenhouse effect produced by SF6 was equivalent to CO2 within ground level upper 100 year
23900 times.
In order to protect environment, people actively make great efforts to seek the succedaneum of SF6, have had technical scheme disclosed in some.Ratio
As CN101302588A discloses the compositions of a kind of hexafluoropropene and carrier gas；CN1352583A disclose a kind of tetrafluoroethane and
The compositions of air；CN101321597A discloses a kind of with HFC-245fa, HFO-1234ze and HFE-254pc as activity
The compositions of composition；3M company discloses the technical scheme using perfluor ketone.But, these technical schemes all there are disadvantages that
And deficiency, although the material used having does not damages the ozone layer but still has greenhouse effect, some protected effect are relatively
Difference, some use costs are higher.
It addition, the admixture of gas being currently used for magnesium alloy protection generally uses traditional gas mixing arrangement to prepare.Pass
The gas mixer of system is often formed in parallel by a plurality of gas circuit, after gas is reduced pressure by air relief valve, uses spinner flowmeter
The flow of each component gas is individually measured, completes gas mixed process at a storage tank, have many to mix even without special
Close unit.Such gas mixing device is applicable at some for the occasion such as welding protection that mixed gas prescription is the highest
, but it exists many not enough, first by flow measurement instrument be spinner flowmeter, spinner flowmeter is general when dispatching from the factory
25 DEG C, demarcate under the conditions of 101325Pa, marked gas is nitrogen or water, needs according to use when measuring other gas
Time pressure, temperature, the practical situation such as gas density utilize empirical equation to be corrected, result precision is relatively low, it addition, gas
Actual flow value also affected by factors such as variation of ambient temperature, pipeline pressure fluctuations；Secondly, tradition gas mixing device
When rear end consumption changes, need to operate regulation effusion meter frequently, extremely inconvenience；Again, the mixed gas dress of traditional type
Put and in use need groping of long period, the demand of user could be met.
Summary of the invention
The technical problem to be solved is to overcome the deficiencies in the prior art, it is provided that a kind of protected effect is good and ring
The environmental-protection type magnesium alloy melting protection gas protected.
The present invention also provides for the preparation method and application of described environmental-protection type magnesium alloy melting protection gas simultaneously.
For solving above technical problem, a kind of technical scheme that the present invention takes is as follows:
, in fusion process, there is oxidation combustion including magnesium and magnesium alloy can be suppressed in a kind of environmental-protection type magnesium alloy melting protection gas
The suppression gas burnt and carrier gas, particularly, described suppression gas comprises 2,2,2-trifluoro ethyl mercaptans.
Preferably, described suppression gas volume content in described protection gas is 0.01%～1%.It is highly preferred that press down
The gas processed volume content in protection gas is 0.1%～0.5%.Most preferably, suppression gas volume in protection gas contains
Amount is 0.1%～0.3%.
Further, from a cost perspective, described suppression gas can also and preferably comprise selected from 1,1,1,2-tetrafluoro
The combination of one or more in ethane (R134a), pentafluoroethane (R125) and difluoromethane (R-32).
Further, it can be 0～100% that 2,2,2-trifluoro ethyl mercaptans account for the volume content of described suppression gas, preferably
It is 5～50%, more preferably 10～30%.
According to the present invention, described carrier gas can be conventional those, concretely dry air, carbon dioxide, nitrogen, argon
One or more in gas etc., the most more preferably nitrogen and carbon dioxide.
The present invention also provides for the preparation method of a kind of above-mentioned environmental-protection type magnesium alloy melting protection gas, and it uses gas to mix
Each component of composition protection gas is mixed in proportion and obtains protecting gas by device, and gas mixer includes mixed gas tank and multiple gas
Transfer pipeline, the one end of gas transfer pipeline is connected with air accumulator, the other end is connected with mixed gas tank, particularly, described gas
It is sequentially provided with air relief valve and electromagnetic proportional valve from described one end towards the direction of described the other end on body transfer pipeline, described
Gas mixer also include being connected with described mixed gas tank, for the gas in described mixed gas tank forms the gas being analyzed
Body component analysis instrument and the PLC being connected with described gas composition analysis instrument, described electromagnetic proportional valve is controlled with described PLC
Device processed connects and controlled, and described PLC receives the analysis result of described gas composition analysis instrument and according to analysis result
Electromagnetic proportion regulating on corresponding gas transfer pipeline is adjusted the composition realizing accurately controlling mixed gas.
Preferably, on gas transfer pipeline, the downstream of air relief valve, the upstream of electromagnetic proportional valve are provided with filter.Filtration is set
Device, to remove minute solid particles impurity that may be present in gas piping, protects electromagnetic proportional valve.
Preferably, on gas transfer pipeline, the downstream of electromagnetic proportional valve is provided with check (non-return) valve, flows backwards to prevent gas from occurring
Phenomenon.
It is further preferred that described gas mixer also includes being positioned at mixed gas tank top for the pressure to mixed gas tank
Power carries out the pressure transducer detected, and this pressure transducer is connected with PLC, and PLC is according to pressure transducer
Electromagnetic proportion regulating is adjusted by testing result.
Further, in the plurality of gas transfer pipeline is carrier gas gas circuit, and remaining is work gas gas circuit, PLC
Electromagnetic proportion regulating in carrier gas gas circuit is adjusted by controller according to the testing result of pressure transducer.Carrier gas gas circuit and
Work gas circuit divides according to gas circuit composition, and wherein carrier gas gas circuit typically walks the gas that content in mixed gas is higher, work
Make gas gas circuit to take a walk the relatively low gas of content in mixed gas.
Further, described gas transfer pipeline is connected with the bottom of mixed gas tank, makes gas enter from the bottom of mixed gas tank
In mixed gas tank, gas composition analysis instrument is connected with the middle and upper part of mixed gas tank, and the mixed gas outlet of mixed gas tank is positioned at mixed gas tank
Top.
The present invention also provides for a kind of method stoping magnesium and magnesium alloy that oxidizing fire occurs in fusion process, the method
For: when magnesium and magnesium alloy smelting, environmental-protection type magnesium alloy melting protection gas above-mentioned for the present invention is introduced the surface of motlten metal,
Form fine and close protecting film with the reactive magnesium under molten condition, thus stop it that oxidizing fire occurs.
The object that the present invention protects gas to protect includes the melting of the magnesium alloy of pure magnesium and the various trade mark, applicable melting
Temperature is below 760 DEG C.
The present invention protects in gas, 2,2,2-trifluoro ethyl mercaptans protected effect during magnesium alloy smelting and sulfur hexafluoride
Close, the skin covering of the surface of formation has metallic luster, mainly by MgS, MgO, MgF2Deng composition, wherein it is mingled with micro activated carbon particle and fills out
Filling gap, therefore its actual minimum amount is even better than sulfur hexafluoride, and 2,2,2-trifluoro ethyl mercaptans also do not have greenhouse effect simultaneously.
Therefore, the present invention relates particularly to, and 2,2,2-trifluoro ethyl mercaptans protect magnesium and the purposes of magnesium alloy in magnesium and magnesium alloy smelting.
So, the harm to environment can be reduced on the premise of ensureing protected effect, for accelerating to eliminate sulfur hexafluoride, environmental conservation
Also there is the biggest contribution.
Due to the enforcement of above technical scheme, the present invention compared with prior art has the advantage that
The melting protective gas that the present invention uses use 2,2,2-trifluoro ethyl mercaptan or 2,2,2-trifluoro ethyl mercaptan with
The mixture that R134a, R125, R32 etc. are formed is inhibitor, dry air, nitrogen, carbon dioxide, argon etc. as carrier gas,
Melted magnesium alloy is carried out surface protection.The fluoro-gas taked in this programme does not all have destruction to ozone layer, right
For greenhouse effect value (GWP value), R134a is 1300, and R125 is 3200, and R32 is 580, and 2,2,2-trifluoro ethyl mercaptans do not have
There is greenhouse effect value, relative to the 23900 of SF6, it is possible to meet the requirement of environmental conservation.
The preparation of melting of the present invention protection gas uses the gas mixer improved, and the device after this improvement has abandoned use
Spinner flowmeter sums up the pattern of metering mixture, introduces gas composition analysis instrument, the directly work gas in the mixed gas tank of monitoring
Body forms, and result is fed back to PLC, PLC forms result through computer journey according to the gas fed back
Sequence calculates, and the electromagnetic proportion regulating of relevant work gas circuit is adjusted by the result according to calculating, it is achieved accurately control gas
Form this function；For rear end gas consumption situation of change that may be present, pressure sensor monitoring is used to mix the pressure of gas tank,
Result is fed back to PLC, after being judged by PLC equally, the electromagnetic proportion regulating of carrier gas gas circuit is adjusted
Joint, it is achieved stably supply this function；Use PLC and the combination of electromagnetic proportion regulating, it is achieved automatically control this
Function, is easy to use quick.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the present invention is not limited to following enforcement
Example.The implementation condition used in embodiment can do further adjustment, not marked enforcement according to specifically used different requirement
Condition is the condition in normal experiment.
Embodiment 1
This example provides a kind of gas mixer, and gas mixer mainly includes that air accumulator (includes carrier gas reservoir and work
Make gas storage tank, multiple gas transfer pipelines, be arranged on the air relief valve on each gas transfer pipeline, filter, electromagnetic proportional valve and
Check (non-return) valve, mixed gas tank, pressure transducer, gas composition analysis instrument and PLC.From the point of view of from gas circuit is constituted, Duo Geqi
Body transfer pipeline is divided into carrier gas gas circuit and work gas gas circuit, and wherein carrier gas gas circuit typically walks the gas that content in mixed gas is higher
Body, such as nitrogen, air, carbon dioxide etc.；Work gas gas circuit is taken a walk the relatively low gas of content in mixed gas, as sulfur dioxide,
Sulfur hexafluoride etc..When needing multiple gases to mix, it is only necessary to increase corresponding gas circuit, structurally can take same side
Formula.
In each gas circuit, from gas feed end, air relief valve, filter, electromagnetic proportional valve, check (non-return) valve set successively
Put, wherein air relief valve act as regulate gas piping initial pressure；Filter removes in gas piping that may be present small
Solid particle polluter, protects electromagnetic proportional valve, recommends the pneumatic filter using filter diameter less than 40 microns in this device；
The size of flow in electromagnetic proportional valve control piper, accepts the signal from PLC and drives；Check (non-return) valve prevents gas from occurring
The phenomenon flow backwards.
On mixed gas tank, working gas and carrier gas all enter from mixed gas tank bottom, and pressure transducer is positioned at the top of mixed gas tank
Portion, gas composition analysis instrument is positioned in mixed gas tank position, and mixed gas outlet is positioned at mixed gas tank top.Mixed gas tank should have
Certain volume, depending on concrete size is according to final gas usage.
Automatically controlling part, PLC accepts pressure transducer and the signal of gas composition analysis instrument, through calculating
Program controls the aperture of the electromagnetic proportional valve of corresponding gas circuit after calculating.Such as, mixed gas tank pressure more than or less than setting value, is then controlled
The aperture of carrier gas gas circuit electromagnetic proportional valve processed reduces or increases.It is true that PLC is for mixture pressure and composition
It is in Sustainable Control state.
Embodiment 2
Without sealing the melting carrying out magnesium alloy AZ31 in iron pot furnace, smelting furnace is covered with a gas and is passed through steel pipe, outward
Footpath is 6mm, smelting furnace diameter 150mm, highly 250mm, equipped with AZ91D magnesium alloy the most dried for 3.5kg.Open heating by electric cooker
Switch, sets in-furnace temperature as 600 DEG C, when internal temperature reaches 400 DEG C, starts to be passed through protection gas, when after magnesium alloy thawing,
Setting in-furnace temperature 670 DEG C, the gas mixer now by embodiment 1 regulates the protection composition of gas and consumption, tests it
Protected effect；Continuing to heat up, measure smelting temperature respectively at 720 DEG C, protected effect at 760 DEG C, concrete result data is shown in
Following table:
Abbreviation and the meaning (as follows) of symbology in upper table:
TFET 2,2,2-trifluoro ethyl mercaptan is called for short；
N2, 3 represent that using carrier gas is nitrogen, and flow is 3L/min；
★ protected effect is excellent, and concrete judgment criteria is for opening upper cover, after atmosphere is taken off the film of cleaved surface, and skin covering of the surface
Can heal the most rapidly, form new film, without burning-point, basic non-oxidation slag, the operating time can support more than 5min；
■ protected effect is good, and concrete judgment criteria is for opening upper cover, after atmosphere is taken off the film of cleaved surface, and skin covering of the surface
Energy self-heal, forms new film, without burning-point, has a small amount of oxidizing slag, and the operating time can support more than 3min；
▲ protected effect is poor, and concrete judgment criteria is for opening upper cover, after atmosphere is taken off the film of cleaved surface, and skin covering of the surface
Can maybe can not heal by indolence, there is burning-point in surface, has more oxidizing slag, and the operating time is within 3min；
Upper table experimental data illustrates, takes 2,2,2-trifluoro ethyl mercaptans and itself and containing that R134a, R125, R32 etc. form
Fluorine suppression gas, can effectively protect the fusion process of magnesium alloy AZ31.
Embodiment 3
Carrying out the melting of magnesium alloy AM50 in nothing seals iron pot furnace, other operation and condition are complete with embodiment 2
Identical, concrete result data see table:
In upper table, experimental data explanation, takes 2,2,2-trifluoro ethyl mercaptans and its with R134a, R125, R32 etc. composition
Fluorine-containing suppression gas, can effectively protect the fusion process of magnesium alloy AM50.
Embodiment 4
Without sealing the melting carrying out pure magnesium in iron pot furnace, other operation is identical with embodiment 1 with condition, tool
The result data of body see table:
In upper table, experimental data explanation, takes 2,2,2-trifluoro ethyl mercaptans and its with R134a, R125, R32 etc. composition
Fluorine-containing suppression gas, can effectively protect the fusion process of pure magnesium.
Comparative example 1
Without sealing in iron pot furnace the melting carrying out magnesium alloy AZ31, contrast R134a, R125 and R32 purely with
Protected effect after mixing TFET, concrete result data see table:
As can be seen here, compared to R134a, R125 and R32 purely, it is mixed with the fluorine-containing suppression gas energy after TFET
Enough fusion process more efficiently protecting magnesium alloy.
Above the present invention is described in detail, its object is to allow the personage being familiar with this art will appreciate that this
Invention content and be carried out, can not limit the scope of the invention with this, all spirit institutes according to the present invention
The equivalence change made or modification, all should contain within the scope of the present invention.
Claims (10)
1. environment friendly magnesium and a magnesium alloy smelting protection gas, aoxidize in fusion process including suppressing magnesium and magnesium alloy
The suppression gas of burning and carrier gas, it is characterised in that: described suppression gas comprises 2,2,2-trifluoro ethyl mercaptans.
Environment friendly magnesium the most according to claim 1 and magnesium alloy smelting protection gas, it is characterised in that: described suppression gas exists
Volume content in described protection gas is 0.01%～1%.
Environment friendly magnesium the most according to claim 2 and magnesium alloy smelting protection gas, it is characterised in that: described suppression gas exists
Volume content in described protection gas is 0.1%～0.5%.
4. protect gas according to the environment friendly magnesium described in claim 1 or 2 or 3 and magnesium alloy smelting, it is characterised in that: described suppression
Gas also comprises the combination of one or more in 1,1,1,2-tetrafluoroethane, pentafluoroethane and difluoromethane.
Environment friendly magnesium the most according to claim 4 and magnesium alloy smelting protection gas, it is characterised in that: described 2,2,2-trifluoros
It is 5 ~ 50% that ethyl mercaptan accounts for the volume content of described suppression gas.
Environment friendly magnesium the most according to claim 5 and magnesium alloy smelting protection gas, it is characterised in that: described 2,2,2-trifluoros
It is 10 ~ 30% that ethyl mercaptan accounts for the volume content of described suppression gas.
Environment friendly magnesium the most according to claim 1 and magnesium alloy smelting protection gas, it is characterised in that: described carrier gas is for being selected from
The combination of one or more in dry air, carbon dioxide, nitrogen, argon.
8. environment friendly magnesium described in claim any one of claim 1-7 and the preparation side of magnesium alloy smelting protection gas
Method, its use gas mixer by composition protection gas each component be mixed in proportion obtain protect gas, described gas mixing dress
Putting and include mixed gas tank and multiple gas transfer pipeline, the one end of described gas transfer pipeline is connected with air accumulator, the other end
It is connected with described mixed gas tank, it is characterised in that: from described one end towards described the other end on described gas transfer pipeline
Direction is sequentially provided with air relief valve and electromagnetic proportional valve, described gas mixer also includes being connected with described mixed gas tank, for
Gas in described mixed gas tank is formed the gas composition analysis instrument being analyzed and is connected with described gas composition analysis instrument
PLC, described electromagnetic proportional valve is connected and controlled with described PLC, described PLC receive described gas
Electromagnetic proportional valve on corresponding gas transfer pipeline is also adjusted by the analysis result of body component analysis instrument according to analysis result
Realize accurately controlling the composition of mixed gas.
9. one kind stops the method that magnesium and magnesium alloy occur oxidizing fire in fusion process, it is characterised in that: close at magnesium and magnesium
Gas is protected to introduce the environment friendly magnesium described in claim any one of claim 1-7 and magnesium alloy smelting during gold melting melted
Reactive magnesium under metallic surface, with molten condition forms the protecting film of densification, thus stops it that oxidizing fire occurs.
10.2,2,2-trifluoro ethyl mercaptan protects magnesium and the purposes of magnesium alloy in magnesium and magnesium alloy smelting.
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| CN107299241B (en) * | 2017-06-02 | 2019-01-29 | 青海盐湖工业股份有限公司 | A kind of air supply system and Mg alloy smelting furnace of magnesium alloy smelting protective gas |
| CN112264601A (en) * | 2020-09-30 | 2021-01-26 | 青海海镁特镁业有限公司 | Environment-friendly mixed protective gas for magnesium alloy production process and application thereof |
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| CN1962905A (en) * | 2006-11-29 | 2007-05-16 | 青岛地恩地投资集团有限公司 | Method for protecting tetrafluoroethane gas in magnesium or magnesium alloy smelting furnace |
| CN101396726A (en) * | 2008-11-07 | 2009-04-01 | 李远发 | Molten metal protection method using HFC-134a and nitrogen gas during magnesium alloy pressure-casting process |
| CN101914696B (en) * | 2010-06-24 | 2012-01-11 | 西北工业大学 | Combustion-oxidation preventing method in magnesium alloy smelting and antigravity casting process and mixture system |
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