CN104498744A - Environment-friendly magnesium alloy smelting protective gas as well as preparation method and application thereof - Google Patents
Environment-friendly magnesium alloy smelting protective gas as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to an environment-friendly magnesium alloy smelting protective gas as well as a preparation method and an application thereof. The protective gas comprises an inhibiting gas capable of inhibiting oxidative combustion of magnesium and magnesium alloy in the smelting process, and a carrier gas. Particularly, the inhibiting gas contains 2,2,2-trifluoroethanethiol. According to the invention, the smelting protective gas adopts a mixture composed of 2,2,2-trifluoroethanethiol or a mixture of 2,2,2-trifluoroethanethiol, R134a, R125, R32 and the like is utilized as an inhibitor; dry air, nitrogen, carbon dioxide, argon and the like are adopted as the carrier gas; and the molten magnesium alloy is subjected to surface protection. The fluorine-containing gas contained in the protective gas does not have a destroy effect on an ozone layer; and the greenhouse effect value is much smaller than SF6, and thus the requirements of environmental protection can be met.
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 reduces the oxidizing fire of magnesium in magnesium alloy smelting process, and its method roughly can be divided into three kinds: flux protection, gas shield, alloying ignition-proof.Flux protection is the guard method used the earliest in magnesium alloy smelting process.The protection mechanism of magnesium alloy flux mainly utilizes the mineral compound of low melting point, makes it be molten into liquid state at a lower temperature, and spreads out at magnesium alloy liquid level, stops magnesium liquid to contact with air, thus plays a protective role.Although flux protection is easy to use in production, cost is lower, and protected effect is obvious, also there is a lot of problem, as flux can discharge the obnoxious flavoures such as C12, HC1 in melting process simultaneously; Then can sink gradually or be blended in magnesium alloy fused mass in fusion process, thus pollute Serum Magnesium; In addition, also there will be flux protection and make the problems such as the loss in fusion process of magnesium alloy liquation is larger.Melt alloying fire-retardant method by adding some alloying element thus the method improving Serum Magnesium surface film oxide density realizes fire-resisting protection in magnesium alloy.Although alloying ignition-proof protection method contributes to improving the corrosion resisting property of magnesium alloy parts and resistance toheat: flame-retardant alloy element add the production cost not only significantly improving magnesium alloy; and change the chemical composition of magnesium alloy, phase composite and tissue morphology, often finally cause magnesium alloy mechanical property to decline.Gas protection method reacts by shielding gas and magnesium alloy the high-compactness surface embrane method generated to realize fire-retardant.Gas protection method have protected effect good, not pollute in Serum Magnesium, fusion process the advantages such as loss is few, these be additive method incomparable.Therefore, gas protection method has now become most popular smelting flame-proof protection method for magnesium alloy, is widely used among the liquid forming of magnesium alloy, remelting refining and thermal treatment.
In magnesium alloy gas shield application; there have been many gas application in past; such as use rare gas element as argon gas, nitrogen; reactive gas is as carbonic acid gas, sulfurous gas etc.; wherein sulfurous gas is widely used within the longer time due to its cheap, easy acquisition; but due to it, there is larger stink, metal protection and toxicity, receive equipment and environmental limit.Alternatively; widely use now low toxicity and tasteless sulfur hexafluoride (SF6); it mainly has following features: nontoxic, tasteless, protected effect is good, consumption is few, do not pollute, and effectively can reduce the erosion rate of Mg alloy castings, improves corrosion resisting property.Although SF6 has lot of advantages, pass through the experimental demonstration of some researchers in recent years, SF6 is a kind of gas that strongly can produce Greenhouse effect.The ability that SF6 absorbs long wave due to it is strong, and the time retained in an atmosphere is long, belongs to the gas highly producing Greenhouse effect.According to the estimation of the climate change council of government department of United Nations (IPCC), SF6 is a kind of gas with very high GWP global warming potential, and namely the Greenhouse effect that produce of SF6 were equivalent to 23900 times of CO2 within ground level upper 100 year.
In order to protection of the environment, people actively make great efforts the substitute of seeking SF6, have had technical scheme disclosed in some.Such as CN101302588A discloses the composition of a kind of R 1216 and carrier gas; CN1352583A discloses the composition of a kind of Tetrafluoroethane and air; CN101321597A discloses a kind of composition being activeconstituents with HFC-245fa, HFO-1234ze and HFE-254pc; 3M company discloses the technical scheme using perfluor ketone.But these technical schemes all exist some shortcoming and defect, although the material used had does not damage the ozone layer but still has Greenhouse effect, some protected effect are relatively poor, and some use costs are higher.
In addition, the existing gaseous mixture for magnesium alloy protection adopts traditional gas mixing device to prepare usually.Traditional gas mixer is often formed in parallel by many gas circuits, after gas is reduced pressure by reducing valve, use the flow of spinner-type flowmeter to each component gas to measure separately, complete gas and vapor permeation process at a storage tank, having manyly even does not have special mixed cell.Such gas mixing device is applicable at some for occasion such as the welding protection that mixed gas specification of quality is not high, but there is many deficiencies in it, first the flow metering instrument used is spinner-type flowmeter, spinner-type flowmeter when dispatching from the factory generally at 25 DEG C, demarcate under 101325Pa condition, marked gas is nitrogen or water, need when measuring other gas according to pressure when using, temperature, the practical situation such as gas density utilize experimental formula to correct, result precision is lower, in addition, the actual flow value of gas is also subject to variation of ambient temperature, the impact of the factors such as pipeline pressure fluctuation, secondly, traditional gas mixing device, when rear end consumption changes, needs to operate adjust flux meter frequently, very inconvenience, again, the gas mixing device of traditional type in use needs groping of long period, could meet the demand of user.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, provides a kind of protected effect good and the environmental-protection type magnesium alloy melting of environmental protection protection gas.
The present invention also provides described environmental-protection type magnesium alloy melting to protect the preparation method and application of gas simultaneously.
For solving above technical problem, a kind of technical scheme that the present invention takes is as follows:
A kind of environmental-protection type magnesium alloy melting protection gas, comprise suppression gas and the carrier gas that can suppress Mg-based hydrogen storage that oxidizing fire occurs in fusion process, particularly, described suppression gas comprises 2,2,2-trifluoro sulfur alcohol.
Preferably, the volume content of described suppression gas in described protection gas is 0.01% ~ 1%.More preferably, the volume content of gas in protection gas is suppressed to be 0.1% ~ 0.5%.Most preferably, the volume content of gas in protection gas is suppressed to be 0.1% ~ 0.3%.
Further, consider from cost angle, described suppression gas can also and preferably comprise and be selected from 1,1, one or more combination in 1,2-Tetrafluoroethane (R134a), pentafluoride ethane (R125) and methylene fluoride (R-32).
Further, the volume content that 2,2,2-trifluoro sulfur alcohol accounts for described suppression gas can be 0 ~ 100%, is preferably 5 ~ 50%, is more preferably 10 ~ 30%.
According to the present invention, described carrier gas can be conventional those, specifically can be one or more in dry air, carbonic acid gas, nitrogen, argon gas etc., wherein more preferably nitrogen and carbonic acid gas.
The present invention also provides a kind of above-mentioned environmental-protection type magnesium alloy melting to protect the preparation method of gas, it adopts gas mixer each component of composition protection gas to be mixed in proportion and obtains protecting gas, gas mixer comprises mixed gas tank and multiple gas transfer pipeline, one end of gas transfer pipeline is connected with gas-holder, the other end is connected with mixed gas tank, particularly, described gas transfer pipeline is provided with reducing valve and electromagnetic proportional valve from a described end successively towards the direction of described the other end, described gas mixer also comprises and being connected with described mixed gas tank, for the gas composition analysis instrument analyzed the gas composition in described mixed gas tank and the PLC be connected with described gas composition analysis instrument, described electromagnetic proportional valve is connected with described PLC and controlled, described PLC receives the analytical results of described gas composition analysis instrument and carries out regulating the composition realizing accurately controlling mixed gas according to analytical results to the electromagnetic proportion regulating on corresponding gas transfer pipeline.
Preferably, on gas transfer pipeline, the downstream of reducing valve, the upstream of electromagnetic proportional valve are provided with strainer.Strainer is set to remove the minute solid particles impurity that may exist in gas piping, protection electromagnetic proportional valve.
Preferably, on gas transfer pipeline, the downstream of electromagnetic proportional valve is provided with non-return valve, occurs the phenomenon flow backwards to prevent gas.
Further preferably, described gas mixer also comprises and is positioned at the pressure transmitter of mixed gas tank top for detecting the pressure of mixed gas tank, this pressure transmitter is connected with PLC, and PLC regulates electromagnetic proportion regulating according to the detected result of pressure transmitter.
Further, one in described multiple gas transfer pipeline is carrier gas gas circuit, and all the other are work gas gas circuit, and PLC regulates the electromagnetic proportion regulating in carrier gas gas circuit according to the detected result of pressure transmitter.Carrier gas gas circuit and work gas circuit form according to gas circuit and divide, and wherein carrier gas gas circuit generally walks the higher gas of content in mixed gas, and work gas gas circuit is taken a walk the lower gas of content in mixed gas.
Further, described gas transfer pipeline is connected with the bottom of mixed gas tank, and make gas enter in mixed gas tank from the bottom of 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 the top of mixed gas tank.
The present invention also provides a kind of method stoping Mg-based hydrogen storage that oxidizing fire occurs in fusion process; the method is: the surface of when Mg-based hydrogen storage melting, environmental-protection type magnesium alloy melting above-mentioned for the present invention protection gas being introduced molten metal; form fine and close protective membrane with the reactive magnesium under molten state, thus stop it that oxidizing fire occurs.
The object that the present invention protects gas to protect comprises the melting of the magnesium alloy of pure magnesium and the various trade mark, and applicable smelting temperature is below 760 DEG C.
The present invention protects in gas, the protected effect of 2,2,2-trifluoro sulfur alcohol in magnesium alloy smelting process and sulfur hexafluoride close, the surface film of formation has metalluster, primarily of MgS, MgO, MgF
2deng composition, be wherein mingled with micro activated carbon particle and fill gap, therefore its actual minimum amount is even better than sulfur hexafluoride, and 2,2,2-trifluoro sulfur alcohols also do not have Greenhouse effect simultaneously.Therefore, the present invention also in particular to, 2,2,2-trifluoro sulfur alcohol protects the purposes of Mg-based hydrogen storage in Mg-based hydrogen storage melting.So, the harm to environment can be reduced under the prerequisite ensureing protected effect, for the superseded sulfur hexafluoride of acceleration, environment protection, also there is very large contribution.
Due to the enforcement of above technical scheme, the present invention compared with prior art tool has the following advantages:
The melting shielding gas that the present invention adopts uses 2,2,2-trifluoro sulfur alcohol or 2; 2; the mixture that 2-trifluoro sulfur alcohol and R134a, R125, R32 etc. form is inhibitor, and dry air, nitrogen, carbonic acid gas, argon gas etc., as carrier gas, carry out surface protection to the magnesium alloy of melting.The fluoro-gas taked in this programme does not all have destruction to ozonosphere; for Greenhouse effect value (GWP value); R134a is 1300; R125 is 3200, R32 is 580, and 2; 2; 2-trifluoro sulfur alcohol does not have Greenhouse effect value, relative to 23900 of SF6, can meet the requirement of environment protection.
The preparation of melting protection gas of the present invention adopts the gas mixer improved, device after this improvement has been abandoned and has been used spinner-type flowmeter to sum up the pattern of metering mixture, introduce gas composition analysis instrument, direct monitoring mixes the working gas composition in gas tank, by result feedback to PLC, calculated through computer program according to fed back gas composition result by PLC, the electromagnetic proportion regulating of result to relevant work gas circuit according to calculating regulates, and realizes accurately controlling this function of gas composition; For the changing conditions that rear end gas consumption may exist, pressure sensor monitoring is used to mix the pressure of gas tank, by result feedback to PLC, after being judged by PLC equally, the electromagnetic proportion regulating of carrier gas gas circuit is regulated, realizes stable this function of supply; Use the combination of PLC and electromagnetic proportion regulating, realize automatically controlling this function, be easy to use quick.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the present invention is not limited to following examples.The implementation condition adopted in embodiment can require to do further adjustment according to the concrete difference used, and not marked implementation condition is the condition in normal experiment.
Embodiment 1
This example provides a kind of gas mixer, gas mixer mainly comprises gas-holder and (comprises carrier gas reservoir and work gas storage tank, multiple gas transfer pipeline, be arranged on the reducing valve on each gas transfer pipeline, strainer, electromagnetic proportional valve and non-return valve, mixed gas tank, pressure transmitter, gas composition analysis instrument and PLC.Form from gas circuit, multiple gas transfer pipeline is divided into carrier gas gas circuit and work gas gas circuit, and wherein carrier gas gas circuit generally walks the higher gas of content in mixed gas, as nitrogen, air, carbonic acid gas etc.; Work gas gas circuit is taken a walk the lower gas of content in mixed gas, as sulfurous gas, sulfur hexafluoride etc.When needing multiple gases to mix, only need to increase corresponding gas circuit, structurally can take same mode.
In each gas circuit, from gas feed end, reducing valve, strainer, electromagnetic proportional valve, non-return valve set gradually, wherein reducing valve act as adjustments of gas pipeline original pressure; The minute solid particles impurity that may exist in strainer removing gas piping, protection electromagnetic proportional valve, recommends the gas filter adopting filter diameter to be less than 40 microns in this device; The size of flow in electromagnetic proportional valve pilot piping, the signal accepted from PLC drives; 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 transmitter is positioned at the top of mixed gas tank, and gas composition analysis instrument is arranged in the upper position of mixed gas tank, and mixed gas outlet is positioned at mixed gas tank top.Mixed gas tank should have certain volume, and concrete size is determined according to final gas usage.
Automatic control section, PLC accepts the signal of pressure transmitter and gas composition analysis instrument, controls the aperture of the electromagnetic proportional valve of corresponding gas circuit after computation program calculates.Such as, mixed gas tank pressure is greater than or less than set(ting)value, then the aperture controlling carrier gas gas circuit electromagnetic proportional valve reduces or increases.In fact, PLC is in Sustainable Control state for mixture pressure and composition.
Embodiment 2
In nothing sealing iron pot furnace, carry out the melting of magnesium alloy AZ31, smelting furnace is covered with a gas and passes into steel pipe, external diameter is 6mm, smelting furnace diameter 150mm, and height 250mm, is equipped with the AZ91D magnesium alloy that 3.5kg is dried in advance.Open heating by electric cooker switch, setting in-furnace temperature is 600 DEG C, when internal temperature reaches 400 DEG C, start to pass into protection gas, after magnesium alloy melts, setting in-furnace temperature 670 DEG C, now regulated composition and the consumption of protection gas by the gas mixer of embodiment 1, test its protected effect; Continue to heat up, measure the protected effect of smelting temperature at 720 DEG C, 760 DEG C respectively, concrete result data sees the following form:
The meaning (as follows) of abbreviation and symbology in upper table:
TFET-2,2,2-trifluoro sulfur alcohol is called for short;
N
2, 3-representing that use carrier gas is nitrogen, flow is 3L/min;
★-protected effect is excellent, and concrete judgment criteria is for opening upper cover, and take off the film of cleaved surface in atmosphere after, surface film can heal rapidly voluntarily, forms new film, without burning-point, and 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, and take off the film of cleaved surface in atmosphere after, surface film energy self-heal, forms new film, and without burning-point, have a small amount of oxidation sludge, the operating time can support more than 3min;
▲-protected effect is poor, and concrete judgment criteria is for opening upper cover, and take off the film of cleaved surface in atmosphere after, surface film energy indolence maybe can not heal, and burning-point appears in surface, and have more oxidation sludge, the operating time is within 3min;
Upper table experimental data illustrates, takes the fluorine-containing suppression gas that 2,2,2-trifluoro sulfur alcohol and itself and R134a, R125, R32 etc. form, the fusion process of energy available protecting magnesium alloy AZ31.
Embodiment 3
In nothing sealing iron pot furnace, carry out the melting of magnesium alloy AM50, other operation is identical with embodiment 2 with condition, and concrete result data sees the following form:
In upper table, experimental data illustrates, takes the fluorine-containing suppression gas that 2,2,2-trifluoro sulfur alcohol and itself and R134a, R125, R32 etc. form, the fusion process of energy available protecting magnesium alloy AM50.
Embodiment 4
In nothing sealing iron pot furnace, carry out the melting of pure magnesium, other operation is identical with embodiment 1 with condition, and concrete result data sees the following form:
In upper table, experimental data illustrates, takes the fluorine-containing suppression gas that 2,2,2-trifluoro sulfur alcohol and itself and R134a, R125, R32 etc. form, the fusion process of the pure magnesium of energy available protecting.
Comparative example 1
In nothing sealing iron pot furnace, carry out the melting of magnesium alloy AZ31, contrast pure R134a, R125 and R32 and mix the protected effect after TFET, concrete result data sees the following form:
As can be seen here, compared to pure R134a, R125 and R32, the fluorine-containing suppression gas after being mixed with TFET can protect the fusion process of magnesium alloy more effectively.
Above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed in protection scope of the present invention.
Claims (10)
1. an environmental-protection type magnesium alloy melting protection gas, comprises suppression gas and the carrier gas that can suppress Mg-based hydrogen storage that oxidizing fire occurs in fusion process, it is characterized in that: described suppression gas comprises 2,2,2-trifluoro sulfur alcohol.
2. environmental-protection type magnesium alloy melting protection gas according to claim 1, is characterized in that: the volume content of described suppression gas in described protection gas is 0.01% ~ 1%.
3. environmental-protection type magnesium alloy melting protection gas according to claim 2, is characterized in that: the volume content of described suppression gas in described protection gas is 0.1% ~ 0.5%.
4. the environmental-protection type magnesium alloy melting protection gas according to claim 1 or 2 or 3, is characterized in that: described suppression gas also comprises one or more the combination be selected from HFA 134a, pentafluoride ethane and methylene fluoride.
5. environmental-protection type magnesium alloy melting protection gas according to claim 4, is characterized in that: the volume content that described 2,2,2-trifluoro sulfur alcohols account for described suppression gas is 5 ~ 50%.
6. environmental-protection type magnesium alloy melting protection gas according to claim 5, is characterized in that: the volume content that described 2,2,2-trifluoro sulfur alcohols account for described suppression gas is 10 ~ 30%.
7. environmental-protection type magnesium alloy melting protection gas according to claim 1, is characterized in that: described carrier gas is one or more the combination be selected from dry air, carbonic acid gas, nitrogen, argon gas.
8. the preparation method of the environmental-protection type magnesium alloy melting protection gas any one of a claim 1-7 described in claim, it adopts gas mixer each component of composition protection gas to be mixed in proportion and obtains protecting gas, described gas mixer comprises mixed gas tank and multiple gas transfer pipeline, one end of described gas transfer pipeline is connected with gas-holder, the other end is connected with described mixed gas tank, it is characterized in that: described gas transfer pipeline is provided with reducing valve and electromagnetic proportional valve from a described end successively towards the direction of described the other end, described gas mixer also comprises and being connected with described mixed gas tank, for the gas composition analysis instrument analyzed the gas composition in described mixed gas tank and the PLC be connected with described gas composition analysis instrument, described electromagnetic proportional valve is connected with described PLC and controlled, described PLC receives the analytical results of described gas composition analysis instrument and carries out regulating the composition realizing accurately controlling mixed gas according to analytical results to the electromagnetic proportion regulating on corresponding gas transfer pipeline.
9. the method stoping Mg-based hydrogen storage that oxidizing fire occurs in fusion process; it is characterized in that: the surface of when Mg-based hydrogen storage melting, the environmental-protection type magnesium alloy melting protection gas described in claim any one of claim 1-7 being introduced molten metal; form fine and close protective membrane with the reactive magnesium under molten state, thus stop it that oxidizing fire occurs.
10.2,2,2-trifluoro sulfur alcohol protects the purposes of Mg-based hydrogen storage in Mg-based hydrogen storage melting.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107299241A (en) * | 2017-06-02 | 2017-10-27 | 青海盐湖工业股份有限公司 | The air supply system and Mg alloy smelting furnace of a kind 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107299241A (en) * | 2017-06-02 | 2017-10-27 | 青海盐湖工业股份有限公司 | The air supply system and Mg alloy smelting furnace of a kind of magnesium alloy smelting protective gas |
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| 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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