CN110106327A - A kind of composite antioxidant, hierarchical quenching oil and preparation method thereof - Google Patents
A kind of composite antioxidant, hierarchical quenching oil and preparation method thereof Download PDFInfo
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- CN110106327A CN110106327A CN201910354876.9A CN201910354876A CN110106327A CN 110106327 A CN110106327 A CN 110106327A CN 201910354876 A CN201910354876 A CN 201910354876A CN 110106327 A CN110106327 A CN 110106327A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
- C21D1/58—Oils
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Abstract
The application provides a kind of composite antioxidant, hierarchical quenching oil and preparation method thereof, wherein the composite antioxidant includes phenol antioxidant and amine antioxidants.The parts by weight of each component in the composite antioxidant are as follows: 3.4~6 parts by weight of phenol antioxidant；1.5~3.4 parts by weight of amine antioxidants；Wherein, 1 parts by weight are calculated as based on 1g.Antioxidant provided by the present application is applicable under hot conditions mainly for the preparation of hierarchical quenching oil, the hierarchical quenching oil, and use scope is 140~180 DEG C.When carrying out grade quench processing using the hierarchical quenching oil, amine antioxidants and phenol antioxidant synergistic effect, can capture the free radical in oil product, generate small molecule stable material, to prevent free radical from carrying out the build phase of chain, solve the problems, such as that oil product is easy aging.
Description
Technical field
This application involves antioxidant technology fields, and in particular to a kind of composite antioxidant, hierarchical quenching oil and its system
Preparation Method.
Background technique
In metal works manufacture field, hardenability and the good metal works of harden ability, usually used to quench in order to obtain
Oil is quenched metal works as hardening media.Quenching treatment is that the higher metal works of temperature are cooled to room temperature
Process, in the process, the temperature difference on metal works center portion and surface can make metal works center portion and surface generate heat to answer
Power, meanwhile, the temperature difference on metal works center portion and surface also results in the asynchronism of metal works center portion and surface phase transformation
And structural stress is generated, the superposition of thermal stress and structural stress constitutes the residual stress after quenching treatment, and residual stress can be led
Metal works are caused to generate deformation.
Deformation is generated in order to reduce the metal works after quenching treatment, metal works are carried out by the way of grade quench
Quenching treatment.Grade quench refers to cool down step by step for the higher metal works of temperature, for example, the metal for being 200 DEG C for temperature
Metal works are first cooled to 150 DEG C, then 150 DEG C of metal works are cooled to 100 DEG C by workpiece, according to the side to cool down step by step
Metal works are reduced to room temperature by formula.During quenching treatment at different levels, control quenching oil temperature and metal works it is initial
Temperature difference is in a lesser range, so that metal works center portion and the temperature difference on surface are unlikely to excessive, to reduce
The residual stress of metal works center portion and surface reduces the deformation of metal works.
The quenching oil for being applied to grade quench is known as hierarchical quenching oil, in the quenching process at different levels of grade quench, is needed
Hierarchical quenching oil is heated to different temperature, the initial temperature of hierarchical quenching oil and temperature and metal works is closer, then
Metal works center portion and the temperature difference on surface are smaller, and the deformation that metal works generate is smaller.But it is hydrocarbon in hierarchical quenching oil
Compound and non-hydrocarbon compound are easy to lose hydrogen atom, obtain free radical, and the oxygen in free radical and air occurs a series of anti-
Macromolecular stabilizer product should be generated, detailed process is as follows:
1. free radical generates:
RH→R·+H·
R·+O2→ROO·Or RO·
2. the growth of chain:
ROO·+RH→ROOH+R·
R·+O2→ROO·
ROOH→RO·+OH·
2ROOH→RO·+ROO·+H2O
3. end stopping of chain:
2ROO·
2R·
The temperature of hierarchical quenching oil is higher, so that the reaction rate of above-mentioned reaction is accelerated, i.e. the life of macromolecular stabilizer product
Accelerate at rate, since the molecular weight of macromolecular stabilizer product is larger, causes to generate precipitating or floating material in hierarchical quenching oil, from
And the quenching property of hierarchical quenching oil is reduced, this phenomenon is known as to " aging " phenomenon of hierarchical quenching oil.
In order to solve the problems, such as that hierarchical quenching oil is easy aging, antioxidant is usually added in hierarchical quenching oil, however,
Inventor has found that usually used antioxidant is not useful in hierarchical quenching oil in oil product in the research process of the application
In, or even there are also opposite negative effects, therefore, developing suitable for the antioxidant of hierarchical quenching oil is current urgent need to resolve
The problem of.
Summary of the invention
The application provides a kind of composite antioxidant, hierarchical quenching oil and preparation method thereof, traditional anti-oxidant to solve
Agent is not particularly suited for the problem of hierarchical quenching oil.
The application's in a first aspect, provides a kind of composite antioxidant, including phenol antioxidant and amine antioxidants.
Optionally, in the composite antioxidant each component parts by weight are as follows: 3.4~6 parts by weight of phenol antioxidant；Amine
1.5~3.4 parts by weight of class antioxidant；Wherein, 1 parts by weight are calculated as based on 1g.
Optionally, the phenol antioxidant includes the component of following weight proportion: simple phenol antioxidant 2.4~5
Parts by weight；1~1.2 parts by weight of phenolic ester class antioxidant；Wherein, 1 parts by weight, the simple phenol antioxidant are calculated as based on 1g
For BHT or BHA.
Optionally, the amine antioxidants is diphenylamine antioxidant.
The second aspect of the application provides compound anti-provided by a kind of any one possible implementation of first aspect
The preparation method of oxidant, comprising: phenol antioxidant is heated to 60~80 DEG C；It is added under 60~80 DEG C of whipping temp
Amine antioxidants continues to stir evenly up to composite antioxidant.
The third aspect of the application, provides a kind of hierarchical quenching oil, and the hierarchical quenching oil includes following weight proportion
Component: 600~900 parts by weight of refined paraffin wax base base oil；5~10 parts by weight of composite antioxidant；60~90 weight of additive
Part；Wherein, 1 parts by weight are calculated as based on 1g；The composite antioxidant is mentioned by any one implementation of the application second aspect
The preparation method of confession is prepared.
Optionally, the additive includes urging cryogen, brightener, antirust agent and dispersing agent；Each component in the additive
Parts by weight are as follows: urge 30~40 parts by weight of cryogen；20~30 parts by weight of brightener；5~10 parts by weight of antirust agent；Dispersing agent 5~
10 parts by weight；Wherein, 1 parts by weight are calculated as based on 1g.
The fourth aspect of the application provides a kind of provided be classified of any one possible implementation of the third aspect and quenches
The preparation method of kerosene, comprising: refined paraffin wax base base oil is heated to 60~80 DEG C；Add under 60~80 DEG C of whipping temp
Enter composite antioxidant and additive, continues 3~4h of stirring up to hierarchical quenching oil.
The application provides a kind of composite antioxidant, hierarchical quenching oil and preparation method thereof, wherein the compound anti-oxidation
Agent includes phenol antioxidant and amine antioxidants.The parts by weight of each component in the composite antioxidant are as follows: phenols antioxygen
3.4~6 parts by weight of agent；1.5~3.4 parts by weight of amine antioxidants；Wherein, 1 parts by weight are calculated as based on 1g.The application provides
Antioxidant mainly for the preparation of hierarchical quenching oil, which is applicable under hot conditions, use scope 140
~180 DEG C.When carrying out grade quench processing using the hierarchical quenching oil, amine antioxidants and phenol antioxidant collaboration are made
With, it can capture the free radical in oil product, generate small molecule stable material, so that free radical is prevented to enter the build phase of chain,
Solve the problems, such as that oil product is easy aging.
Specific embodiment
The application is described in detail below.
The application provides a kind of composite antioxidant, including phenol antioxidant and amine antioxidants.
There are mainly two types of the mechanisms of action of antioxidant, the first is chain termination type, and second is prevention type.Wherein, chain
The mechanism of action of termination type antioxidant is so that free radical is lost activity in such a way that addition, electronics are given or hydrogen is given, is kept away
Exempt from the build phase that free radical enters chain；The mechanism of action for preventing type antioxidant is the generation source for removing free radical, inhibits
Or delay to cause the reaction that free radical generates.
Phenol antioxidant and amine antioxidants are chain termination type antioxidant, the phenolic hydroxyl group of phenol antioxidant or
Hydrogen atom can be combined with free radical in the amido of person's amine antioxidants, generate small molecule stable product, to prevent certainly
The build phase for entering chain by base prevents from generating macromolecule polyalcohol.
When there are when a variety of antioxidants, generally produce two kinds of effects between various antioxidants in same system: collaboration
Effect and anti-synergistic effect, present inventor pass through lot of experiments, final choice go out two kinds of phenol antioxidant and
A kind of amine antioxidants is compounded, and between the various antioxidants in composite antioxidant made of compounding there is collaboration to make
With, so that the antioxidant effect of composite antioxidant is greater than the antioxidant effect of any single antioxidant, so that
Hierarchical quenching oil using composite antioxidant preparation has better antioxidant effect.
Composite antioxidant provided by the present application is applicable under hot conditions, and high temperature described herein is 140 DEG C~180
DEG C, since under the condition of high temperature, phenol antioxidant and antioxygenic property are weaker than amine antioxidants, therefore amine antioxidants rises
To oxidation resistant effect, specifically: amine antioxidants can capture free radical, and redox reaction occurs with free radical, so that
Free radical generates stable material in conjunction with the hydrogen atom in amine antioxidants；Meanwhile phenol antioxidant can with lose hydrogen
Amine antioxidants after atom combines, and provides hydrogen atom to lose the amine antioxidants after hydrogen atom, that is to say, that system
In amine antioxidants consumption while can be constantly regenerating, regenerated amine antioxidants can combine again with free radical,
To have the function that collaboration.
Optionally, in the composite antioxidant each component parts by weight are as follows: 3.4~6 parts by weight of phenol antioxidant；Amine
1.5~3.4 parts by weight of class antioxidant；Wherein, 1 parts by weight are calculated as based on 1g.
In the application, phenol antioxidant is mainly used for lose the amine antioxidants of hydrogen atom and providing hydrogen atom, because
The additive amount of this phenol antioxidant is more than the additive amount of amine antioxidants, and still, the additive amount of phenol antioxidant is unsuitable
Excessively, if the additive amount of phenol antioxidant is more than four times of amine antioxidants, lead to the dense of phenol antioxidant in system
Height is spent, then will affect the antioxygenic property of amine antioxidants.
Optionally, the phenol antioxidant includes the component of following weight proportion: simple phenol antioxidant 2.4~5
Parts by weight；1~1.2 parts by weight of phenolic ester class antioxidant；Wherein, 1 parts by weight are calculated as based on 1g；The simple phenol antioxidant
For BHT or BHA.
BHA (butylated hydroxy anisole) and BHT (2,6 di tert butyl 4 methyl phenol) is that common phenols is anti-oxidant
Agent, wherein BHT is the excellent antioxidant agent of various oils products, when BHT is used alone as single antioxidant, work temperature
For degree at 100 degree, antioxidant effect is best.In this application, BHT or BHA is as a component in composite antioxidant, with
Amine antioxidants synergistic effect, has better antioxidant effect.
Phenolic ester class antioxidant is made of phenol ester type compound, and the high-temperature oxidation resistance of phenolic ester class antioxidant is excellent
Different, dissolubility is good in mineral oil and esters base oil, and is compounded with synergistic effect with arylamine class antioxygen China agent.
In the application, the additive amount of phenolic ester class antioxidant is excessive or very few will affect the anti-oxidant of composite antioxidant
Performance.
Optionally, the amine antioxidants is diphenylamine antioxidant.It is suitable that diphenylamine antioxidant belongs to high temperature
Ashless type antioxidant, and such antioxidant does not have the elements such as sulphur, phosphorus, it is small to oil pollution.
In the application, the composite antioxidant is prepared by method comprising the following steps:
Step 1-1；Phenol antioxidant is heated to 60~80 DEG C；
Step 2-1；Amine antioxidants is added under 60~80 DEG C of whipping temp, continues to stir evenly to get compound
Antioxidant.
When preparing composite antioxidant, temperature is too low or too low, is unfavorable for the dissolution of all kinds of antioxidants.
The application also provides a kind of hierarchical quenching oil, and the hierarchical quenching oil includes the component of following weight proportion: purification
600~900 parts by weight of paraffin base oil；5~10 parts by weight of composite antioxidant；60~90 parts by weight of additive；Wherein, base
1 parts by weight are calculated as in 1g.
Present inventor it has been investigated that, the saturation degree of base oil and the aging of hierarchical quenching oil are related, if basic
It include unsaturated bond in oil, the stability of unsaturated bond is lower, then is subject to attack and generate free radicals.To make grade quench
The stability of oil is higher, and the application prepares hierarchical quenching oil using refined paraffin wax base base oil, and refined paraffin wax base base oil is full
And hydro carbons, therefore high stability, it is not subject to attack and generate free radicals, that is to say, that use refined paraffin wax base base oil
The yield of the hierarchical quenching oil of preparation, free radical is less, then precipitates and reduce as made of free radical polymerization, to effectively inhibit
The aging of hierarchical quenching oil.
In the application, the additive amount of composite antioxidant is too low, and antioxygenic property is lower, then does not have the effect for inhibiting aging
Fruit；But the additive amount of composite antioxidant is also unsuitable excessively high, if the adding too much of composite antioxidant, may cause point
The viscosity of grade quenching oil is excessive, influences the mobility of hierarchical quenching oil.
Optionally, the additive includes urging cryogen, brightener, antirust agent and dispersing agent；Each component in the additive
Parts by weight are as follows: urge 30~40 parts by weight of cryogen；20~30 parts by weight of brightener；5~10 parts by weight of antirust agent；Dispersing agent 5~
10 parts by weight；Wherein, 1 parts by weight are calculated as based on 1g.
It urges cryogen to can be improved the High-temperature cooling ability of hierarchical quenching oil, and can be improved the thermal stability of hierarchical quenching oil
And thermal oxidation stability.Urge the additive amount of cryogen in 30~40 parts by weight, the High-temperature cooling ability of hierarchical quenching oil is moderate, no
As for cooling too fast or too slow.
The effect of brightener be mainly manifested in by active surface remove rest on surface of workpiece greasy dirt, oxidation and
Unoxidized impurity keeps cleaning, glossiness and the color fastness of surface of workpiece.Brightener additive amount is very few, metal works
The impurity elimination effect on surface is poor.
Antirust agent can prevent metal works from getting rusty, and the additive amount of antirust agent is excessive or very few will affect rust-proof effect.
Component one of of the dispersing agent as additive uniform can disperse those and be insoluble in the component of liquid, while can also prevent
The only sedimentation and cohesion of particle, promotes mixed system to form stable suspension.The additive amount of dispersing agent is very few, influences dispersion effect
Fruit；The additive amount of dispersing agent is excessive, so that mixed system excessively disperses, is then easy to cause viscosity or adhesive force of mixed system etc.
Sharply decline, influences using effect.
In the application, the hierarchical quenching oil is prepared by method comprising the following steps:
Step 2-1；Refined paraffin wax base base oil is heated to 60~80 DEG C；
Step 2-1；Composite antioxidant and additive are added under 60~80 DEG C of whipping temp, continues 3~4h of stirring
Up to hierarchical quenching oil.
The application is further described with reference to embodiments.
Composite antioxidant provided by the present application is mainly for the preparation of hierarchical quenching oil, the antioxygenic property of composite antioxidant
It is embodied on the antioxygenic property of hierarchical quenching oil.In industrial application, oil product acid value in use is usually detected
Variation, acid value is the index for indicating the amount in oil product containing acidic materials, can use and neutralizes every gram of oil product middle acid substance institute
The milligram number of potassium hydroxide is needed to indicate.As oil product uses the extension of time, acid value is increasing, illustrates acid in oil product
Matter is more and more, after reaching a certain limit value, the variation of increasing speed of acid value, it may be possible to which the free radical in system enters chain
Build phase, so that oil product accelerated ageing, therefore, acid value can illustrate that oil product enters the ageing step after reaching the limit value,
Acid value can illustrate that oil product is weathered when being higher than the limit value, for example, limit value can be set as 1.5mgKOH/g, once it is sour
Value can illustrate oil product aging more than 1.5mgKOH/g.
It in the application, is tested using multiple embodiment and comparative examples, experimental method is as follows: preparing a variety of different components
The composite antioxidant of content is prepared a variety of quenching oils using composite antioxidant, is quenched using hierarchical quenching oil
Experiment detects hierarchical quenching oil in the different acid values using time point.
The proportion of each component is as shown in Table 1 in each embodiment and comparative example:
The proportion of one each component of table
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| BHA | 2.4g | - | - | - | 1.2g |
| BHT | - | 5 | 4 | - | - |
| Phenolic ester class antioxidant | 1.2 | 1 | 1.1 | - | 1 |
| Diphenylamine antioxidant | 1.5 | 3.4 | 2.5 | 3.4 | 3.4 |
| Refined paraffin wax base base oil | 600 | 900 | 800 | 900 | 900 |
| Urge cryogen | 30 | 40 | 35 | 40 | 40 |
| Brightener | 20 | 30 | 25 | 30 | 30 |
| Antirust agent | 5 | 10 | 8 | 10 | 10 |
| Dispersing agent | 5 | 10 | 8 | 10 | 10 |
The experimental result of each embodiment and comparative example is as shown in Table 2:
The experimental result of each embodiment and comparative example of table two
It can be seen from table two 180 DEG C at use temperature, embodiment one, embodiment two and embodiment three are within 72h
Acid value is normal, aging phenomenon does not occur.Single diphenylamine antioxidant is used only in comparative example one, when using 72h, oil
The acid value of product has reached 1.53mgKOH/g, illustrates that quenching oil has generated aging phenomenon, comparative example one and embodiment two at this time
It is better than single diphenylamine antioxidant compared to the antioxygenic property that can be seen that composite antioxidant provided by the present application
Antioxygenic property.The additive amount of phenol antioxidant is less in comparative example two, and when using 72h, the acid value of oil product is had reached
1.4mgKOH/g illustrates that oil product is close to aging at this time, and comparative example two is compared with embodiment two can be seen that phenol antioxidant
Additive amount is very few, influences the antioxygenic property of oil product.
Combine detailed description and exemplary example that the application is described in detail above, but these explanations are simultaneously
It should not be understood as the limitation to the application.It will be appreciated by those skilled in the art that without departing from the application spirit and scope,
A variety of equivalent substitution, modification or improvements can be carried out to technical scheme and embodiments thereof, these each fall within the application
In the range of.The protection scope of the application is determined by the appended claims.
Claims (8)
1. a kind of composite antioxidant, which is characterized in that including phenol antioxidant and amine antioxidants.
2. composite antioxidant according to claim 1, which is characterized in that the weight of each component in the composite antioxidant
Measure part are as follows:
3.4~6 parts by weight of phenol antioxidant；
1.5~3.4 parts by weight of amine antioxidants；
Wherein, 1 parts by weight are calculated as based on 1g.
3. composite antioxidant according to claim 1, which is characterized in that the phenol antioxidant includes following weight
The component of proportion:
2.4~5 parts by weight of simple phenol antioxidant；
1~1.2 parts by weight of phenolic ester class antioxidant；
Wherein, 1 parts by weight are calculated as based on 1g；
The simple phenol antioxidant is BHT or BHA.
4. composite antioxidant according to claim 1, which is characterized in that the amine antioxidants is anti-for diphenylamine
Oxidant.
5. a kind of preparation method of the composite antioxidant as described in any one of Claims 1 to 4 characterized by comprising
Phenol antioxidant is heated to 60~80 DEG C；
Amine antioxidants is added under 60~80 DEG C of whipping temp, continues to stir evenly up to composite antioxidant.
6. a kind of hierarchical quenching oil, which is characterized in that the hierarchical quenching oil includes the component of following weight proportion:
600~900 parts by weight of refined paraffin wax base base oil；
5~10 parts by weight of composite antioxidant；
60~90 parts by weight of additive；
Wherein, 1 parts by weight are calculated as based on 1g；
Composite antioxidant preparation method described in claim 5 is prepared.
7. hierarchical quenching oil according to claim 6, which is characterized in that the additive includes urging cryogen, brightener, preventing
Become rusty agent and dispersing agent；
The parts by weight of each component in the additive are as follows:
Wherein, 1 parts by weight are calculated as based on 1g.
8. a kind of preparation method of hierarchical quenching oil as claimed in claims 6 or 7 characterized by comprising
Refined paraffin wax base base oil is heated to 60~80 DEG C；
Composite antioxidant and additive are added under 60~80 DEG C of whipping temp, continues 3~4h of stirring up to grade quench
Oil.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061693A (en) * | 2021-03-19 | 2021-07-02 | 广东剑鑫科技股份有限公司 | Rapid and stable overspeed bright quenching oil and preparation method thereof |
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Application publication date: 20190809 |