CN109880668A - The preparation method of extreme pressure anti-wear additives and the application in total synthesis water-base shaping dope - Google Patents
The preparation method of extreme pressure anti-wear additives and the application in total synthesis water-base shaping dope Download PDFInfo
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Abstract
The invention discloses the preparation method of extreme pressure anti-wear additives and the applications in total synthesis water-base shaping dope, are related to metal forming lubricant field, including following weight percentage components: including following weight percentage components: basal liquid 70%~85%；Oiliness improver 10%~19%；Extreme pressure anti-wear additives 2.3~8%；Antirust agent 2~8.7%.Weigh the graphene oxide compound that water glycol mixed liquor, water soluble polyether, benzotriazole, phthalocyanine lanthanum are modified；Weighed water glycol mixed liquor is put into stirred autoclave, and water soluble polyether is added, heating water bath stops heating to 60 DEG C and after being stirred continuously to solution clear homogeneous in kettle；The graphene oxide compound of benzotriazole, the modification of phthalocyanine lanthanum is sequentially added into obtained solution, often plus a kind of component need to be stirred to a kind of lower reagent is added after mixing, and all components are stirred for 10~30 minutes to after mixing up to total synthesis water-base shaping dope after the completion of being added.
Description
Technical field
The present invention relates to the preparation method of metal forming lubricant field more particularly to extreme pressure anti-wear additives and fully synthetic
Application in water base shaping dope.
Background technique
Water-based metal working fluid is since the forties in last century comes out, due to the cooling performance to hardly match with oil-base fluid
And cheap cost is caused original oil base metal working fluid gradually to be processed by water-base metal by the extensive concern in market
Liquid (especially fully synthetic type water-based metal working fluid) substitution.
Water-based metal working fluid has been passed by western developed country and has been sent out from emulsion to Synthesis liquid, again to microemulsion
The process of exhibition, and microemulsion has obtained unprecedented development and application.In China, metal working fluid is at present still with cream
Change based on liquid, manufacturing enterprise occurs the upsurge of development and production and application Synthesis liquid in the eighties in last century, but up to the present
Emulsion still occupies the biggish market share.
With the continual development of Chinese national economy, auto industry and its attached mating industry obtain hair at full speed
Exhibition, mechanical industry have obtained tremendous development.Currently, China has become demand maximum, while the area that demand growth is most fast.Entirely
Synthesis water base lubricant is also constantly expanding in the application range of field of machining, especially applies most in water base lubricant
The requirement of wide metal working fluid is higher and higher.Due to the enhancing that worldwide energy shortage problem and conservation of natural environment are realized,
Fully synthetic type water-based metal working fluid has technology and application advantage more and more prominent.And advanced manufacturing technology is continuous deep
The development entered, existing metal working fluid has been unable to meet wanting for higher and higher intermetallic composite coating level and green manufacturing in the market
It asks, therefore the requirement of more Gao Gengxin is proposed to fully synthetic type water-based metal working fluid and its formula composition.This will be pushed entirely
Synthesis type water-based metal working fluid market is to more high-end development.In addition, the fully synthetic type water-based metal working fluid continued to develop is not
But it is required that its additive has more efficient antirust and greasy property, and under the conditions of certain special operation conditions, also require additive
With the properties such as hard water resistance.Therefore, release a existing greasy property on the market has rustless property and more excellent again
The multi-functional total synthesis water-base metal working fluid that property requires has certain positive effect.
Since traditional extreme pressure anti-wear additives face various environmental issues, and exist it is multi-functional poor, anti-oxidant, anti-detergency with
And repair function it is weak the deficiencies of, more sight are invested rare earth and its compound by people in recent years.Rare earth is scandium, yttrium, lanthanum
It is the general name of totally 17 elements, as a kind of novel nonactive extreme-pressure anti-friction additive, with it with unique 4f electronics knot
Structure, chemical activity are strong, electronegativity is low, atomic radius is big, after ionization atomic radius it is small, friction surface fusing point is low, many rare earths
Compound has the properties such as hexagonal crystallographic texture system layer structure, is more and more paid attention to by people.Due to its not with metal
It chemically reacts, because having like that friction pair material rather than traditional extreme-pressure anti-friction additive (containing elements such as P, S, Cl)
Corrosivity and selectivity, do not impact environment, meet requirement of the environmental protection to metal forming Development of Additives, attract me
Be applied in water-base metal shaping dope.
Summary of the invention
The invention proposes the preparation method of extreme pressure anti-wear additives and the applications in total synthesis water-base shaping dope.
To achieve the goals above, present invention employs following technical solutions:
A kind of preparation method of antiwear additive, includes the following steps,
(1) preparation of the DMF uniform dispersion of Carboxylation graphene oxide:
Graphene oxide uniform dispersion is taken, hydrobromic acid is added, is vigorously stirred 8-15h at room temperature, second is being added
Diacid, the reaction was continued 3-5h, adjusting Ph value to neutrality, then with DMF adjusting concentration, continuous ultrasound dispersion 20-30h, obtained carboxylic
It is acidified the DMF uniform dispersion of graphene oxide.
(2) the graphene oxide compound of phthalocyanine lanthanum modification
DMF uniform dispersion, tetramino phthalocyanine lanthanum EDC, the DMAP for taking Carboxylation graphene oxide are protected in vacuum nitrogen
Under conditions of heat 80-99 DEG C, react 45-55h, cooling centrifuge washing obtains the graphene oxide compound of phthalocyanine lanthanum modification,
Up to antiwear additive.
Further, the concentration of the graphene oxide in the step (1) is 1mg/mL.
Further, it after the step (1) the reaction was continued 3-5h, is washed with deionized to neutrality.
Further, the step (1) is 1mg/mL with DMF wiring solution-forming concentration.
Further, the EDC is 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride.
Further, the DMAP is 4-dimethylaminopyridine.
A kind of total synthesis water-base shaping dope adding extreme pressure anti-wear additives, including following weight percentage components:
Basal liquid 70%~85%；
Oiliness improver 10%~19%；
Extreme pressure anti-wear additives 2.3~8%；
Antirust agent 2~8.7%.
Further, the basal liquid is water glycol mixed liquor.
Further, the oiliness improver is water soluble polyether.
Further, the antirust agent is benzotriazole.
A kind of preparation method of total synthesis water-base shaping dope, comprising the following steps:
(1) it is multiple that water glycol mixed liquor, water soluble polyether, benzotriazole, the graphene oxide of phthalocyanine lanthanum modification are weighed
Close object；
(2) the weighed water glycol mixed liquor of step (1) is put into stirred autoclave, and water soluble polyether is added, water
Bath stops heating after being heated to 60 DEG C and being stirred continuously to solution clear homogeneous in kettle；
(3) it is compound that benzotriazole, the graphene oxide of phthalocyanine lanthanum modification are sequentially added in the solution obtained to step (2)
Object, often plus a kind of component need to be stirred to a kind of lower reagent is added after mixing, and all components are stirred for 10 after the completion of being added
~30 minutes to after mixing up to total synthesis water-base shaping dope.
Usefulness: this environmentally protective extreme-pressure anti-wear multifunction additive, preferably existing funcitonal rust-proof agent, friction improver etc.
The fully synthetic type water-based metal working fluid that multiple functions additive is modulated through careful balance assessment.With excellent anti-corrosion, prevent
Performance of becoming rusty and abrasion resistance, good biodegradability.The fully synthetic type water-based metal working fluid has good wear-resistant
The performances such as property, antirust, anticorrosion.Product quality is in the leading level in the world, can be the life of internal lube oil after product is gone into operation
Produce provide high-quality fully synthetic type water-based metal working fluid, and will greatly push metal working fluid industry to environment compatibility,
Biological degradability, reproducibility direction develop energy.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.
Embodiment 1:
A kind of preparation method of antiwear additive, includes the following steps,
(1) preparation of the DMF uniform dispersion of Carboxylation graphene oxide:
1mg/mL graphene oxide uniform dispersion is taken, hydrobromic acid is added, is vigorously stirred 8h at room temperature, is being added
Ethanedioic acid, the reaction was continued 3h are washed with deionized to neutrality, are then 1mg/mL, continuous ultrasound with DMF wiring solution-forming concentration
Disperse 20h, the DMF uniform dispersion of Carboxylation graphene oxide is made.
(2) the graphene oxide compound of phthalocyanine lanthanum modification
DMF uniform dispersion, tetramino phthalocyanine lanthanum EDC, the DMAP for taking Carboxylation graphene oxide are protected in vacuum nitrogen
Under conditions of heat 80 DEG C, react 45h, cooling centrifuge washing obtains the graphene oxide compound of phthalocyanine lanthanum modification to get anti-
Grinding agent.
The EDC is 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride.The DMAP is 4- dimethylamino
Pyridine.
Embodiment 2:
A kind of preparation method of antiwear additive, includes the following steps,
(1) preparation of the DMF uniform dispersion of Carboxylation graphene oxide:
1mg/mL graphene oxide uniform dispersion is taken, hydrobromic acid is added, is vigorously stirred 15h at room temperature, is adding
Enter ethanedioic acid, the reaction was continued 5h is washed with deionized to neutrality, is then 1mg/mL with DMF wiring solution-forming concentration, continuous super
Sound disperses 30h, and the DMF uniform dispersion of Carboxylation graphene oxide is made.
(2) the graphene oxide compound of phthalocyanine lanthanum modification
DMF uniform dispersion, tetramino phthalocyanine lanthanum EDC, the DMAP for taking Carboxylation graphene oxide are protected in vacuum nitrogen
Under conditions of heat 99 DEG C, react 55h, cooling centrifuge washing obtains the graphene oxide compound of phthalocyanine lanthanum modification to get anti-
Grinding agent.
The EDC is 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride.The DMAP is 4- dimethylamino
Pyridine.
Embodiment 3:
A kind of preparation method of antiwear additive, includes the following steps,
(1) preparation of the DMF uniform dispersion of Carboxylation graphene oxide:
1mg/mL graphene oxide uniform dispersion is taken, hydrobromic acid is added, is vigorously stirred 12h at room temperature, is adding
Enter ethanedioic acid, the reaction was continued 4h is washed with deionized to neutrality, is then 1mg/mL with DMF wiring solution-forming concentration, continuous super
Sound disperses for 24 hours, the DMF uniform dispersion of Carboxylation graphene oxide to be made.
(2) the graphene oxide compound of phthalocyanine lanthanum modification
DMF uniform dispersion, tetramino phthalocyanine lanthanum EDC, the DMAP for taking Carboxylation graphene oxide are protected in vacuum nitrogen
Under conditions of heat 90 DEG C, react 48h, cooling centrifuge washing obtains the graphene oxide compound of phthalocyanine lanthanum modification to get anti-
Grinding agent.
The EDC is 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride.The DMAP is 4- dimethylamino
Pyridine.
Embodiment 4:
On the basis of embodiment 1: a kind of total synthesis water-base shaping dope adding extreme pressure anti-wear additives, including following weight hundred
Divide the component of ratio: water glycol mixed liquor 70%；Water soluble polyether 19%；Extreme pressure anti-wear additives 5.4%；Benzotriazole 5.6%.
Embodiment 5:
On the basis of embodiment 2: a kind of total synthesis water-base shaping dope adding extreme pressure anti-wear additives, including following weight hundred
Divide the component of ratio: water glycol mixed liquor 85%；Water soluble polyether 10%；Extreme pressure anti-wear additives 2.3%；Benzotriazole 2.7%.
Embodiment 6:
On the basis of embodiment 3: a kind of total synthesis water-base shaping dope adding extreme pressure anti-wear additives, including following weight hundred
Divide the component of ratio: water glycol mixed liquor 76%；Water soluble polyether 15%；Extreme pressure anti-wear additives 5.3%；Benzotriazole 2.7%.
Embodiment 7:
On the basis of embodiment 4, a kind of preparation method of total synthesis water-base shaping dope, comprising the following steps:
(1) it is multiple that water glycol mixed liquor, water soluble polyether, benzotriazole, the graphene oxide of phthalocyanine lanthanum modification are weighed
Close object；
(2) the weighed water glycol mixed liquor of step (1) is put into stirred autoclave, and water soluble polyether is added, water
Bath stops heating after being heated to 50 DEG C and being stirred continuously to solution clear homogeneous in kettle；
(3) it is compound that benzotriazole, the graphene oxide of phthalocyanine lanthanum modification are sequentially added in the solution obtained to step (2)
Object, often plus a kind of component need to be stirred to a kind of lower reagent is added after mixing, and all components are stirred for 10 after the completion of being added
Minute is to after mixing up to total synthesis water-base shaping dope.
Embodiment 8:
On the basis of embodiment 5, a kind of preparation method of total synthesis water-base shaping dope, comprising the following steps:
(1) it is multiple that water glycol mixed liquor, water soluble polyether, benzotriazole, the graphene oxide of phthalocyanine lanthanum modification are weighed
Close object；
(2) the weighed water glycol mixed liquor of step (1) is put into stirred autoclave, and water soluble polyether is added, water
Bath stops heating after being heated to 100 DEG C and being stirred continuously to solution clear homogeneous in kettle；
(3) it is compound that benzotriazole, the graphene oxide of phthalocyanine lanthanum modification are sequentially added in the solution obtained to step (2)
Object, often plus a kind of component need to be stirred to a kind of lower reagent is added after mixing, and all components are stirred for 30 after the completion of being added
Minute is to after mixing up to total synthesis water-base shaping dope.
Embodiment 9:
On the basis of embodiment 6, a kind of preparation method of total synthesis water-base shaping dope, comprising the following steps:
(1) it is multiple that water glycol mixed liquor, water soluble polyether, benzotriazole, the graphene oxide of phthalocyanine lanthanum modification are weighed
Close object；
(2) the weighed water glycol mixed liquor of step (1) is put into stirred autoclave, and water soluble polyether is added, water
Bath stops heating after being heated to 60 DEG C and being stirred continuously to solution clear homogeneous in kettle；
(3) it is compound that benzotriazole, the graphene oxide of phthalocyanine lanthanum modification are sequentially added in the solution obtained to step (2)
Object, often plus a kind of component need to be stirred to a kind of lower reagent is added after mixing, and all components are stirred for 19 after the completion of being added
Minute is to after mixing up to total synthesis water-base shaping dope.
The detection of load and maximum nonseizure load is sintered to the obtained total synthesis water-base shaping dope of embodiment 9,
And result is compared with commercial product, table specific as follows.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of antiwear additive, it is characterised in that: the following steps are included:
(1) preparation of the DMF uniform dispersion of Carboxylation graphene oxide:
Graphene oxide uniform dispersion is taken, hydrobromic acid is added, is vigorously stirred 8-15h at room temperature, ethanedioic acid is being added,
The reaction was continued 3-5h adjusts Ph value to neutrality, then adjusts concentration with DMF, continuous ultrasound disperses 20-30h, Carboxylation oxygen is made
The DMF uniform dispersion of graphite alkene.
(2) the graphene oxide compound of phthalocyanine lanthanum modification
DMF uniform dispersion, tetramino phthalocyanine lanthanum EDC, DMAP for taking Carboxylation graphene oxide, in the item of vacuum nitrogen protection
Heat 80-99 DEG C under part, react 45-55h, cooling centrifuge washing, obtain the graphene oxide compound of phthalocyanine lanthanum modification to get
Antiwear additive.
2. a kind of preparation method of antiwear additive according to claim 1, which is characterized in that the oxidation in the step (1)
The concentration of graphene is 1mg/mL.
3. a kind of preparation method of antiwear additive according to claim 1, which is characterized in that the reaction was continued for the step (1)
After 3-5h, it is washed with deionized to neutrality.
4. a kind of preparation method of antiwear additive according to claim 1, which is characterized in that the step (1) is made into DMF
Solution concentration is 1mg/mL.
5. the total synthesis water-base shaping dope of extreme pressure anti-wear additives described in any one, feature in a kind of addition claim 1-4
It is: including following weight percentage components:
Basal liquid 70%~85%；
Oiliness improver 10%~19%；
Extreme pressure anti-wear additives 2.3~8%；
Antirust agent 2~8.7%.
6. a kind of total synthesis water-base shaping dope according to claim 5, which is characterized in that the basal liquid is water glycol
Mixed liquor.
7. a kind of total synthesis water-base shaping dope according to claim 6, which is characterized in that the oiliness improver is water-soluble poly
Ether.
8. a kind of total synthesis water-base shaping dope according to claim 7, which is characterized in that the antirust agent is three nitrogen of benzo
Azoles.
9. a kind of preparation method of total synthesis water-base shaping dope as claimed in claim 8, it is characterised in that: including following step
It is rapid:
(1) the graphene oxide compound that water glycol mixed liquor, water soluble polyether, benzotriazole, phthalocyanine lanthanum are modified is weighed；
(2) the weighed water glycol mixed liquor of step (1) is put into stirred autoclave, and water soluble polyether is added, water-bath adds
Heat stops heating to 60 DEG C and after being stirred continuously to solution clear homogeneous in kettle；
(3) the graphene oxide compound of benzotriazole, the modification of phthalocyanine lanthanum is sequentially added in the solution obtained to step (2),
Often plus a kind of component need to be stirred to a kind of lower reagent is added after mixing, and all components are stirred for 10~30 after the completion of being added
Minute is to after mixing up to total synthesis water-base shaping dope.
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Application publication date: 20190614 |