CN114196459A - Dry film lubricant, preparation method and application thereof - Google Patents

Dry film lubricant, preparation method and application thereof Download PDF

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Publication number
CN114196459A
CN114196459A CN202111573340.XA CN202111573340A CN114196459A CN 114196459 A CN114196459 A CN 114196459A CN 202111573340 A CN202111573340 A CN 202111573340A CN 114196459 A CN114196459 A CN 114196459A
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dry film
parts
film lubricant
silicate
titanium alloy
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CN114196459B (en
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周峰
于波
张丽慧
于强亮
杨武芳
马正峰
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M167/00Lubricating compositions characterised by the additive being a mixture of a macromolecular compound, a non-macromolecular compound and a compound of unknown or incompletely defined constitution, each of these compounds being essential
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21FWORKING OR PROCESSING OF METAL WIRE
    • B21F5/00Upsetting wire or pressing operations affecting the wire cross-section
    • B21F5/005Upsetting wire
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/041Carbon; Graphite; Carbon black
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/061Carbides; Hydrides; Nitrides
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/102Silicates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/105Silica
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/022Ethene
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08Resistance to extreme temperature
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/64Environmental friendly compositions
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/20Metal working
    • C10N2040/24Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Lubricants (AREA)

Abstract

The invention provides a dry film lubricant, a preparation method and application thereof, and relates to the technical field of lubricating coatings. The dry film lubricant provided by the invention comprises the following preparation raw materials in parts by weight: 10.0-30.0 parts of silicate, 5.0-10.0 parts of silica sol, 1.0-5.0 parts of polyethylene emulsion, 10.0-50.0 parts of graphite, 7.5-20.0 parts of boron nitride, 0.1-1.0 part of silicone oil, 40.0-60.0 parts of water and 0.50-2.50 parts of auxiliary agent. When the dry film lubricant provided by the invention is used as a continuous warm-heading lubricating coating of a titanium alloy wire, the dry film lubricant has excellent temperature resistance, good adhesive force and environmental friendliness on the premise of having a low friction coefficient.

Description

Dry film lubricant, preparation method and application thereof
Technical Field
The invention relates to the technical field of lubricating coatings, in particular to a dry film lubricant and a preparation method and application thereof.
Background
With the rapid development of aerospace industry and the continuous improvement of the performance requirements of aircrafts in China, the demand of titanium alloy fasteners for aerospace is continuously increased, and the requirements on the comprehensive performance of the titanium alloy fasteners are higher and higher. Upsetting is one of important processes for forming fasteners, and in order to improve the production efficiency of titanium alloy fasteners in China and guarantee the quality stability, multiple fastener production units in China import continuous warm upsetting fastener processing equipment from abroad. The equipment of the type can exert the advantages only by using large single-weight disc round wire materials as raw materials for upsetting fasteners, and the purpose of efficient and stable production is achieved.
However, due to the upsetting processing mode adopted during the production of the fastener, the material is easy to have the phenomena of strain, cracking tendency and strain die damage, and even the die can be scrapped when the material is serious. In order to ensure the lubricating effect in the upsetting process, improve the metal flowing state of the surface of the material during upsetting and increase the qualified rate of an upset finished product, a lubricating coating must be coated on the surface of the titanium alloy wire.
At present, related reports and products about dry film lubricant coating on an upsetting surface are very few, and Chinese patent CN201911369775.5 discloses a surface coating agent for hot upsetting of a titanium alloy wire and a coating method thereof. However, the temperature of continuous warm heading of some manufacturers is as high as 800 ℃, and the scheme is difficult to meet the temperature resistance requirement.
The dry film lubricant with the Biloda brand number 1301 meets the requirements of a continuous warm heading process after being used by a plurality of manufacturers, but the organic resin is adopted as an adhesive, so that the filler content is high, the bonding force with a substrate is poor, and smoke is generated after high-temperature heating in the warm heading process, so that the environment pollution is caused, and the harm is caused to the bodies of construction personnel.
Therefore, the existing lubricating coating technology still has the problems of poor bonding force with a substrate and poor temperature resistance, and cannot meet the processing requirements and environmental protection requirements of continuous hot heading of titanium alloy wires of different manufacturers.
Disclosure of Invention
The invention aims to provide a dry film lubricant, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a dry film lubricant, which comprises the following preparation raw materials in parts by weight:
10.0-30.0 parts of silicate, 5.0-10.0 parts of silica sol, 1.0-5.0 parts of polyethylene emulsion, 10.0-50.0 parts of graphite, 7.5-20.0 parts of boron nitride, 0.1-1.0 part of silicone oil, 40.0-60.0 parts of water and 0.50-2.50 parts of auxiliary agent;
the solid content of the silica sol is 25-35 wt%; the solid content of the polyethylene emulsion is 30-50 wt%.
Preferably, the silicate is one or more of potassium silicate, sodium silicate, lithium silicate and stabilized potassium silicate.
Preferably, the particle size of the graphite is 1-5 μm.
Preferably, the particle size of the boron nitride is 0.5-3 μm.
Preferably, the number average molecular weight of the silicone oil is 500-5000.
Preferably, the auxiliary agent comprises one or more of a wetting dispersant, a defoaming agent, a leveling agent and a thickening agent.
The invention provides a preparation method of the dry film lubricant in the technical scheme, which comprises the following steps:
mixing silicate, silica sol, polyethylene emulsion, graphite, boron nitride, silicone oil, water and an auxiliary agent to obtain a mixed material;
and sequentially grinding and filtering the mixed material to obtain the dry film lubricant.
The invention provides an application of the dry film lubricant in the technical scheme or the dry film lubricant prepared by the preparation method in the technical scheme in continuous warm heading of titanium alloy wires.
Preferably, the application comprises the steps of:
carrying out sand blasting treatment on the titanium alloy wire to obtain a roughened titanium alloy wire;
spraying or dipping the dry film lubricant on the surface of the roughened titanium alloy wire, and heating and curing to obtain a titanium alloy wire with a lubricating coating coated on the surface;
and carrying out continuous warm heading on the titanium alloy wire coated with the lubricating coating on the surface.
Preferably, the temperature of the continuous warm heading is 700-800 ℃.
The invention provides a dry film lubricant, which comprises the following preparation raw materials in parts by weight: 10.0-30.0 parts of silicate, 5.0-10.0 parts of silica sol, 1.0-5.0 parts of polyethylene emulsion, 10.0-50.0 parts of graphite, 7.5-20.0 parts of boron nitride, 0.1-1.0 part of silicone oil, 40.0-60.0 parts of water and 0.50-2.50 parts of auxiliary agent; the solid content of the silica sol is 25-35 wt%; the solid content of the polyethylene emulsion is 30-50 wt%. According to the invention, silicate is used as an adhesive, so that the coating has excellent temperature resistance, high hardness and strong adhesive force with the titanium alloy wire; the temperature resistance and the wear resistance of the coating are further improved by adopting silica sol; graphite and boron nitride are adopted to endow the coating with high-temperature antifriction and wear-resistant properties; adding polyethylene emulsion to further improve the toughness, surface hydrophobicity, smoothness and coating glossiness of the lubricating coating prepared by the dry film lubricant; water is adopted as a dispersing agent, so that the environment is more green and more environment-friendly; the auxiliary agent can ensure that the dry film lubricant is not easy to settle, the filler is uniformly dispersed in the system, and the wetting and leveling property on the surface of the base material is good. The lubricating coating formed by the dry film lubricant provided by the invention is compact, and has no defects of bubbles, nodulation and the like. The results of the examples show that the coefficient of friction of the lubricating coating prepared from the dry film lubricant provided by the invention is less than 0.15; the thickness is 4-10 μm; the adhesive force is 0-1 grade; the neutral salt spray lasts for 96 hours, and the coating does not foam, fall off or rust; the qualification rate of the warm heading finished product is more than 98 percent.
Drawings
FIG. 1 is a graph of the thickness of the lubricating coating test results obtained in example 1;
FIG. 2 is a graph of the thickness of the lubricating coating test results obtained from example 2;
FIG. 3 is a graph of the thickness of the lubricating coating test results obtained in example 3;
FIG. 4 is a graph of the thickness of the lubricating coating test results obtained in example 4;
FIG. 5 is a graph of the thickness of the lubricating coating test results obtained in example 5;
FIG. 6 is a graph of the thickness of the lubricating coating test results obtained from example 6;
FIG. 7 is a graph showing the results of a coefficient of friction test on a lubricating coating prepared in example 1;
FIG. 8 is a graph showing the results of a coefficient of friction test on a lubricating coating prepared in example 2;
FIG. 9 is a graph showing the results of a coefficient of friction test on a lubricating coating prepared in example 3;
FIG. 10 is a graph showing the results of a cohesion test of the lubricating coating prepared in example 1;
FIG. 11 is a graph showing the results of a cohesion test of the lubricating coating prepared in example 2;
FIG. 12 is a graph showing the results of a cohesion test of the lubricating coating prepared in example 3.
Detailed Description
The invention provides a dry film lubricant, which comprises the following preparation raw materials in parts by weight:
10.0-30.0 parts of silicate, 5.0-10.0 parts of silica sol, 1.0-5.0 parts of polyethylene emulsion, 10.0-50.0 parts of graphite, 7.5-20.0 parts of boron nitride, 0.1-1.0 part of silicone oil, 40.0-60.0 parts of water and 0.50-2.50 parts of auxiliary agent;
the solid content of the silica sol is 25-35 wt%; the solid content of the polyethylene emulsion is 30-50 wt%.
The dry film lubricant provided by the invention comprises 10.0-30.0 parts by weight of silicate, preferably 15.0-28.0 parts by weight of silicate, and more preferably 20.0-25.0 parts by weight of silicate. In the present invention, the silicate is preferably one or more of potassium silicate, sodium silicate, lithium silicate and stabilized potassium silicate, more preferably a mixture of lithium silicate and sodium silicate, a mixture of potassium silicate and stabilized potassium silicate, a mixture of potassium silicate and lithium silicate or a mixture of potassium silicate and sodium silicate. In a specific embodiment of the present invention, when the silicate is a mixture of lithium silicate and sodium silicate, the mass ratio of the lithium silicate to the sodium silicate is 1: 1; when the silicate is a mixture of potassium silicate and stable potassium silicate, the mass ratio of the potassium silicate to the stable potassium silicate is 1.5: 1; when the silicate is a mixture of potassium silicate and lithium silicate, the mass ratio of the potassium silicate to the lithium silicate is 1-1.5: 1; when the silicate is a mixture of potassium silicate and sodium silicate, the mass ratio of the potassium silicate to the sodium silicate is 1-1.5: 1.
In the present invention, the stabilized potassium silicate is potassium silicate treated by a stabilizer; the stabilizer is preferably a silane. In the present invention, the stabilized potassium silicate has a high silica content (i.e., low alkali content) and high stability. The invention adopts silane to carry out chemical modification on potassium silicate, leads silicon atoms in the potassium silicate to be connected with organic groups, properly reduces the number of active functional groups (silanol groups) of the potassium silicate, reduces the reaction activity of the potassium silicate, and can further adjust the stability of the potassium silicate through the steric hindrance of the organic groups. In the present invention, the modulus of the stabilized potassium silicate is preferably 3.3 to 3.9.
According to the invention, the silicate has the characteristics of strong binding power, high strength, high temperature resistance and the like, and the silicate is used as the binder, so that the coating can have excellent temperature resistance, high hardness and strong adhesive force with the titanium alloy wire.
Based on the weight part of the silicate, the dry film lubricant provided by the invention comprises 5.0-10.0 parts of silica sol, preferably 7.0-9.0 parts, and more preferably 7.5-8.0 parts. In the present invention, the solid content of the silica sol is preferably 25 to 35 wt%, and more preferably 30 wt%. In the invention, the silica sol can improve the adhesion, temperature resistance and wear resistance of the coating.
Based on the weight part of the silicate, the dry film lubricant provided by the invention comprises 1.0-5.0 parts of polyethylene emulsion, preferably 1.5-3.0 parts, and more preferably 2.0-2.5 parts. In the invention, the solid content of the polyethylene emulsion is preferably 30-50 wt%, and more preferably 35-45 wt%. According to the invention, the polyethylene emulsion can improve the hydrophobicity, toughness, surface scratch resistance and glossiness of the coating. The polyethylene emulsion adopted by the invention has good compatibility with the silicate aqueous solution, good stability and good film forming uniformity.
Based on the weight part of the silicate, the dry film lubricant provided by the invention comprises 10.0-50.0 parts of graphite, preferably 30.0-40.0 parts, and more preferably 35.0-37.5 parts. In the present invention, the particle size of the graphite is preferably 1 to 5 μm. In the invention, the graphite has good lubricating property and good adhesion property.
Based on the weight part of the silicate, the dry film lubricant provided by the invention comprises 7.5-20.0 parts of boron nitride, preferably 10.0-15.0 parts. In the present invention, the particle size of the boron nitride is preferably 0.5 to 3 μm. In the invention, the boron nitride has good high-temperature antifriction and antiwear performance.
Based on the weight part of the silicate, the dry film lubricant provided by the invention comprises 0.1-1.0 part of silicone oil, preferably 0.3-0.5 part, and more preferably 0.35-0.45 part. In the invention, the number average molecular weight of the silicone oil is preferably 500-5000, and more preferably 3000-4000. In the invention, the silicone oil can improve the surface hydrophobicity of the coating and improve the surface smoothness.
Based on the weight portion of the silicate, the dry film lubricant provided by the invention comprises 40.0-60.0 parts of water, preferably 48.0-55.0 parts of water, and more preferably 50.0 parts of water. In the present invention, the water is preferably deionized water. The dry film lubricant prepared by using water as a dispersion medium has very low VOC content, is environment-friendly, and is environment-friendly and safe.
Based on the weight part of the silicate, the dry film lubricant provided by the invention comprises 0.50-2.50 parts of an auxiliary agent, preferably 0.7-1.2 parts, and more preferably 0.85-1.05 parts. In the present invention, the auxiliary agent preferably includes one or more of a wetting dispersant, a defoaming agent, a leveling agent and a thickener.
In the invention, the dry film lubricant provided by the invention preferably comprises 0.4-0.6 part of wetting dispersant, more preferably 0.5-0.6 part by weight of silicate. In the present invention, the wetting dispersant is preferably BYK 191 or BYK 2012.
In the invention, the dry film lubricant provided by the invention preferably comprises 0.1-0.15 part of defoaming agent by weight of the silicate. In the present invention, the antifoaming agent is preferably BYK 028 or BYK 024.
In the invention, the dry film lubricant provided by the invention preferably comprises 0.1-0.15 part of leveling agent by weight of the silicate. In the present invention, the leveling agent is preferably BYK 333 or BYK 349.
In the invention, the dry film lubricant provided by the invention preferably comprises 0.1-0.3 part of thickening agent, more preferably 0.15-0.2 part of thickening agent based on the weight part of silicate. In the present invention, the thickener is preferably sodium carboxymethylcellulose or polyacrylamide.
The lubricating coating formed by the dry film lubricant provided by the invention can reduce the risk of large-area falling off and ensure the warm heading lubricating effect.
The invention also provides a preparation method of the dry film lubricant, which comprises the following steps:
mixing silicate, silica sol, polyethylene emulsion, graphite, boron nitride, silicone oil, water and an auxiliary agent to obtain a mixed material;
and sequentially grinding and filtering the mixed material to obtain the dry film lubricant.
According to the invention, silicate, silica sol, polyethylene emulsion, graphite, boron nitride, silicone oil, water and an auxiliary agent are mixed to obtain a mixed material. In the present invention, the mixing is preferably performed under stirring conditions; the rotating speed of the stirring is preferably 500 r/min; the stirring time is preferably 20-40 min, and more preferably 30 min. In the present invention, the mixing of the silicate, the silica sol, the polyethylene emulsion, the graphite, the boron nitride, the silicone oil, the water and the auxiliary preferably comprises: adding silicate and silica sol into water, and then sequentially adding an auxiliary agent, silicone oil, graphite, boron nitride and polyethylene emulsion. The invention adopts the charging sequence, can ensure that the adhesive (silicate and silica sol) is dissolved and dispersed uniformly in water, and the functional filler (graphite and boron nitride) can be well wetted and dispersed.
After the mixed material is obtained, the mixed material is sequentially ground and filtered to obtain the dry film lubricant. In the present invention, the grinding is preferably carried out in a ball mill; the rotation speed of the ball mill is preferably 200-500 r/min, and more preferably 300-400 r/min. In the invention, the grinding time is preferably 6-24 h, more preferably 10-20 h, and further preferably 18-20 h.
In the present invention, the filtration is preferably performed using a 200 mesh filter cloth.
The invention also provides the application of the dry film lubricant in the technical scheme or the dry film lubricant prepared by the preparation method in the technical scheme in the continuous warm heading of the titanium alloy wire.
In the present invention, the application preferably comprises the steps of:
carrying out sand blasting treatment on the titanium alloy wire to obtain a roughened titanium alloy wire;
spraying or dipping the dry film lubricant on the surface of the roughened titanium alloy wire, and heating and curing to obtain a titanium alloy wire with a lubricating coating coated on the surface;
and carrying out continuous warm heading on the titanium alloy wire coated with the lubricating coating on the surface.
The invention preferably carries out sand blasting treatment on the titanium alloy wire to obtain the roughened titanium alloy wire. In the invention, the surface roughness of the roughened titanium alloy wire is preferably 0.5-2.0 μm. In the invention, the diameter of the titanium alloy wire is preferably 2.0-8.0 mm.
After the roughened titanium alloy wire is obtained, the dry film lubricant is preferably sprayed or soaked on the surface of the roughened titanium alloy wire, and is heated and cured to obtain the titanium alloy wire with the surface coated with the lubricating coating. According to the invention, the dry film lubricant and water are mixed to obtain a coating solution, and then the coating solution is sprayed or impregnated on the surface of the roughened titanium alloy wire. In the invention, the mass ratio of the dry film lubricant to water is preferably 1: 1-2.
In the invention, the heating and curing temperature is preferably 150-180 ℃, and more preferably 160-170 ℃; the time for heating and curing is preferably 1-2 h, and more preferably 1.5-2 h. In the invention, the thickness of the lubricating coating in the titanium alloy wire with the surface coated with the lubricating coating is preferably 4-10 μm, and more preferably 5-7 μm; the coefficient of friction of the lubricious coating is preferably <0.15, more preferably < 0.12; the adhesive force is preferably 0-1 grade; the neutral salt spray lasts for 96 hours, and the lubricating coating does not blister, fall off or rust.
After the titanium alloy wire with the surface coated with the lubricating coating is obtained, the titanium alloy wire with the surface coated with the lubricating coating is preferably subjected to continuous warm heading. In the invention, the temperature of the continuous warm heading is preferably 700-800 ℃.
The dry film lubricant provided by the invention is environment-friendly, has the advantages of strong adhesive force and good temperature resistance, can effectively reduce the friction force between a titanium alloy wire and a mold in the upsetting process, solves the problems of easy pulling and difficult demolding of parts in the forming process, prolongs the service life of the mold, improves the production efficiency and the qualification rate of finished products, and can meet the requirement of continuous warm upsetting processing of titanium alloy fasteners.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 10.0g of lithium silicate, 10.0g of sodium silicate and 7.5g of silica sol (the solid content is 30 wt%) into 50.0g of deionized water, uniformly stirring, then sequentially adding 0.5g of BYK 191, 0.1g of BYK 024, 0.1g of BYK 333, 0.15g of sodium carboxymethylcellulose, 0.3g of silicone oil, 30.0g of graphite, 15.0g of boron nitride and 2.0g of polyethylene emulsion (the solid content is 40 wt%), stirring and dispersing for 30min, grinding the coating at the rotating speed of 300r/min for 10h, and finally filtering by using a 200-mesh filter cloth to obtain the dry film lubricant.
And adding the obtained dry film lubricant into deionized water with the same mass for dilution, stirring and dispersing uniformly, then dip-coating the dry film lubricant on the surface of the titanium alloy wire with the diameter of 6.0mm after sand blasting treatment, and curing at 150 ℃ for 2h to obtain the titanium alloy wire with the surface coated with the lubricating coating.
And carrying out continuous warm heading on the titanium alloy wire with the surface coated with the lubricating coating, wherein the temperature of the continuous warm heading is 700-750 ℃.
Example 2
Adding 15.0g of potassium silicate, 10.0g of stable potassium silicate and 8.0g of silica sol (the solid content is 30 wt%) into 50.0g of deionized water, uniformly stirring, then sequentially adding 0.5g of BYK 2012, 0.1g of BYK 028, 0.1g of BYK 349, 0.1g of polyacrylamide, 0.4g of silicone oil, 35.0g of graphite, 10.0g of boron nitride and 2.5g of polyethylene emulsion (the solid content is 35 wt%), stirring and dispersing for 30min, grinding the coating for 20h at a rotating speed of 300r/min, and finally filtering by using a filter cloth of 200 meshes to obtain the dry film lubricant.
And adding the obtained dry film lubricant into deionized water with the same mass for dilution, stirring and dispersing uniformly, then dip-coating the dry film lubricant on the surface of the titanium alloy wire with the diameter of 3.5mm after sand blasting treatment, and curing at 180 ℃ for 2h to obtain the titanium alloy wire with the surface coated with the lubricating coating.
And carrying out continuous warm heading on the titanium alloy wire with the surface coated with the lubricating coating, wherein the temperature of the continuous warm heading is 700-750 ℃.
Example 3
Adding 15.0g of potassium silicate, 10.0g of lithium silicate and 8.0g of silica sol (the solid content is 30 wt%) into 50.0g of deionized water, uniformly stirring, then sequentially adding 0.5g of BYK 191, 0.1g of BYK 024, 0.1g of BYK 349, 0.1g of sodium carboxymethylcellulose, 0.5g of silicone oil, 37.5g of graphite, 7.5g of boron nitride and 1.5g of polyethylene emulsion (the solid content is 45 wt%), stirring and dispersing for 30min, grinding the coating for 18h at the rotating speed of 300r/min, and finally filtering by using a 200-mesh filter cloth to obtain the dry film lubricant.
And adding the obtained dry film lubricant into deionized water with the same mass for dilution, stirring and dispersing uniformly, then dip-coating the dry film lubricant on the surface of the titanium alloy wire with the diameter of 5.0mm after sand blasting treatment, and curing at 180 ℃ for 2h to obtain the titanium alloy wire with the surface coated with the lubricating coating.
And carrying out continuous warm heading on the titanium alloy wire with the surface coated with the lubricating coating, wherein the temperature of the continuous warm heading is 750-800 ℃.
Example 4
Adding 15.0g of potassium silicate, 10.0g of sodium silicate and 7.0g of silica sol (the solid content is 30 wt%) into 48.0g of deionized water, uniformly stirring, then sequentially adding 0.6g of BYK 191, 0.15g of BYK 028, 0.1g of BYK 349, 0.1g of polyacrylamide, 0.45g of silicone oil, 37.5g of graphite, 7.5g of boron nitride and 2.5g of polyethylene emulsion (the solid content is 40 wt%), stirring and dispersing for 30min, grinding the coating for 18h at a rotating speed of 300r/min, and finally filtering by using 200-mesh filter cloth to obtain the dry film lubricant.
And adding the obtained dry film lubricant into deionized water with the same mass for dilution, stirring and dispersing uniformly, then dip-coating the dry film lubricant on the surface of the titanium alloy wire with the diameter of 2.0mm after sand blasting treatment, and curing at 160 ℃ for 2h to obtain the titanium alloy wire with the surface coated with the lubricating coating.
And carrying out continuous warm heading on the titanium alloy wire with the surface coated with the lubricating coating, wherein the temperature of the continuous warm heading is 700-750 ℃.
Example 5
Adding 15.0g of potassium silicate, 15.0g of sodium silicate and 8.0g of silica sol (the solid content is 30 wt%) into 50.0g of deionized water, uniformly stirring, then sequentially adding 0.4g of BYK 2012, 0.1g of BYK 028, 0.1g of BYK 333, 0.3g of polyacrylamide, 0.35g of silicone oil, 30.0g of graphite, 15.0g of boron nitride and 3.0g of polyethylene emulsion (the solid content is 40 wt%), stirring and dispersing for 30min, grinding the coating for 18h at a rotating speed of 300r/min, and finally filtering by using 200-mesh filter cloth to obtain the dry film lubricant.
And adding the obtained dry film lubricant into deionized water with the mass of 1.5 times to dilute, stirring and dispersing uniformly, then dip-coating the dry film lubricant on the surface of the titanium alloy wire with the diameter of 8.0mm after sand blasting treatment, and curing at 180 ℃ for 2 hours to obtain the titanium alloy wire with the surface coated with the lubricating coating.
And carrying out continuous warm heading on the titanium alloy wire with the surface coated with the lubricating coating, wherein the temperature of the continuous warm heading is 750-800 ℃.
Example 6
Adding 15.0g of potassium silicate, 15.0g of lithium silicate and 10.0g of silica sol (the solid content is 30 wt%) into 55.0g of deionized water, uniformly stirring, then sequentially adding 0.4g of BYK 191, 0.1g of BYK 024, 0.1g of BYK 333, 0.3g of sodium carboxymethylcellulose, 0.3g of silicone oil, 40.0g of graphite, 10.0g of boron nitride and 3.0g of polyethylene emulsion (the solid content is 40 wt%), stirring and dispersing for 30min, grinding the coating for 18h at the rotating speed of 300r/min, and finally filtering by using a 200-mesh filter cloth to obtain the dry film lubricant.
And adding the obtained dry film lubricant into deionized water with the mass of 1.5 times to dilute, stirring and dispersing uniformly, then dip-coating the dry film lubricant on the surface of the titanium alloy wire with the diameter of 8.0mm after sand blasting treatment, and curing at 180 ℃ for 1.5 hours to obtain the titanium alloy wire with the surface coated with the lubricating coating.
And carrying out continuous warm heading on the titanium alloy wire with the surface coated with the lubricating coating, wherein the temperature of the continuous warm heading is 700-750 ℃.
Test example
The performance of the lubricating coatings in the titanium alloy wires with the lubricating coatings coated on the surfaces prepared in the examples 1-6 is tested, the test results are shown in figures 1-12 and table 1, and figure 1 is a test result graph of the thickness of the lubricating coating prepared in the example 1; FIG. 2 is a graph of the thickness of the lubricating coating test results obtained from example 2; FIG. 3 is a graph of the thickness of the lubricating coating test results obtained in example 3; FIG. 4 is a graph of the thickness of the lubricating coating test results obtained in example 4; FIG. 5 is a graph of the thickness of the lubricating coating test results obtained in example 5; FIG. 6 is a graph of the thickness of the lubricating coating test results obtained from example 6; FIG. 7 is a graph showing the results of a coefficient of friction test on a lubricating coating prepared in example 1; FIG. 8 is a graph showing the results of a coefficient of friction test on a lubricating coating prepared in example 2; FIG. 9 is a graph showing the results of a coefficient of friction test on a lubricating coating prepared in example 3; FIG. 10 is a graph showing the results of a cohesion test of the lubricating coating prepared in example 1; FIG. 11 is a graph showing the results of a cohesion test of the lubricating coating prepared in example 2; FIG. 12 is a graph showing the results of a cohesion test of the lubricating coating prepared in example 3.
The specific test method comprises the following steps:
coating thickness: testing is carried out according to an optical method of 5.4 in GB T13452.2-2008 'determination of paint film thickness of colored paint and varnish';
salt spray resistance: testing is carried out according to the method in GB T1771-2007 test for neutral salt fog resistance of colored paint and varnish; the specific test conditions were: 3.5 wt% sodium chloride solution, 35 +/-2 ℃, 96 h;
frictional wear performance: testing the frictional wear performance of the coating by using a CSM (Carrier sense multiple Access) friction testing machine, wherein the contact stress is 600MPa, the frequency is 1Hz, and the dual phi 6 stainless steel balls are arranged;
adhesion force: the tests were carried out according to the method described in GB/T9286-1998 test for marking test of paint and varnish films.
TABLE 1 Performance test results for lubricating coatings of examples 1-6
Figure BDA0003424519900000111
As can be seen from table 1 and fig. 1 to 12, the coefficient of friction of the lubricant coating obtained from the dry film lubricant provided by the present invention is < 0.15; the adhesive force is 0-1 grade; after the neutral salt spray is tested for 96h, the coating has no bubbling, no shedding and no corrosion; the continuous warm heading qualification rate reaches more than 98 percent. The results show that the dry film lubricant provided by the invention has good adhesive force, temperature resistance and neutral salt spray resistance on the premise of lower friction coefficient when being used as a titanium alloy wire lubricating coating.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The dry film lubricant is characterized by comprising the following preparation raw materials in parts by weight:
10.0-30.0 parts of silicate, 5.0-10.0 parts of silica sol, 1.0-5.0 parts of polyethylene emulsion, 10.0-50.0 parts of graphite, 7.5-20.0 parts of boron nitride, 0.1-1.0 part of silicone oil, 40.0-60.0 parts of water and 0.50-2.50 parts of auxiliary agent;
the solid content of the silica sol is 25-35 wt%; the solid content of the polyethylene emulsion is 30-50 wt%.
2. The dry film lubricant according to claim 1, wherein the silicate is one or more of potassium silicate, sodium silicate, lithium silicate, and stabilized potassium silicate.
3. The dry film lubricant according to claim 1, wherein the graphite has a particle size of 1 to 5 μm.
4. The dry film lubricant according to claim 1, wherein the boron nitride has a particle size of 0.5 to 3 μm.
5. The dry film lubricant according to claim 1, wherein the silicone oil has a number average molecular weight of 500 to 5000.
6. The dry film lubricant according to claim 1, wherein the auxiliary agent comprises one or more of a wetting dispersant, a defoamer, a leveling agent and a thickener.
7. The method of preparing the dry film lubricant according to any one of claims 1 to 6, comprising the steps of:
mixing silicate, silica sol, polyethylene emulsion, graphite, boron nitride, silicone oil, water and an auxiliary agent to obtain a mixed material;
and sequentially grinding and filtering the mixed material to obtain the dry film lubricant.
8. Use of the dry film lubricant according to any one of claims 1 to 6 or the dry film lubricant prepared by the preparation method according to claim 7 in continuous warm heading of titanium alloy wire.
9. Use according to claim 8, characterized in that it comprises the following steps:
carrying out sand blasting treatment on the titanium alloy wire to obtain a roughened titanium alloy wire;
spraying or dipping the dry film lubricant on the surface of the roughened titanium alloy wire, and heating and curing to obtain a titanium alloy wire with a lubricating coating coated on the surface;
and carrying out continuous warm heading on the titanium alloy wire coated with the lubricating coating on the surface.
10. The use according to claim 9, wherein the temperature of the continuous warm heading is 700-800 ℃.
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