CN111411009B - Metal drawing lubricant and preparation method thereof - Google Patents

Metal drawing lubricant and preparation method thereof Download PDF

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Publication number
CN111411009B
CN111411009B CN201911280658.1A CN201911280658A CN111411009B CN 111411009 B CN111411009 B CN 111411009B CN 201911280658 A CN201911280658 A CN 201911280658A CN 111411009 B CN111411009 B CN 111411009B
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coupling agent
metal drawing
drawing lubricant
acid esters
metal
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CN111411009A (en
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姚华强
何友德
刘安荣
何瞻
王振杰
彭伟
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GUIZHOU INSTITUTE OF METALLURGY AND CHEMICAL ENGINEERING
Guizhou Shuigang Metal Technology Co ltd
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GUIZHOU INSTITUTE OF METALLURGY AND CHEMICAL ENGINEERING
Guizhou Shuigang Tongxinsheng Metal Products Co ltd
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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
    • C10M105/00Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/32Esters
    • C10M105/34Esters of monocarboxylic acids
    • 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
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04Mixtures of base-materials and additives
    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/281Esters of (cyclo)aliphatic monocarboxylic acids
    • C10M2207/2815Esters of (cyclo)aliphatic monocarboxylic acids used as base material
    • 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
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/04Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions having a silicon-to-carbon bond, e.g. organo-silanes
    • 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
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06Organic compounds derived from inorganic acids or metal salts
    • C10M2227/065Organic compounds derived from inorganic acids or metal salts derived from Ti or Zr

Abstract

The invention relates to the technical field of wire drawing lubrication, in particular to a metal drawing lubricant and a preparation method thereof.

Description

Metal drawing lubricant and preparation method thereof
Technical Field
The invention relates to the technical field of wire drawing lubrication, in particular to a metal drawing lubricant and a preparation method thereof.
Background
The metal drawing is a plastic processing technology for obtaining wires or pipes with high precision and high glossiness by reducing the sectional area of processing materials through a die hole, belongs to a shape mark processing technology, is widely applied to various metal materials such as carbon steel, stainless steel, alloy steel, copper, aluminum, alloy and the like, and can produce thousands of products with different specifications and purposes such as bars or pipes with diameters as large as tens of millimeters, wires and threads with diameters as small as micrometers. The metal drawing process needs to consume a large amount of energy, the energy consumption is on the friction between the die and the drawing material, the temperature of a drawing interface is increased in the drawing process, a large amount of heat is generated, and the yield and the qualification rate of a metal drawing product are low.
However, with the continuous development of metal drawing technology, the drawing efficiency is continuously improved, so that the quality requirement on the lubricant is higher and higher, the lubricant has good lubricating property and cooling property, the treatment of the next process cannot be influenced, and the lubricant also has high-temperature resistance and wear resistance, so that the phenomena of cracking and even sintering of a lubricant film layer caused by the metal drawing process are avoided, and the smooth metal drawing is ensured. At present, in the metal drawing process, the adopted lubricant is mainly full-oil or synthetic, is prepared by taking vegetable oil and industrial product oil as main raw materials, and the cost of the lubricant gradually rises along with the continuous rise of the price of petroleum; the cooling effect of the all-oil lubricant is poor, and the generated heat causes oil to evaporate during metal drawing, so that unpleasant smell is generated, the environment of a production workshop is influenced, and the health of workers is threatened; in addition, the lubricant in the prior art has poor high temperature resistance, so that the lubricant film layer is damaged and even sintered by heat generated during friction between a metal material and a die in the drawing process, sparks are generated by drawing friction, and serious potential safety hazards exist.
In view of this, the present researchers found that a lot of research was made on the technical problem in the prior art through search.
For example, in order to improve the heat dissipation rate of the lubricant, generate oil mist, and generate sparks, patent No. ZL200810026982.6 discloses a metal wire drawing lubricant using a water-based lubricant, a vegetable fermented material, vegetable oil, nitride, and water; the nitride is amide and/or ammonium salt, and the plant fermentation material is lignocelluloses and/or lignosulphonate.
For another example: in order to reduce the friction coefficient, repair the friction surface, reduce the breakage rate of the metal wire and prevent the generation of unpleasant gas, the patent application No. 201611135240.8 discloses a preparation method of a metal wire drawing lubricant, which comprises the steps of preparing lubricating oil base oil by taking methyl ricinoleate as a raw material, compounding the prepared molybdenum disulfide with a graphene-like structure with a carbon nano tube dispersion liquid by using ultrasonic-assisted glass molybdenum disulfide crystals to obtain a dispersion liquid, stirring the lubricating oil base oil, polyvinyl alcohol and deionized water, adding the dispersion liquid, and mixing to obtain the metal wire drawing lubricant.
However, in the metal drawing process, the lubricant is required to have the performances of protecting the environment, weakening the safety risk, reducing the cost, improving the heat dissipation effect, ensuring the drawing speed and the like, and also to ensure strong adhesion, so that the metal is prevented from falling in the metal drawing process, and the dust generation rate of a metal drawing workshop is reduced. However, in the prior art, the lubricant used for metal drawing is not studied according to the lubricant adhesion capacity, so that the obtained lubricant product has low effect in the metal drawing process, a large amount of dust is generated in a metal drawing workshop, the metal wire breakage rate is high, and the product yield is low.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a metal drawing lubricant and a preparation method thereof.
The method is realized by the following technical scheme:
the preparation method of the metal drawing lubricant comprises the steps of reacting ricinoleic acid esters with alcohol organic matters under the catalysis of a catalyst, and adding a titanate coupling agent and silane coupling agent mixture which account for 1% of the mass of the ricinoleic acid esters in the reaction process by the mass of the titanate coupling agent; the metal drawing lubricant is prepared by the catalytic reaction of ricinoleic acid esters and alcohol organic matters, the ricinoleic acid esters are rich in raw materials, the cost is reduced, and a mixture of a titanate coupling agent and a silane coupling agent is added in the reaction process, so that the mixture participates in the reaction of the ricinoleic acid esters and the alcohol organic matters, the adhesive force of the lubricant on the metal surface in the metal drawing process is improved, the heat dissipation efficiency is improved, the metal drawing speed is improved, and the dust generation rate of a metal drawing workshop is reduced.
Wherein: the adopted ricinoleic acid esters are methyl ricinoleate and/or polyoxypropylene ricinoleate, and when the methyl ricinoleate and the polyoxypropylene ricinoleate are preferably mixed according to the volume ratio of 1:1, the lubricating effect is good, the friction coefficient of the metal surface attached by the lubricant is reduced, and the metal drawing speed is improved; adopting alcohol organic matter as isooctyl alcohol and/or isobutyl alcohol, preferably mixing isooctyl alcohol and isobutyl alcohol according to the volume ratio of 1: 0.8; the catalyst is a solid strong acid catalyst and/or a D001 resin catalyst, and the solid strong acid catalyst and the D001 resin catalyst are preferably mixed according to the mass ratio of 1:0.1-0.3, so that the reaction effect of ricinoleic acid esters and alcohol organic matters is improved, the adhesive force of a lubricant on the metal surface is enhanced, the metal drawing speed is improved, and the production efficiency of drawn products is improved; the conditions of the reaction process are as follows: mixing ricinoleic acid esters and alcohol organic matters, adding the mixture into a reaction kettle, adding a catalyst accounting for 0.2-0.8% of the mass of the mixed solution, stirring for 8-12min at the speed of 150-200r/min, heating to 92-95 ℃, stirring while heating, adding a titanate coupling agent and silane coupling agent mixture during stirring, and reacting for 1-2h at constant temperature to obtain the castor oil.
Preferably, the solid strong acid catalyst is SO4 2-/WO3And/or SO4 2-/TiO2
Preferably, the mixing volume ratio of the ricinoleic acid esters to the alcohol organic matters is 1: 3-4.
Preferably, the mixing volume ratio of the ricinoleic acid esters to the alcohol organic matters is 1: 3.5.
Preferably, the mixing mass ratio of the titanate coupling agent to the silane coupling agent mixture is 1: 0.2-0.5.
Preferably, the mixing mass ratio of the titanate coupling agent to the silane coupling agent mixture is 1: 0.3-0.4.
Preferably, the mixing mass ratio of the titanate coupling agent to the silane coupling agent mixture is 1: 0.35.
Compared with the prior art, the invention has the technical effects that:
by adding the mixture of the titanate coupling agent and the silane coupling agent in the reaction process of the ricinoleic acid esters and the alcohol organic matters, the adhesive force of the lubricant for metal drawing prepared by the reaction of the ricinoleic acid esters and the alcohol organic matters on the surface of the metal wire is improved, the flame retardant property of the lubricant is improved, the phenomenon that the lubricant burns due to high temperature generated in the drawing process of the metal wire is prevented, the surface smoothness of the steel wire in the metal drawing process is improved, the friction coefficient between the surface of the steel wire and a mold in the metal drawing process is reduced, the drawing energy consumption is reduced, and the quality of the drawn steel wire product is ensured.
The invention is suitable for being used as a lubricant when metal materials such as copper, iron, carbon steel, aluminum alloy and the like are drawn into corresponding wire materials, and has high heat dissipation efficiency; in the research process, the catalyst composition and the mixture ratio of the coupling agent mixture are controlled, so that the performance of the lubricant is greatly improved when the steel wire is drawn, the drawing temperature is reduced, the phenomenon of sintering into coke in the drawing process is avoided, the surface smoothness of the drawn steel wire is ensured, and the quality of the drawn product is ensured. The following tests show that: when the concentration of the lubricant is 2%, the strength of a film formed on the surface of the metal wire rod can reach above 71kg, and during the drawing process of the steel wire, no burning smoke and smog are found, so that the adsorption strength and the flame retardant property after the coupling agent is added are fully utilized, the comprehensive performance of the lubricant is improved to the maximum extent, the quality of the lubricant is improved, and the quality of a metal drawing product is ensured.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
Example 1
Weighing 50mL of methyl ricinoleate, weighing 150mL of isooctanol, mixing, putting into a reaction kettle, adding 0.342g of D001 resin catalyst into the reaction kettle, stirring at 200r/min for 8-12min, heating to 92-95 ℃, stirring while heating, and reacting at constant temperature for 1-2h to obtain the product.
Example 2
Weighing 100mL of polyoxypropylene ricinoleate, 400mL of isobutanol, mixing, filling into a reaction kettle, adding 3.432g of SO into the reaction kettle4 2-/WO3Stirring at 200r/min for 8-12min at 150-.
Example 3
Methyl ricinoleate (75 mL) and isobutanol (225 mL) were measured, mixed, charged into a reaction kettle, and 1.51g SO was added to the reaction kettle4 2-/TiO2Stirring at 200r/min for 8-12min at 150-.
Example 4
Respectively measuring 35mL of methyl ricinoleate and 35mL of polyoxypropylene ricinoleate, and mixing the methyl ricinoleate with the polyoxypropylene ricinoleate to obtain mixed oleate; measuring 150mL of isooctyl alcohol and 95mL of isobutanol, and mixing the isooctyl alcohol and the isobutanol to obtain mixed alcohol; mixing mixed alcohol and mixed oleate, loading into a reaction kettle, adding 1.3538g of D catalyst into the reaction kettle, wherein the catalyst is SO4 2-/WO3The catalyst and the D001 resin catalyst are mixed according to the mass ratio of 1: 0.1; after adding the catalyst, stirring at the speed of 200r/min for 8-12min at the speed of 150-.
Examples 5 to 8
On the basis of the embodiments 1 to 4, the other embodiments are the same as the embodiments 1 to 4, in the preparation process, in the reaction process of ricinoleic acid esters and alcohol organic matters, a titanate coupling agent, a mixture of the titanate coupling agent and a silane coupling agent, and the silane coupling agent are added, and the specific adding amount is shown in the following table 1:
TABLE 1
Figure BDA0002316644870000061
Example 9
On the basis of the embodiment 4, the other steps are the same as the embodiment 4, in the preparation process, in the reaction process of ricinoleic acid esters and alcohol organic matters, a mixture of a titanate coupling agent 201 and a silane coupling agent A151 is added, and in the adding process, the titanate coupling agent 201 and the silane coupling agent A151 are mixed according to the mass ratio of 1: 0.35; the catalyst added in the reaction process is SO4 2-/TiO2Mixed with a D001 resin catalyst according to the mass ratio of 1: 0.3.
Film strength test:
the film strength refers to the pressure that the adsorption film can bear when the lubricant is processed in a pressed state after being adsorbed on the metal surface, namely, the adsorption capacity of the lubricant on the metal surface is expressed. The test is carried out by using a domestic MQ-800 type four-ball wear tester and measuring the strength of the film formed on the metal surface by the lubricant according to the test method introduced in the SY-2665-77 standard, and the test results are shown in Table 2.
TABLE 2
Figure BDA0002316644870000071
The data in table 2 show that the technical scheme of the invention improves the capability of the obtained product to be attached to the surface of the metal wire when the product is used as a lubricant in the metal drawing process by adding the mixture of the titanate coupling agent and the silane coupling agent to participate in the reaction process of ricinoleic acid esters and alcohol organic matters, and the film strength formed on the surface of the metal wire is higher when the product is used, particularly when the mass concentration of the product is 2%, compared with the condition that the mixture of the titanate coupling agent and the silane coupling agent is not added or the titanate coupling agent is simply added or the silane coupling agent is simply added, the film strength is greatly improved, and the adhesive force of the lubricant is improved by adding the mixture of the titanate coupling agent and the silane coupling agent to react.
Drawing performance test:
the test adopts a medium carbon steel wire with the steel diameter of 5.89mm, and the tensile strength of the steel wire is 85.3kg/mm2. The steel wire was drawn after being treated with the lubricant prepared in examples 1 to 9 using a chain type drawing machine under the same conditions, and the results of the drawing performance test are shown in table 3 below.
TABLE 3
Figure BDA0002316644870000081
The data in table 3 show that the invention improves the viscosity performance of the obtained lubricant and reduces the friction coefficient by the mixture of titanate coupling agent and silane coupling agent participating in the reaction process of ricinoleic acid esters and alcohols organic matter, so that the friction between the metal wire and the die is low in the drawing process of the metal wire, the electric energy consumed in the drawing process is reduced, and the energy consumption is reduced; meanwhile, the cooling effect is excellent, the heat dissipation and cooling efficiency of the lubricant is improved, the temperature generated on the surface of the metal during drawing is reduced, and the drawing quality is ensured.
In addition, the researchers also tested and microscopically observed the broken end condition in the drawing performance test process and the color and the surface smoothness of the drawn product, and the results are as follows:
when the lubricants prepared in examples 1 to 4 are used for drawing treatment, the phenomenon of end breakage occurs, and the surface of the steel wire obtained by drawing is dark black and has drawing marks; in the groups 1 and 2 added in the examples 5 to 8, the phenomenon of end breakage occurs, the surface of the steel wire obtained by drawing is light black, and the surface has drawing marks; in addition 3 groups of examples 5 to 8 and example 9, the phenomenon of end breakage did not occur, and the surface of the steel wire obtained by drawing was oil black and bright, and no drawing mark was formed on the surface. Meanwhile, the smoke generated in the drawing process is counted, and the following results are found: in examples 1 to 4, there were generated fumes, and scorched carbon black substances existed on the surface of the steel wire obtained by drawing; slight generation of fumes was observed in the addition groups 1 and 2 of examples 5 to 8, and no burnt carbon black material was found to remain on the surface of the drawn wire; in the addition groups 3 and 9 of examples 5 to 8, no smoke generation and no charred carbon black material were observed; therefore, the lubricant provided by the invention can improve the friction coefficient between a metal wire and a die in the drawing process of a steel wire, can reduce the drawing scratches, ensures the quality of the steel wire, is not easy to be burnt to generate gas harmful to human bodies in the drawing process, and improves the health safety coefficient of production workers. The steel wire obtained by drawing is stored for half a year in a natural environment, and no corrosion is generated.
The present invention is not to be limited to the details of the procedures and techniques disclosed in the prior art.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (9)

1. A metal drawing lubricant preparation method, react ricinoleic acid esters with alcoholic organic matter under the catalytic action of catalyst, characterized by, add titanate coupling agent and silane coupling agent mixture in the reaction process; wherein: the ricinoleic acid esters are methyl ricinoleate and/or polyoxypropylene ricinoleate; the alcohol organic matter is isooctanol and/or isobutanol; the catalyst is a solid strong acid catalyst and/or a D001 resin catalyst; the conditions of the reaction process are as follows: mixing ricinoleic acid esters and alcohol organic matters, adding the mixture into a reaction kettle, adding a catalyst accounting for 0.2-0.8% of the mass of the mixed solution, stirring for 8-12min at the speed of 150-200r/min, heating to 92-95 ℃, stirring while heating, adding a titanate coupling agent and silane coupling agent mixture during stirring, and reacting for 1-2h at constant temperature to obtain the castor oil.
2. The method of preparing a metal drawing lubricant according to claim 1, wherein the solid strong acid catalyst is SO4 2-/WO3And/or SO4 2-/TiO2
3. The method of preparing a metal drawing lubricant according to claim 1, wherein the mixing volume ratio of ricinoleic acid esters to alcohol organics is 1: 3-4.
4. The method for preparing the metal drawing lubricant according to claim 1 or 3, wherein the mixing volume ratio of the ricinoleic acid esters to the alcohol organic substance is 1: 3.5.
5. The method of preparing a metal drawing lubricant according to claim 1, wherein the titanate coupling agent and the silane coupling agent mixture are mixed in a mass ratio of 1: 0.2-0.5.
6. The method of preparing the metal drawing lubricant according to claim 1 or 5, wherein the mixing mass ratio of the titanate coupling agent and the silane coupling agent mixture is 1: 0.3-0.4.
7. The method of preparing a metal drawing lubricant according to claim 1 or 5, wherein the titanate coupling agent and the silane coupling agent mixture are mixed in a mass ratio of 1: 0.35.
8. The method of preparing a metal drawing lubricant according to claim 1, wherein the titanate coupling agent and silane coupling agent mixture is added to the reaction vessel in an amount of 1% by mass of ricinoleic acid esters based on the mass of titanate coupling agent.
9. Metal drawing lubricant prepared according to any one of claims 1 to 8, for use in the production of drawn steel wire.
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CN111778093A (en) * 2020-08-05 2020-10-16 陕西高精尖新材料科技有限责任公司 Titanium alloy wire high-temperature drawing oil-based lubricant and preparation method thereof

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CN104004572A (en) * 2014-04-25 2014-08-27 蚌埠市时代电子有限公司 Titanium dioxide-containing copper wire drawing oil
CN107778976A (en) * 2016-08-31 2018-03-09 天津天女化工集团股份有限公司 A kind of ink vehicle for adding modified castor oil

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CN103614219A (en) * 2013-10-21 2014-03-05 全威(铜陵)铜业科技有限公司 High-temperature wire drawing lubricant and preparation method thereof
CN104004572A (en) * 2014-04-25 2014-08-27 蚌埠市时代电子有限公司 Titanium dioxide-containing copper wire drawing oil
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Address before: 553000 Guizhou Shuigang tongxinsheng metal products Co., Ltd. Hongqiao Industrial Park, Zhongshan Economic Development Zone, Liupanshui City, Guizhou Province

Patentee before: GUIZHOU SHUIGANG TONGXINSHENG METAL PRODUCTS CO.,LTD.

Patentee before: GUIZHOU INSTITUTE OF METALLURGY AND CHEMICAL ENGINEERING