CN103525507B - Metal surface alloying agent and preparation method thereof - Google Patents
Metal surface alloying agent and preparation method thereof Download PDFInfo
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- CN103525507B CN103525507B CN201310473282.2A CN201310473282A CN103525507B CN 103525507 B CN103525507 B CN 103525507B CN 201310473282 A CN201310473282 A CN 201310473282A CN 103525507 B CN103525507 B CN 103525507B
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Abstract
The invention discloses a metal surface alloying agent, which is prepared from the following components by weight: 80-92% of vegetable oil, 2-8% of metal compounds and 5-15% of a catalyst. The metal compounds include an aluminum-containing compound, a calcium-containing compound, a boron-containing compound, a magnesium-containing compound, a titanium-containing compound and a molybdenum-containing compound. Amount of each metal compound realizes the following mass fraction of metal atoms in the metal surface alloying agent: 0.01-0.3% of aluminum atoms, 0.01-0.5% of titanium atoms, 0.1-0.5% of boron atoms, 0.5-2% of calcium atoms and 0.5-3% molybdenum atoms. The invention also discloses a preparation method of the alloying agent. The metal surface alloying agent does not contain sulfur, chlorine or phosphorus, meets the requirements of environmental protection and has good extreme pressure antiwear performance and antioxidant properties.
Description
Technical field
The present invention relates to high energy mechanical alloying process field, particularly relate to a kind of metal surface alloy agent and preparation method thereof.
Background technology
According to internal authority mechanism statistics, Material Wear, corrosion and fatigue three lossy account for 30% of gross industrial output value.Frictional wear is ubiquitous spontaneous phenomenon, the frictionloss primary energy source in the world about 1/3rd, wearing and tearing are one of three kinds of topmost forms causing material and damage of facilities and inefficacy, and lubrication is then reduce friction, reduce or avoid the most effective technology that weares and teares.Development has good wear resistance, high bearing capacity, wear surface is had to the lubrication technology of certain repairing effect, environmentally safe or less contamination, is chemistry and one of important topic of Materials science and tribology in the present age.
The efficient extreme pressure anti-wear additives of zinc dialkyl dithiophosphate (ZDDP) has been the indispensable addO-on therapy of oil engine wet goods oil product since 20 middle of century always, and widespread use is have also been obtained in gear oil, hydraulic pressure wet goods technical oils, but it has seemed and to be difficult to adapt to the situation the needs of development now.This is because: the phosphorous converted product of (1) ZDDP can be used in the poisoning of catalyst in the three way catalytic converter reducing the noxious gas emissions such as oxynitride (NOx) in vehicle exhaust and affect oxygen sensor; (2) ZDDP can produce ash content, and blocking filtering system, can produce detrimentally affect to the particle trapper of diesel engine; (3) element Zn can make some alloy bearing (mainly referring to argentiferous, plumbous parts) produce galvanic corrosion; (4) anti-oxidant and extreme pressure and antiwear behavior can be lost because sharply decomposing under higher than the operating mode of 160 degree.
Chinese patent patent of invention ZL200910067880.3 discloses a kind of cermet couplant, this couplant is the wear preventive additive containing magnesium, aluminium, boron and titanium ceramic metal, for the mixture of each component, in order to ensure good suspension and dispersiveness, its dispersion agent used is chloride, has potential safety and environmental protection risk.
Chinese patent ZL200710143950.X discloses a kind of nano-stage ceramic metal mixture additive for lubricating oil, fat, this additive for including boron nitride, molybdenum, the composition liquid of copper powder body; This boron nitride, molybdenum, the solid particulate matter that copper powder body powder a kind of nano level that to be boron nitride and molybdenum formed with coordinate bond structure with covalent bond structure, copper is spherical; Boron nitride is spherical skeleton, and molybdenum is coated on it with lamellar, and copper is combined with the lattice defect place of spheroid with point, sheet; In this powder, shared by boron nitride, molybdenum and copper, the ratio of component is 7 ~ 8.5: 1 ~ 1.5: 0.5 ~ 1, and the shortcoming of this additive is that oil soluble is poor, easily produces precipitation.
In sum, there is following shortcoming in existing metal surface alloy agent:
(1) sulfur-bearing, phosphorus and zinc, easily produces burn into and poisons and high temperature failure; (2) containing chlorine, corrosion can be produced; (3) oil soluble is poor, easily produces precipitation.
Summary of the invention
An object of the present invention is to provide the objectionable impuritiess such as a kind of not sulfur-bearing, phosphorus, zinc, chlorine, oil soluble is good, wear resistance is high metal surface alloy agent.
Another object of the present invention is to provide a kind of method preparing above-mentioned metal surface alloy agent.
For this reason, technical scheme of the present invention is as follows:
A kind of metal surface alloy agent, is prepared from by the component of following mass percent:
Vegetables oil: 80-92%
Metallic compound: 2-8%
Catalyzer: 5-15%,
Wherein, described metallic compound comprises aluminum contained compound, calcium containing compound, boron-containing compound, magnesium-containing compound, titanium-containing compound and molybdate compound, and the consumption of each compound makes the massfraction of atoms metal in prepared metal surface alloy agent be respectively:
Aluminium atom: 0.01-0.3%,
Titanium atom: 0.01-0.5%,
Boron atom: 0.1-0.5%,
Calcium atom: 0.5-2%,
Molybdenum atom: 0.5-3%.
Preferably, described vegetables oil be in peanut oil, soybean oil, oleum lini, plam oil, Oleum Cocois, Viscotrol C, rape seed oil one or more with arbitrarily than mixture.
Described catalyzer is ammoniacal liquor, hydrochloric acid, bicarbonate of ammonia, hydrogen peroxide or potassium permanganate.
Described aluminum contained compound be aluminum isopropylate, Aluminate, Tai-Ace S 150, aluminum nitrate and aluminium powder one or more with arbitrarily than mixture.
Described calcium containing compound be in calcium hydroxide, calcium oxide, organic sulfonic acid calcium, calcium carbonate and alkyl sodium salicylate one or more with arbitrarily than mixture.
Described boron-containing compound be a kind of in boric acid, boron oxide, boric acid ester or wherein multiple with arbitrarily than mixture.
Described magnesium-containing compound be in magnesium oxide, magnesium hydroxide, magnesium nitrate, organic sulfonic acid magnesium one or more with arbitrarily than mixture.
Described titanium-containing compound be in titanic acid ester, titanium oxide, titanium tetrachloride, titanium isopropylate, titanium sulfate one or more with arbitrarily than mixture.
Described molybdate compound be in molybdenum oxide, ammonium molybdate, organic-molybdenum one or more with arbitrarily than mixture.
A preparation method for above-mentioned metal surface alloy agent, comprises the following steps:
1) preparation of metallic compound:
Under agitation, in reactor, add aluminum contained compound, titanium-containing compound, calcium containing compound, boron-containing compound, magnesium-containing compound and molybdate compound according to formula, stir 1 ~ 4 hour, obtain brown viscous liquid;
2) preparation of metal surface alloy agent:
The above-mentioned brown liquid that obtains is moved in autoclave, vegetables oil and hydrochloric acid is added by formula, then autoclave is closed, pass into carbonic acid gas to supercritical pressure 72.9atm, be warming up to supercritical temperature 31.26 DEG C, after reacting 3 ~ 6 hours under agitation, cooling, separatory, vacuum dehydration, obtain oil soluble transparent liquid or viscous liquid.
The method that metal surface alloy agent of the present invention utilizes chemistry and physical metallurgy to combine to change metal material surface chemical composition and weave construction, thus makes material surface obtain the technological process of required performance.Be carrier with lubricant, utilize fricative heat, by chemical heat treatment technology, material hardness, corrosion-resistant and resistance toheat can be improved on the one hand, the wear resistance of material can also be improved on the other hand.
Metal surface alloy agent of the present invention is the multi-element compounds of boracic, calcium, molybdenum, aluminium and magnesium, itself is sulfur-bearing, chlorine and phosphorus not, meets the low-sulfur of environmental protection and API (API) GF-4, GF-5, phosphorus requires and have good extreme pressure and antiwear behavior and antioxidant property.
Accompanying drawing explanation
Fig. 1 is the obtained metal surface alloy agent of embodiment 3 joins the surface of friction pair element recorded in lubricating oil electronic spectrum in the ratio of 0.5wt%.
Embodiment
Below in conjunction with specific embodiment, method of the present invention is described in detail.
Embodiment 1
A preparation method for metal surface alloy agent, comprises the following steps:
(1) preparation of metallic compound:
In a kettle., add 10g aluminum isopropylate, 15g titanic acid ester, 20g organic sulfonic acid calcium, 10g boric acid, 25g organic sulfonic acid magnesium and 5g ammonium molybdate under agitation successively, stir 1 hour, obtain brown viscous liquid.
(2) preparation of metal surface alloy agent:
The brown liquid that 5g step (1) is obtained moves in autoclave, add 70g plam oil and 5g hydrochloric acid respectively, then capping still, pass into carbonic acid gas to supercritical pressure 72.9atm, be warming up to supercritical temperature 31.26 DEG C, react after 4 hours under agitation condition, after cooling, separatory, vacuum dehydration, obtain oil soluble transparent liquid or viscous liquid.
Embodiment 2
A preparation method for metal surface alloy agent, comprises the following steps:
(1) preparation of metallic compound:
In a kettle., add 12g Aluminate, 13g titanium isopropylate, 24g alkyl sodium salicylate, 12g boric acid, 21g magnesium nitrate and 3g organic-molybdenum under agitation successively, stir 1 hour, obtain brown viscous liquid.
(2) preparation of metal surface alloy agent:
The brown liquid that 5g step (1) is obtained moves in autoclave, add 60g plam oil and 2g potassium permanganate respectively, then capping still, pass into carbonic acid gas to supercritical pressure 72.9atm, be warming up to supercritical temperature 31.26 DEG C, react after 4 hours under agitation condition, after cooling, separatory, vacuum dehydration, obtain oil soluble transparent liquid or viscous liquid.
Embodiment 3
The brown liquid that 5g embodiment 1 step (1) is obtained moves in autoclave, add 60g Oleum Cocois and 2g potassium permanganate respectively, then capping still, pass into carbonic acid gas to supercritical pressure 72.9atm, be warming up to supercritical temperature 31.26 DEG C, react after 4 hours under agitation condition, after cooling, separatory, vacuum dehydration, obtain oil soluble transparent liquid or viscous liquid.
Join in lubricating oil by above-mentioned obtained metal surface alloy agent in the ratio of 0.5wt%, the electronic spectrum (EDX) of the surface of friction pair element recorded as shown in Figure 1.
Following table is the resistance to compression abrasion resistance test result of metal surface alloy agent under different loads that above-mentioned 3 embodiments obtain.
From above-mentioned experimental data, metal surface alloy agent prepared by the embodiment of the present invention, not containing objectionable impuritiess such as sulphur, phosphorus, zinc, chlorine, has extreme pressure and antiwear behavior more better than ZDDP simultaneously, and frictional coefficient declines 70%, and wear scar diameter declines more than 80%.The energy spectrum analysis of Fig. 1 surface of friction pair can prove, this metal surface alloy agent long-term use in lubricating oil can form boracic in metallic surface, magnesium, molybdenum, iron, the alloy layer structure of titanium.
Claims (3)
1. a preparation method for metal surface alloy agent, comprises the following steps:
(1) preparation of metallic compound:
In a kettle., add 10g aluminum isopropylate, 15g titanic acid ester, 20g organic sulfonic acid calcium, 10g boric acid, 25g organic sulfonic acid magnesium and 5g ammonium molybdate under agitation successively, stir 1 hour, obtain brown viscous liquid;
(2) preparation of metal surface alloy agent:
The brown viscous liquid that 5g step (1) is obtained moves in autoclave, add 70g plam oil and 5g hydrochloric acid respectively, then autoclave is closed, pass into carbonic acid gas to supercritical pressure 72.9atm, be warming up to supercritical temperature 31.26 DEG C, react after 4 hours under agitation condition, after cooling, separatory, vacuum dehydration, obtain oil soluble transparent liquid or viscous liquid.
2. a preparation method for metal surface alloy agent, comprises the following steps:
(1) preparation of metallic compound:
In a kettle., add 12g Aluminate, 13g titanium isopropylate, 24g alkyl sodium salicylate, 12g boric acid, 21g magnesium nitrate and 3g organic-molybdenum under agitation successively, stir 1 hour, obtain brown viscous liquid;
(2) preparation of metal surface alloy agent:
The brown viscous liquid that 5g step (1) is obtained moves in autoclave, add 60g plam oil and 2g potassium permanganate respectively, then autoclave is closed, pass into carbonic acid gas to supercritical pressure 72.9atm, be warming up to supercritical temperature 31.26 DEG C, react after 4 hours under agitation condition, after cooling, separatory, vacuum dehydration, obtain oil soluble transparent liquid or viscous liquid.
3. a preparation method for metal surface alloy agent, comprises the following steps:
(1) preparation of metallic compound:
In a kettle., add 10g aluminum isopropylate, 15g titanic acid ester, 20g organic sulfonic acid calcium, 10g boric acid, 25g organic sulfonic acid magnesium and 5g ammonium molybdate under agitation successively, stir 1 hour, obtain brown viscous liquid;
(2) preparation of metal surface alloy agent:
The brown viscous liquid that 5g step (1) is obtained moves in autoclave, add 60g Oleum Cocois and 2g potassium permanganate respectively, then autoclave is closed, pass into carbonic acid gas to supercritical pressure 72.9atm, be warming up to supercritical temperature 31.26 DEG C, react after 4 hours under agitation condition, after cooling, separatory, vacuum dehydration, obtain oil soluble transparent liquid or viscous liquid.
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| CN106281582A (en) * | 2015-05-26 | 2017-01-04 | 深圳中嘉能源有限公司 | A kind of repairing type lubricant |
| CN113355147B (en) * | 2021-07-06 | 2023-01-17 | 清研检测（天津）有限公司 | Friction improver, preparation method thereof and lubricating oil containing friction improver |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967419A (en) * | 2010-11-02 | 2011-02-09 | 天津东方舜能润滑材料有限公司 | Ceramic alloy lubricating oil special for dredging workboat engine and preparation method thereof |
| CN103302286A (en) * | 2013-06-18 | 2013-09-18 | 江苏和昊激光科技有限公司 | Cobalt-based metal ceramic alloy powder exclusively used in laser cladding of turning tool |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967419A (en) * | 2010-11-02 | 2011-02-09 | 天津东方舜能润滑材料有限公司 | Ceramic alloy lubricating oil special for dredging workboat engine and preparation method thereof |
| CN103302286A (en) * | 2013-06-18 | 2013-09-18 | 江苏和昊激光科技有限公司 | Cobalt-based metal ceramic alloy powder exclusively used in laser cladding of turning tool |
Non-Patent Citations (1)
| Title |
|---|
| 施利毅等.纳米材料学.《纳米科技基础》.华东理工大学出版社,2005,第43-45页. * |
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