CN116622953A - Environment-friendly inorganic quenching liquid and preparation method thereof - Google Patents
Environment-friendly inorganic quenching liquid and preparation method thereof Download PDFInfo
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- CN116622953A CN116622953A CN202310608893.7A CN202310608893A CN116622953A CN 116622953 A CN116622953 A CN 116622953A CN 202310608893 A CN202310608893 A CN 202310608893A CN 116622953 A CN116622953 A CN 116622953A
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- 238000010791 quenching Methods 0.000 title claims abstract description 83
- 230000000171 quenching effect Effects 0.000 title claims abstract description 83
- 239000007788 liquid Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000002105 nanoparticle Substances 0.000 claims abstract description 49
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 34
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 34
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 239000013556 antirust agent Substances 0.000 claims abstract description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 11
- 239000001103 potassium chloride Substances 0.000 claims abstract description 11
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 11
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011780 sodium chloride Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 55
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 238000003760 magnetic stirring Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 21
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 239000004005 microsphere Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002211 L-ascorbic acid Substances 0.000 claims description 7
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 239000011449 brick Substances 0.000 claims description 7
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 7
- 239000001488 sodium phosphate Substances 0.000 claims description 7
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- -1 boric acid ester Chemical class 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract description 21
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 14
- 239000003921 oil Substances 0.000 description 8
- 238000007865 diluting Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000005619 boric acid group Chemical group 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009661 fatigue test Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
- C21D1/60—Aqueous agents
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Lubricants (AREA)
Abstract
The invention discloses an environment-friendly inorganic quenching liquid and a preparation method thereof, and belongs to the technical field of metal processing treatment. The quenching liquid disclosed by the invention is prepared from the following raw materials in percentage by weight: 20-30% of sodium chloride, 10-15% of potassium chloride, 10-15% of sodium silicate, 5-10% of porous nano particles, 1-1.2% of triethanolamine, 1-1.5% of polyvinylpyrrolidone, 1-3% of antirust agent and the balance of water, wherein the total amount is 100%. The quenching liquid obtained by the invention has the advantages that all the components are synergistic, the cooling speed is effectively controlled, the hardenability is strong, the hardness of the quenched workpiece is high and uniform, the quenching is not cracked, and the mechanical property of the workpiece is excellent. Meanwhile, the components are nontoxic, smokeless and free of harmful substance volatile matters, the quenching medium can be completely recycled, and the quenching medium is safe, green and environment-friendly and has wide economic value and market value.
Description
Technical Field
The invention belongs to the technical field of metal processing treatment, and particularly relates to an environment-friendly inorganic quenching liquid and a preparation method thereof.
Background
The heat treatment process is an important technical link for manufacturing various mechanical products, and the quality of the heat treatment workpiece is directly related to the service performance and service life of various mechanical products. The quenching process is an important core process of heat treatment, and is characterized in that after the workpiece is heated to a specified phase transition temperature region for heat preservation, the workpiece is rapidly cooled by cooling liquid, so that the workpiece can obtain the hardness and strength required by use. The cooling performance of the quenching medium directly influences the work piece cooling phase transition process and the generated structure after the work piece cooling. Thus directly affecting the service performance of the workpiece, and the research on the service performance is very important for each country.
The commonly used quenching media are water, quenching oil and the like, and due to the difference of cooling capacities of the water and the oil, a plurality of workpieces are often deformed and cracked when quenched by water, but the workpieces are not quenched completely and hard by oil, so that research and development of the field are very important in recent years in various countries. The searching of new quenching medium, especially the world energy crisis of the last century, the price of petroleum is rising, and the searching of alternative products of quenching oil is urgent.
At present, the quenching medium for replacing engine oil mainly comprises an organic water-soluble quenching agent (PAG, PVP and the like), an inorganic water-soluble quenching agent and the like, and the quenching medium of an organic matter has the problems of easy deterioration, short service life and the like. And simultaneously, the conditions of large deformation or quenching crack and the like are easy to occur. For example, chinese patent application CN111004898A discloses a composition of oil-like quenching liquid and a preparation method thereof, wherein 5-15% of polyvinylpyrrolidone, 1-5% of polycarboxylic acid, 0-2% of defoamer, 0-2% of corrosion inhibitor and the balance of deionized water; the low-temperature cooling speed of the invention is lower, and the invention can be used for materials with high hardenability, but the high-temperature cooling speed is too low, and the high hardness requirement is not easy to be reached.
The inorganic water-soluble quenching liquid not only has the cooling capacity between water and oil, but also has good hardenability; meanwhile, the environment-friendly fire-resistant water-based paint has the advantages of no toxicity, no harmful gas, no fire hazard, no environmental pollution, low cost and the like, can be used for a long time, and is simple in later maintenance. However, various problems remain in the inorganic quenching liquid in the prior art.
For example, chinese patent application CN102061365a discloses an inorganic polymer water-soluble quenching medium and a preparation method thereof, wherein 59-62 parts of polyaluminum chloride, 19-21 parts of 10% sodium hydroxide, 14-16 parts of zinc chloride, 11-13 parts of potassium chloride and the balance of water; the high cooling rate Wen Lengsu of the invention can reach the water level, but the low temperature stage cooling rate control capability is insufficient, so that deformation and cracking exist.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the inorganic quenching medium which has the advantages of stable and easily controlled cooling rate, stable performance, difficult deterioration, safety and environmental protection, and few cracks and excellent performance of the obtained quenching parts.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
an environment-friendly inorganic quenching liquid is prepared from the following raw materials in percentage by weight: 20-30% of sodium chloride, 10-15% of potassium chloride, 10-15% of sodium silicate, 5-10% of porous nano particles, 1-1.2% of triethanolamine, 1-1.5% of polyvinylpyrrolidone, 1-3% of antirust agent and the balance of water, wherein the total amount is 100%.
Further, the sodium silicate modulus is not greater than 2.
Further, the preparation method of the porous nanoparticle comprises the following steps:
(1) 10mL of 2mol/L NaOH solution is dripped into 100mLCuCl under the magnetic stirring of 55 ℃ water bath 2 ·2H 2 O aqueous solution, reacting for 30min, adding 10mL of 0.5mol/L ascorbic acid solution into the solution, centrifuging and washing after the solution turns into brick red, and vacuum drying at 40deg.C for 12h to obtain Cu 2 An O template;
(2) Under the conditions of ultrasonic and magnetic stirring, 10g of Cu is added 2 Dispersing the O template in 100mL of ethanol solution, dropwise adding 50mL of tetrabutyl titanate into the solution, keeping the temperature at 50-80 ℃, continuously stirring for reaction for 3-5h, and centrifuging, filtering, washing and drying to obtain Cu with the surface coated with titanium oxide 2 O microspheres;
(3) The microspheres obtained in the step (2) are mixed according to a solid-to-liquid ratio of 1g:10mL of ultrasonic dispersion is carried out in deionized water, 10-20mL of 1mol/L sodium hydroxide solution is added under the condition of heating at 70-80 ℃ and stirring, after continuous reaction, the porous nano particles are obtained through centrifugation, filtration, washing, drying and roasting.
Further, the mass concentration of the ethanol solution in the step (2) is 50%.
The average particle diameter of the obtained porous nano particles is 10-20nm.
Further, the antirust agent is one or more of boric acid, boric acid ester and sodium phosphate.
Further, when the inorganic quenching liquid is used, water is used for preparing a diluting liquid with the weight percentage of 20 percent.
The preparation method of the environment-friendly inorganic quenching liquid comprises the following steps:
(1) Preparing porous nano particles: 10mL of 2mol/L NaOH solution is dripped into 100mLCuCl under the magnetic stirring of 55 ℃ water bath 2 ·2H 2 O aqueous solution, reacting for 30min, adding 10mL of 0.5mol/L ascorbic acid solution into the solution, centrifuging and washing after the solution turns into brick red, and vacuum drying at 40deg.C for 12h to obtain Cu 2 An O template; under the conditions of ultrasonic and magnetic stirring, 10g of Cu is added 2 Dispersing the O template in 100mL of ethanol solution, dropwise adding 50mL of tetrabutyl titanate into the solution, keeping the temperature at 50-80 ℃, continuously stirring for reaction for 3-5h, and centrifuging, filtering, washing and drying to obtain Cu with the surface coated with titanium oxide 2 O microspheres; the obtained microspheres have a solid-to-liquid ratio of 1g:
dispersing 10mL of ultrasonic wave in deionized water, adding 10-20mL of 1mol/L sodium hydroxide solution under the condition of heating at 70-80 ℃ and stirring, continuously reacting, centrifuging, filtering, washing, drying and roasting to obtain porous nano particles;
(2) Uniformly dispersing sodium silicate and porous nano particles in water according to parts by weight, carrying out ultrasonic and magnetic stirring for 1-2 hours to enable the porous nano particles to fully adsorb the sodium silicate, uniformly dispersing the rest raw materials in the water, and continuously stirring and uniformly mixing to obtain a finished quenching liquid.
The quenching liquid is composed of inorganic salt and the like, wherein sodium chloride, potassium chloride and the like are favorable for membrane rupture in a high-temperature region, after a high-temperature workpiece is immersed in the cooling medium, salt and alkali crystals are separated out in a vapor membrane stage and burst immediately, the vapor membrane is destroyed, and oxide skin on the surface of the workpiece is also burst, so that the cooling capacity of the medium in the high-temperature region can be improved.
Meanwhile, inorganic salt crystals can generate solidification bonding reaction with added low-modulus sodium silicate to form a heat-insulating film, so that the low-temperature cooling speed is reduced, and the heat-insulating film formed by bonding is easy to break.
The invention adds a small amount of polyvinylpyrrolidone, which has excellent solubility, film forming property and bonding dispersibility, on one hand can promote the uniform dispersion of porous nano particles, on the other hand, can be matched with inorganic salt and the like, and can integrally improve the cooling rate control capability of quenching liquid, thereby achieving the purposes of high Wen Lengsu speed and low-temperature cooling rate.
The invention also adds triethanolamine, antirust agent and other components to provide base number reserve and corrosion protection for the quenching liquid, and assists in improving the corrosion resistance of the workpiece.
Compared with the prior art, the invention has the following beneficial effects:
the quenching liquid obtained by the invention has the advantages that all the components are synergistic, the cooling speed is effectively controlled, the hardenability is strong, the hardness of the quenched workpiece is high and uniform, the quenching is not cracked, and the mechanical property of the workpiece is excellent. Meanwhile, the components are nontoxic, smokeless and free of harmful substance volatile matters, the quenching medium can be completely recycled, and the quenching medium is safe, green and environment-friendly and has wide economic value and market value.
Drawings
FIG. 1 is a graph showing thermal fatigue surface cracking of a test piece in the quenching liquid obtained in example 4 and comparative examples 1 to 4;
FIG. 2 is an SEM image of porous nanoparticles prepared in example 4 of the present invention.
Detailed Description
The technical scheme of the present invention is further described below with reference to specific examples, but is not limited thereto.
Example 1
An environment-friendly inorganic quenching liquid is prepared from the following raw materials in percentage by weight: 20% of sodium chloride, 10% of potassium chloride, 10% of sodium silicate, 5% of porous nano particles, 1% of triethanolamine, 1% of polyvinylpyrrolidone, 1% of antirust agent and the balance of water, wherein the total amount is 100%.
The sodium silicate modulus is not greater than 2.
The preparation method of the porous nano particles comprises the following steps:
(1) 10mL of 2mol/L NaOH solution is dripped into 100mLCuCl under the magnetic stirring of 55 ℃ water bath 2 ·2H 2 O aqueous solution, reacting for 30min, adding 10mL of 0.5mol/L ascorbic acid solution into the solution, centrifuging and washing after the solution turns into brick red, and vacuum drying at 40deg.C for 12h to obtain Cu 2 An O template;
(2) Under the conditions of ultrasonic and magnetic stirring, 10g of Cu is added 2 Dispersing the O template in 100mL of ethanol solution, dropwise adding 50mL of tetrabutyl titanate into the solution, keeping the temperature at 50 ℃, continuously stirring for reaction for 3 hours, centrifuging, filtering, washing and drying to obtain Cu with titanium oxide coated on the surface 2 O microspheres;
(3) The microspheres obtained in the step (2) are mixed according to a solid-to-liquid ratio of 1g:10mL of ultrasonic dispersion is carried out in deionized water, 10mL of 1mol/L sodium hydroxide solution is added under the condition of heating at 70 ℃ and stirring, and after continuous reaction, the porous nano particles are obtained through centrifugation, filtration, washing, drying and roasting.
The mass concentration of the ethanol solution in the step (2) is 50%.
The rust inhibitor is boric acid.
When the inorganic quenching liquid is used, water is used for preparing a diluting liquid with the weight percentage of 20 percent.
The preparation method of the environment-friendly inorganic quenching liquid comprises the following steps:
(1) Preparing porous nano particles;
(2) Uniformly dispersing sodium silicate and porous nano particles in water according to parts by weight, carrying out ultrasonic and magnetic stirring for 1h to enable the porous nano particles to fully adsorb the sodium silicate, uniformly dispersing the rest raw materials therein, and continuously stirring and uniformly mixing to obtain a finished quenching liquid.
Example 2
An environment-friendly inorganic quenching liquid is prepared from the following raw materials in percentage by weight: 25% of sodium chloride, 13% of potassium chloride, 12% of sodium silicate, 7% of porous nano particles, 1% of triethanolamine, 1% of polyvinylpyrrolidone, 1% of antirust agent and the balance of water, wherein the total amount is 100%.
The sodium silicate modulus is not greater than 2.
The preparation method of the porous nano particles comprises the following steps:
(1) 10mL of 2mol/L NaOH solution is dripped into 100mLCuCl under the magnetic stirring of 55 ℃ water bath 2 ·2H 2 O aqueous solution, reacting for 30min, adding 10mL of 0.5mol/L ascorbic acid solution into the solution, centrifuging and washing after the solution turns into brick red, and vacuum drying at 40deg.C for 12h to obtain Cu 2 An O template;
(2) Under the conditions of ultrasonic and magnetic stirring, 10g of Cu is added 2 Dispersing the O template in 100mL of ethanol solution, dropwise adding 50mL of tetrabutyl titanate into the solution, keeping the temperature at 60 ℃, continuously stirring and reacting for 4 hours, centrifuging, filtering, washing and drying to obtain Cu with titanium oxide coated on the surface 2 O microspheres;
(3) The microspheres obtained in the step (2) are mixed according to a solid-to-liquid ratio of 1g:10mL of ultrasonic dispersion is carried out in deionized water, 20mL of 1mol/L sodium hydroxide solution is added under the condition of heating at 70 ℃ and stirring, and after continuous reaction, the porous nano particles are obtained through centrifugation, filtration, washing, drying and roasting.
The mass concentration of the ethanol solution in the step (2) is 50%.
The antirust agent is sodium phosphate.
When the inorganic quenching liquid is used, water is used for preparing a diluting liquid with the weight percentage of 20 percent.
The preparation method of the environment-friendly inorganic quenching liquid comprises the following steps:
(1) Preparing porous nano particles;
(2) Uniformly dispersing sodium silicate and porous nano particles in water according to parts by weight, carrying out ultrasonic and magnetic stirring for 2 hours to enable the porous nano particles to fully adsorb the sodium silicate, uniformly dispersing the rest raw materials therein, and continuously stirring and uniformly mixing to obtain a finished quenching liquid.
Example 3
An environment-friendly inorganic quenching liquid is prepared from the following raw materials in percentage by weight: 30% of sodium chloride, 10% of potassium chloride, 13% of sodium silicate, 7% of porous nano particles, 1.2% of triethanolamine, 1.5% of polyvinylpyrrolidone, 3% of antirust agent and the balance of water, wherein the total amount is 100%.
The sodium silicate modulus is not greater than 2.
The preparation method of the porous nano particles comprises the following steps:
(1) 10mL of 2mol/L NaOH solution is dripped into 100mLCuCl under the magnetic stirring of 55 ℃ water bath 2 ·2H 2 O aqueous solution, reacting for 30min, adding 10mL of 0.5mol/L ascorbic acid solution into the solution, centrifuging and washing after the solution turns into brick red, and vacuum drying at 40deg.C for 12h to obtain Cu 2 An O template;
(2) Under the conditions of ultrasonic and magnetic stirring, 10g of Cu is added 2 Dispersing the O template in 100mL of ethanol solution, dropwise adding 50mL of tetrabutyl titanate into the solution, keeping the temperature at 80 ℃, continuously stirring and reacting for 4 hours, centrifuging, filtering, washing and drying to obtain Cu with the surface coated with titanium oxide 2 O microspheres;
(3) The microspheres obtained in the step (2) are mixed according to a solid-to-liquid ratio of 1g:10mL of ultrasonic dispersion is carried out in deionized water, 20mL of 1mol/L sodium hydroxide solution is added under the condition of heating at 80 ℃ and stirring, and after continuous reaction, the porous nano particles are obtained through centrifugation, filtration, washing, drying and roasting.
The mass concentration of the ethanol solution in the step (2) is 50%.
The antirust agent is sodium phosphate.
When the inorganic quenching liquid is used, water is used for preparing a diluting liquid with the weight percentage of 20 percent.
The preparation method of the environment-friendly inorganic quenching liquid comprises the following steps:
(1) Preparing porous nano particles;
(2) Uniformly dispersing sodium silicate and porous nano particles in water according to parts by weight, carrying out ultrasonic and magnetic stirring for 2 hours to enable the porous nano particles to fully adsorb the sodium silicate, uniformly dispersing the rest raw materials therein, and continuously stirring and uniformly mixing to obtain a finished quenching liquid.
Example 4
An environment-friendly inorganic quenching liquid is prepared from the following raw materials in percentage by weight: 30% of sodium chloride, 15% of potassium chloride, 15% of sodium silicate, 10% of porous nano particles, 1.2% of triethanolamine, 1.5% of polyvinylpyrrolidone, 3% of antirust agent and the balance of water, wherein the total amount is 100%.
The sodium silicate modulus is not greater than 2.
The preparation method of the porous nano particles comprises the following steps:
(1) 10mL of 2mol/L NaOH solution is dripped into 100mLCuCl under the magnetic stirring of 55 ℃ water bath 2 ·2H 2 O aqueous solution, reacting for 30min, adding 10mL of 0.5mol/L ascorbic acid solution into the solution, centrifuging and washing after the solution turns into brick red, and vacuum drying at 40deg.C for 12h to obtain Cu 2 An O template;
(2) Under the conditions of ultrasonic and magnetic stirring, 10g of Cu is added 2 Dispersing the O template in 100mL of ethanol solution, dropwise adding 50mL of tetrabutyl titanate into the solution, keeping the temperature at 80 ℃, continuously stirring and reacting for 5 hours, centrifuging, filtering, washing and drying to obtain Cu with the surface coated with titanium oxide 2 O microspheres;
(3) The microspheres obtained in the step (2) are mixed according to a solid-to-liquid ratio of 1g:10mL of ultrasonic dispersion is carried out in deionized water, 20mL of 1mol/L sodium hydroxide solution is added under the condition of heating at 80 ℃ and stirring, and after continuous reaction, the porous nano particles are obtained through centrifugation, filtration, washing, drying and roasting.
The mass concentration of the ethanol solution in the step (2) is 50%.
The antirust agent is sodium phosphate.
When the inorganic quenching liquid is used, water is used for preparing a diluting liquid with the weight percentage of 20 percent.
The preparation method of the environment-friendly inorganic quenching liquid comprises the following steps:
(1) Preparing porous nano particles;
(2) Uniformly dispersing sodium silicate and porous nano particles in water according to parts by weight, carrying out ultrasonic and magnetic stirring for 2 hours to enable the porous nano particles to fully adsorb the sodium silicate, uniformly dispersing the rest raw materials therein, and continuously stirring and uniformly mixing to obtain a finished quenching liquid.
Comparative example 1
An environment-friendly inorganic quenching liquid is prepared from the following raw materials in percentage by weight: 30% of sodium chloride, 15% of potassium chloride, 15% of sodium silicate, 1.2% of triethanolamine, 1.5% of polyvinylpyrrolidone, 3% of antirust agent and the balance of water, wherein the total amount is 100%.
The sodium silicate modulus is not greater than 2.
The antirust agent is sodium phosphate.
When the inorganic quenching liquid is used, water is used for preparing a diluting liquid with the weight percentage of 20 percent.
The preparation method of the environment-friendly inorganic quenching liquid comprises the following steps:
(1) Uniformly dispersing sodium silicate in water according to parts by weight, carrying out ultrasonic and magnetic stirring for 2 hours, uniformly dispersing the rest raw materials in the water, and continuously stirring and uniformly mixing to obtain a finished quenching liquid.
The comparative example is the same as example 4 except that no porous nanoparticles are added.
Comparative example 2
An environment-friendly inorganic quenching liquid is prepared from the following raw materials in percentage by weight: 30% of sodium chloride, 15% of potassium chloride, 15% of sodium silicate, 10% of nano particles, 1.2% of triethanolamine, 1.5% of polyvinylpyrrolidone, 3% of antirust agent and the balance of water, wherein the total amount is 100%.
The sodium silicate modulus is not greater than 2.
The nano particles are nano titanium dioxide, and the average particle size is 10-20nm.
The antirust agent is sodium phosphate.
When the inorganic quenching liquid is used, water is used for preparing a diluting liquid with the weight percentage of 20 percent.
The preparation method of the environment-friendly inorganic quenching liquid comprises the following steps:
(1) Uniformly dispersing sodium silicate and nano particles in water according to parts by weight, carrying out ultrasonic and magnetic stirring for 2 hours, uniformly dispersing the rest raw materials in the water, and continuously stirring and uniformly mixing to obtain the finished quenching liquid.
In this comparative example, the raw materials and the preparation method were the same as in example 4, except that the porous nano particles were replaced with nano titanium dioxide having the same particle size.
Comparative example 3
The commercially available quenching oil was used, and the comparative example was selected with respect to the quenching oil GL11 produced by Jiangsu Yingji lubrication technologies Co.
Comparative example 4
Water is used as quenching liquid.
Performance testing
Cooling performance measurement: according to the national standard: GB/T7951 (ISO 9950).
Hardenability measurement: according to national standard GB225-88 (method for testing hardenability end quenching of steel).
And (3) measuring the surface induced crack performance of the quenched workpiece: and (4) grading the surface cracks of the workpiece according to a national standard GB/T15824-2008 (thermal fatigue crack on the surface of the steel part) test method.
Test piece:
and quenching the 30CrMnSi test piece with the diameter of 20mm at 880 ℃ respectively, preserving heat for 20 minutes after the temperature of the workpiece is reached, quenching in different media, and measuring cooling performance respectively.
Quenching medium: examples 1 to 4 and comparative examples 1 to 4.
Table 1 test results
TABLE 2 mechanical test results
As can be seen from the data in tables 1-2, the quenching liquid in the embodiment of the invention has ideal cooling performance and can improve the heat treatment quality of the workpiece. According to the quenching liquid disclosed by the embodiment of the invention, under the addition of the porous nano particles, the bonding effect of sodium silicate is matched, so that the cooling speed is effectively controlled, the cooling speed is higher at high temperature, and the speed in a low-temperature area is lower, thus the transformation speed of martensite can be reduced, the tissue stress during quenching is greatly reduced, the cracking tendency is reduced, and the hardness of a workpiece is improved. In comparative examples 1 to 2, in which no porous nanoparticle or ordinary nano titanium dioxide was added, the interaction between the porous nanoparticle and sodium silicate disappeared or weakened, the temperature controlling ability of the quenching liquid was remarkably lowered, and the properties of the obtained workpiece were weaker than those of the examples.
Meanwhile, as can be seen from the thermal fatigue test chart 1, the quenching media under 1000 cycles of cold and hot treatment have cracks with different degrees on the surface of the sample, and the cracks are netlike. The cracks in the water quenched state of comparative example 4 were strong, were mainly cracks in the left-right direction, and had crack growth. Whereas the thermal fatigue cracks of the examples and comparative examples exhibited finer meshes, the direction was at an angle to the horizontal, with slight crack propagation. The crack growth was slower for example 4 and comparative example 3 (oil), and comparative examples 1-2 exhibited deeper fine cracks.
It should be noted that the above-mentioned embodiments are merely some, but not all embodiments of the preferred mode of carrying out the invention. It is evident that all other embodiments obtained by a person skilled in the art without making any inventive effort, based on the above-described embodiments of the invention, shall fall within the scope of protection of the invention.
Claims (7)
1. The environment-friendly inorganic quenching liquid is characterized by comprising the following raw materials in percentage by weight: 20-30% of sodium chloride, 10-15% of potassium chloride, 10-15% of sodium silicate, 5-10% of porous nano particles, 1-1.2% of triethanolamine, 1-1.5% of polyvinylpyrrolidone, 1-3% of antirust agent and the balance of water, wherein the total amount is 100%.
2. The environmentally friendly inorganic quenching liquid of claim 1 wherein the sodium silicate modulus is no greater than 2.
3. The environment-friendly inorganic quenching liquid as claimed in claim 1, wherein the preparation method of the porous nano particles is as follows:
(1) 10mL of 2mol/L NaOH solution is dripped into 100mLCuCl under the magnetic stirring of 55 ℃ water bath 2 ·2H 2 O aqueous solution, reacting for 30min, adding 10mL of 0.5mol/L ascorbic acid solution into the solution, centrifuging and washing after the solution turns into brick red, and vacuum drying at 40deg.C for 12h to obtain Cu 2 An O template;
(2) Under the conditions of ultrasonic and magnetic stirring, 10g of Cu is added 2 Dispersing the O template in 100mL of ethanol solution, dropwise adding 50mL of tetrabutyl titanate into the solution, keeping the temperature at 50-80 ℃, continuously stirring for reaction for 3-5h, and centrifuging, filtering, washing and drying to obtain Cu with the surface coated with titanium oxide 2 O microspheres;
(3) The microspheres obtained in the step (2) are mixed according to a solid-to-liquid ratio of 1g:10mL of ultrasonic dispersion is carried out in deionized water, 10-20mL of 1mol/L sodium hydroxide solution is added under the condition of heating at 70-80 ℃ and stirring, after continuous reaction, the porous nano particles are obtained through centrifugation, filtration, washing, drying and roasting.
4. The environment-friendly inorganic quenching liquid as claimed in claim 3, wherein the mass concentration of the ethanol solution in the step (2) is 50%.
5. The environment-friendly inorganic quenching liquid according to claim 1, wherein the rust inhibitor is one or more of boric acid, boric acid ester and sodium phosphate.
6. The environment-friendly inorganic quenching liquid according to any one of claims 1 to 5, wherein when the inorganic quenching liquid is used, water is used to prepare a dilution liquid with the weight percentage of 20 percent.
7. A method for preparing the environment-friendly inorganic quenching liquid according to any one of claims 1 to 6, which is characterized by comprising the following steps:
(1) Preparing porous nano particles;
(2) Uniformly dispersing sodium silicate and porous nano particles in water according to parts by weight, carrying out ultrasonic and magnetic stirring for 1-2 hours to enable the porous nano particles to fully adsorb the sodium silicate, uniformly dispersing the rest raw materials in the water, and continuously stirring and uniformly mixing to obtain a finished quenching liquid.
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