Rapid quenching oil and preparation method thereof

Abstract

The invention discloses rapid quenching oil and a preparation method thereof. The rapid quenching oil comprises the following components in percentage by mass: 0.5%-2% of a low-temperature cooling accelerant, 3%-5% of a high-temperature cooling accelerant, 0.5%-1% of an antioxidant, 0.5%-2% of a dispersing agent, 0.1%-1% of a surfactant, 0.5%-1.5% of an antirust agent and the balance of base oil. Wherein the low-temperature cooling accelerant is C10-C25 alkyl sulfonate, and the surface active agent is a gemini quaternary ammonium salt surface active agent. According to the quenching oil, a small amount of gemini quaternary ammonium salt surfactant is introduced into the formula of the quenching oil, so that the cooling performance of the quenching oil can be improved, and the quenching oil has good dehydration property. On the whole, the rapid quenching oil has the advantages of being simple in preparation process, high in stability, long in service life and good in cooling performance.

Description

Technical Field

[0001] The invention relates to the technical field of quenching oil, in particular to a rapid quenching oil and a preparation method thereof. Background Art

[0002] The quenching process refers to the process of heating the workpiece to a certain temperature, keeping it warm, and then dissipating the heat through various cooling media to make the workpiece cool quickly. As a major and important process in the material heat treatment process, it determines many properties of the workpiece. In actual production, different workpieces have different application scenarios and uses, and require workpiece materials to have different mechanical properties. Through the quenching cooling rate, different material phases and organizational structures are obtained, so that the relevant performance of the workpiece meets the needs of its use scenario.

[0003] During the quenching and cooling process, the cooling medium is the quenching liquid, and the various physical and chemical properties of the quenching liquid are such as viscosity, fluidity, chemical volatility, and fluidity during the quenching process. These properties can directly affect the performance of the workpiece. In a sense, quenching and cooling are related to the success or failure of the entire heat treatment, so the performance of the quenching liquid has attracted widespread attention. CN111074045A discloses a fast bright quenching oil and a preparation method thereof, wherein the quenching oil comprises 80-92% of base oil, 4-10% of accelerator, 1.5-5% of surfactant, 0.5-3% of auxiliary dispersant, and 0.5-2% of antioxidant by mass percentage, and has excellent cooling performance, thermal oxidation stability, and brightness. CN107523670A discloses a quenching oil and a preparation method thereof, wherein the quenching oil comprises 75% of base oil, 10% of accelerator, 4% of antioxidant, 6% of trimethylsilyl trifluoroacetate, and 5% of carbitol acetate by mass percentage, and can still improve the brightness of the workpiece after being stored in an adverse environment.

[0004] At present, the types and proportions of base oils in quenching oil are relatively fixed. It is still very important to improve other formulas and enhance the cooling performance and service life of quenching oil. Summary of the invention

[0005] In order to overcome the problems existing in the prior art, the present invention provides a rapid quenching oil, which comprises, by mass percentage,

[0006] 0.5%~2% low-temperature accelerator, 3%~5% high-temperature accelerator, 0.5%~1% antioxidant, 0.5%~2% dispersant, 0.1%~1% surfactant, 0.5%~1.5% rust inhibitor, and base oil as the balance.

[0007] Wherein, the low temperature refrigeration agent is C 10 ~C 25Alkyl sulfonate, the surfactant is a gemini quaternary ammonium salt surfactant. 10 ~C 25 The alkyl sulfonate means that the number of carbon atoms in the alkyl sulfonate is 10 to 25.

[0008] The low temperature quenching agent used in the present invention is C 10 ~C 25 Alkyl sulfonate, adding in quenching oil can play the effect of accelerating low temperature stage speed, can timely neutralize the acidic substance generated in oil product, maintain the stability of oil product performance. However, because sulfonate is a surfactant product, it is easy to emulsify when meeting water, if water content is higher in quenching oil, it can promote the formation of oxidative acidification and oil sludge, and oil sludge can cause the moisture in quenching oil to be difficult to settle and separate, affecting the life-span of quenching oil. On this basis, the present invention has also added gemini quaternary ammonium salt surfactant in formula, and gemini quaternary ammonium salt molecular structure is connected by two quaternary ammonium salt parts through linking group, which gives its excellent dispersibility, solubility, antistatic property and gentle surface activity. By introducing gemini quaternary ammonium salt in formula, simultaneously with alkyl sulfonate in suitable ratio, not only can the cooling performance of quenching oil be improved, but also can make quenching oil have good dehydration.

[0009] Furthermore, the mass ratio of the low-temperature refrigeration agent to the gemini quaternary ammonium salt surfactant is 3-10:1.

[0010] Furthermore, the gemini quaternary ammonium salt surfactant includes at least one of N,N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt, N,N'-bis(octadecyldimethyl)-1,2-dibromide ethylenediammonium salt, N,N'-dimethyl-N,N'-di(2-hydroxyethyl)octanamide gemini quaternary ammonium salt, and N,N'-ethylenebis(methylaminoformamide) gemini quaternary ammonium salt.

[0011] When the hot workpiece is immersed in the quenching medium and the liquid phase and the solid phase are in contact with each other, the quenching and cooling process of the workpiece has begun. The three cooling stages of quenching are, in order, the steam film cooling stage, the boiling cooling stage, and the convection cooling stage. The high-temperature accelerator can pierce the steam film of the quenching medium as early as possible, quickly make the cooling process enter the boiling stage with the most intense cooling rate, and accelerate the cooling rate of the high-temperature stage of quenching cooling. The low-temperature accelerator can make the quenching medium maintain a certain cooling rate at low temperatures, maintain a certain depth of the hardened layer of the quenched workpiece, and enhance the hardening ability of the quenching oil.

[0012] Furthermore, the high-temperature refrigeration agent includes at least one of ethylene-propylene copolymer, polypropylene, polybutene, polyisobutylene, polyisobutylene succinate, and polyisobutylene succinimide.

[0013] The oxidation of quenching oil depends not only on the type of base oil, but also on contact oxidation with air at high temperature and catalytic oxidation of quenching furnace parts. In order to ensure the service life of the oil and the quenching effect, antioxidants must be added to the isothermal quenching oil. Antioxidants can be divided into two types according to their types: phenolic antioxidants and amine antioxidants. Phenolic antioxidants are mainly used in low temperature occasions and have obvious anti-oxidation effects. When the temperature exceeds 100°C, amine antioxidants have better effects.

[0014] Furthermore, the antioxidant includes at least one of a phenolic antioxidant and an amine antioxidant.

[0015] During the use of quenching oil, oxidative polymerization and high-temperature decomposition will occur, producing acidified substances and sintered carbonized substances. These substances will stick together and deteriorate the surface quality of the quenched workpiece, shorten the life of the quenching oil, and affect the quenching cooling rate. Dispersants are needed to evenly disperse and dissolve soot, oxidized acid, and sludge substances in the quenching oil.

[0016] Furthermore, the dispersant includes at least one of sulfur-phosphorylated polyisobutylene polyoxyethylene ester, polyisobutylene succinate, dimethyl phosphate, calcium alkyl salicylate, and alkyl phenol salt.

[0017] Adding rust inhibitors to the quenching oil helps keep the workpiece bright after quenching.

[0018] Furthermore, the rust inhibitor includes at least one of calcium petroleum sulfonate, barium petroleum sulfonate, and barium dinonylnaphthalene sulfonate.

[0019] In the SH / T 0564-93 standard heat treatment oil of the petrochemical industry of the People's Republic of China, the kinematic viscosity of the rapid quenching oil at 40°C is required to be lower than 26 cSt.

[0020] Furthermore, the kinematic viscosity of the base oil at 40° C. is lower than 25 cSt.

[0021] The present invention also provides a method for preparing the above-mentioned rapid quenching oil, comprising:

[0022] The base oil, antioxidant, dispersant and rust inhibitor are stirred and mixed at elevated temperature, and then a low-temperature quenching agent, a high-temperature quenching agent and a surfactant are added and continued to be stirred and mixed to obtain a rapid quenching oil.

[0023] Furthermore, the temperature is increased to 60-100° C. at a rate of 0.2-0.5° C. / s.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] The invention introduces a small amount of gemini quaternary ammonium salt surfactant into the quenching oil formula, which can not only improve the cooling performance of the quenching oil, but also make the quenching oil have good dehydration. Overall, the rapid quenching oil of the invention has the advantages of simple preparation process, high stability, long service life and good cooling performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is the rapid quenching oil of the present invention. DETAILED DESCRIPTION

[0027] The endpoints and any values ​​of the ranges disclosed in the present invention are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more numerical ranges, which should be regarded as specifically disclosed in the present invention.

[0028] Some of the raw materials used in the embodiments of the present invention are described as follows:

[0029] The low-temperature refrigeration agent is sodium octadecyl sulfonate, brand Runfeng, purchased from Jiangsu Runfeng Synthetic Technology Co., Ltd.;

[0030] The high temperature quenching agent was polyisobutylene, model PB1300, purchased from Dalin, South Korea;

[0031] The antioxidant was alkyl diphenylamine, model L57, purchased from Panhua Chemical (Shanghai) Co., Ltd.;

[0032] The dispersant was selected as calcium alkyl salicylate, model T109, purchased from Hebei Tuochi Lubricant Sales Co., Ltd.;

[0033] The gemini quaternary ammonium salt was selected as N, N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt, model RY101, purchased from Guangzhou Ruiyang Surfactant Co., Ltd.;

[0034] The rust inhibitor was selected as barium petroleum sulfonate, model T701, purchased from Shandong Yunxin New Materials Technology Co., Ltd.;

[0035] The base oil is a paraffinic mineral base oil having a kinematic viscosity of about 20 cSt at 40°C.

[0036] Other raw materials not mentioned are common raw materials in the art. The above content is only to help illustrate the present invention and should not be construed as a strict limitation of the present invention. Those skilled in the art can directly purchase or prepare the same / similar raw materials from the market. These contents will not be repeated in the examples.

[0037] The following will be combined with the specific embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0038] Example 1

[0039] A method for preparing rapid quenching oil, the steps are as follows:

[0040] S1. Ingredients by mass percentage: 1% sodium octadecyl sulfonate, 4% polyisobutylene, 0.5% alkyl diphenylamine, 1.5% calcium alkyl salicylate, 1% N, N'-bis (hexadecyl dimethyl) -1,2- dibromide ethylene diammonium salt, 1% barium petroleum sulfonate, 91% paraffin-based mineral base oil;

[0041] S2, mixing paraffin-based mineral base oil, alkyl diphenylamine, alkyl calcium salicylate and barium petroleum sulfonate at a stirring rate of 80 rpm, heating to 80° C. at a heating rate of 0.5° C. / s, and maintaining the temperature and stirring for 30 min to obtain a mixed oil;

[0042] S3. Add sodium octadecylsulfonate, polyisobutylene, and N,N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt to the mixed oil, and continue stirring at 80°C and 80 rpm for 2 h to obtain rapid quenching oil.

[0043] Example 2

[0044] A method for preparing rapid quenching oil, the steps are as follows:

[0045] S1. Ingredients by mass percentage: 1.5% sodium octadecyl sulfonate, 4% polyisobutylene, 0.5% alkyl diphenylamine, 1.5% calcium alkyl salicylate, 0.5% N, N'-bis (hexadecyl dimethyl) -1,2- dibromide ethylene diammonium salt, 1% barium petroleum sulfonate, 91% paraffin-based mineral base oil;

[0046] S2, mixing paraffin-based mineral base oil, alkyl diphenylamine, alkyl calcium salicylate and barium petroleum sulfonate at a stirring rate of 80 rpm, heating to 80° C. at a heating rate of 0.5° C. / s, and maintaining the temperature and stirring for 30 min to obtain a mixed oil;

[0047] S3. Add sodium octadecylsulfonate, polyisobutylene, and N,N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt to the mixed oil, and continue stirring at 80°C and 80 rpm for 2 h to obtain rapid quenching oil.

[0048] Example 3

[0049] A method for preparing rapid quenching oil, the steps are as follows:

[0050] S1. Ingredients by mass percentage: 1.6% sodium octadecyl sulfonate, 4% polyisobutylene, 0.5% alkyl diphenylamine, 1.5% calcium alkyl salicylate, 0.4% N, N'-bis (hexadecyl dimethyl) -1,2- dibromide ethylene diammonium salt, 1% barium petroleum sulfonate, 91% paraffin-based mineral base oil;

[0051] S2, mixing paraffin-based mineral base oil, alkyl diphenylamine, alkyl calcium salicylate and barium petroleum sulfonate at a stirring rate of 80 rpm, heating to 80° C. at a heating rate of 0.5° C. / s, and maintaining the temperature and stirring for 30 min to obtain a mixed oil;

[0052] S3. Add sodium octadecylsulfonate, polyisobutylene, and N,N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt to the mixed oil, and continue stirring at 80°C and 80 rpm for 2 h to obtain rapid quenching oil.

[0053] Example 4

[0054] A method for preparing rapid quenching oil, the steps are as follows:

[0055] S1. Ingredients by mass percentage: 1.8% sodium octadecyl sulfonate, 4% polyisobutylene, 0.5% alkyl diphenylamine, 1.5% calcium alkyl salicylate, 0.2% N, N'-bis (hexadecyl dimethyl) -1,2- dibromide ethylene diammonium salt, 1% barium petroleum sulfonate, 91% paraffin-based mineral base oil;

[0056] S2, mixing paraffin-based mineral base oil, alkyl diphenylamine, alkyl calcium salicylate and barium petroleum sulfonate at a stirring rate of 80 rpm, heating to 80° C. at a heating rate of 0.5° C. / s, and maintaining the temperature and stirring for 30 min to obtain a mixed oil;

[0057] S3. Add sodium octadecylsulfonate, polyisobutylene, and N,N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt to the mixed oil, and continue stirring at 80°C and 80 rpm for 2 h to obtain rapid quenching oil.

[0058] Comparative Example 1

[0059] A method for preparing rapid quenching oil, the steps are as follows:

[0060] S1. Ingredients by mass percentage: 1.9% sodium octadecyl sulfonate, 4% polyisobutylene, 0.5% alkyl diphenylamine, 1.5% calcium alkyl salicylate, 0.1% N, N'-bis (hexadecyl dimethyl) -1,2- dibromide ethylene diammonium salt, 1% barium petroleum sulfonate, 91% paraffin-based mineral base oil;

[0061] S2, mixing paraffin-based mineral base oil, alkyl diphenylamine, alkyl calcium salicylate and barium petroleum sulfonate at a stirring rate of 80 rpm, heating to 80° C. at a heating rate of 0.5° C. / s, and maintaining the temperature and stirring for 30 min to obtain a mixed oil;

[0062] S3. Add sodium octadecylsulfonate, polyisobutylene, and N,N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt to the mixed oil, and continue stirring at 80°C and 80 rpm for 2 h to obtain rapid quenching oil.

[0063] Comparative Example 2

[0064] A method for preparing rapid quenching oil, the steps are as follows:

[0065] S1. Ingredients by mass percentage: 2% sodium octadecyl sulfonate, 4% polyisobutylene, 0.5% alkyl diphenylamine, 1.5% calcium alkyl salicylate, 1% barium petroleum sulfonate, 91% paraffin-based mineral base oil;

[0066] S2, mixing paraffin-based mineral base oil, alkyl diphenylamine, alkyl calcium salicylate and barium petroleum sulfonate at a stirring rate of 80 rpm, heating to 80° C. at a heating rate of 0.5° C. / s, and maintaining the temperature and stirring for 30 min to obtain a mixed oil;

[0067] S3. Add sodium octadecyl sulfate and polyisobutylene to the mixed oil, and continue stirring at 80° C. and 80 rpm for 2 h to obtain rapid quenching oil.

[0068] Comparative Example 3

[0069] A method for preparing rapid quenching oil, the steps are as follows:

[0070] S1. Ingredients by mass percentage: 4% polyisobutylene, 0.5% alkyl diphenylamine, 1.5% calcium alkyl salicylate, 2% N, N'-bis (hexadecyl dimethyl) -1,2- dibromide ethylene diammonium salt, 1% barium petroleum sulfonate, 91% paraffin-based mineral base oil;

[0071] S2, mixing paraffin-based mineral base oil, alkyl diphenylamine, alkyl calcium salicylate and barium petroleum sulfonate at a stirring rate of 80 rpm, heating to 80° C. at a heating rate of 0.5° C. / s, and maintaining the temperature and stirring for 30 min to obtain a mixed oil;

[0072] S3, polyisobutylene, and N,N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt were added to the mixed oil, and the mixture was stirred at 80°C and 80 rpm for 2 h to obtain a rapid quenching oil.

[0073] Test Case

[0074] The maximum cooling rate of the quenching oil prepared in the embodiments of the present invention and the comparative example from 800°C to 400°C was tested with reference to the standard SH / T0220 "Determination of Cooling Performance of Heat Treatment Oil", and the results are shown in Table 1. Among them, for rapid quenching oil, the minimum cooling time is less than 4s, that is, the maximum cooling rate is required to be greater than 100°C / s.

[0075] Table 1 Maximum cooling rate of quenching oil

[0076] From the test results of Table 1, it can be seen that the maximum cooling rate of Comparative Example 3 without adding sodium octadecyl sulfonate is the lowest, because sodium octadecyl sulfonate as a low-temperature quenching agent maintains a certain cooling rate at a lower temperature, and N, N'-bis (hexadecyl dimethyl) -1, 2- dibromide ethylene diammonium salt is more used as a surfactant, and more is to improve the compatibility of the components. From Example 1 to Example 4 and Comparative Example 1, it can be seen that when the total proportion of sodium octadecyl sulfonate and N, N'-bis (hexadecyl dimethyl) -1, 2- dibromide ethylene diammonium salt is 2%, and other components remain unchanged, as the proportion of sodium octadecyl sulfonate increases, the maximum cooling rate shows a trend of first increasing and then decreasing, which may be because the compounding of sodium octadecyl sulfonate and N, N'-bis (hexadecyl dimethyl) -1, 2- dibromide ethylene diammonium salt strengthens the thixotropic property of the quenching oil system, thereby enhancing the cooling performance of the quenching oil.

[0077] 200 mL of the quenching oil prepared in the examples of the present invention and the comparative example were respectively mixed with 200 mL of water, stirred at 300 rpm for 5 min, and then allowed to stand for 15 min to allow the water to settle and separate, and the oil component was obtained. The dehydration rate was tested, and the results are shown in Table 2.

[0078] Table 2 Dehydration rate of quenching oil

[0079]

[0080] From the test results in Table 2, it can be seen that the quenching oil prepared in the embodiment of the present invention has a higher dehydration rate. However, in Comparative Examples 2 and 3, in which only sodium octadecyl sulfonate and N, N'-bis(hexadecyl dimethyl)-1,2-dibromethylene diammonium salt are added, their dehydration rates are worse than those of Examples 1-4 and Comparative Example 1. This result shows that the compounding of sodium octadecyl sulfonate and N, N'-bis(hexadecyl dimethyl)-1,2-dibromethylene diammonium salt is beneficial to improving the dehydration rate of quenching oil, and can reduce the interference caused by a large amount of sludge that may be generated when there is more water in the quenching oil, thereby improving the service life of the quenching oil.

[0081] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A rapid quenching oil, characterized in that: In terms of mass percentage, it includes: 0.5%~2% low-temperature accelerator, 3%~5% high-temperature accelerator, 0.5%~1% antioxidant, 0.5%~2% dispersant, 0.1%~1% surfactant, 0.5%~1.5% rust inhibitor, and base oil as the balance; Wherein, the low temperature refrigeration agent is C 10 ~C 25 The surfactant is an alkyl sulfonate and the surfactant is a gemini quaternary ammonium salt surfactant.

2. The rapid quenching oil according to claim 1, characterized in that: The mass ratio of the low-temperature refrigeration agent to the gemini quaternary ammonium salt surfactant is 3-10:

1.

3. The rapid quenching oil according to claim 2, characterized in that: The gemini quaternary ammonium salt surfactant includes at least one of N,N'-bis(hexadecyldimethyl)-1,2-dibromide ethylenediammonium salt, N,N'-bis(octadecyldimethyl)-1,2-dibromide ethylenediammonium salt, N,N'-dimethyl-N,N'-bis(2-hydroxyethyl)octanamide gemini quaternary ammonium salt, and N,N'-ethylenebis(methylaminoformamide) gemini quaternary ammonium salt.

4. The rapid quenching oil according to claim 1, characterized in that: The high-temperature refrigeration agent includes at least one of ethylene-propylene copolymer, polypropylene, polybutene, polyisobutylene, polyisobutylene succinate, and polyisobutylene succinimide.

5. The rapid quenching oil according to claim 1, characterized in that: The antioxidant includes at least one of a phenolic antioxidant and an amine antioxidant.

6. The rapid quenching oil according to claim 1, characterized in that: The dispersant includes at least one of sulfur-phosphorylated polyisobutylene polyoxyethylene ester, polyisobutylene succinate, dimethyl phosphate, calcium alkyl salicylate, and alkyl phenol salt.

7. The rapid quenching oil according to claim 1, characterized in that: The rust inhibitor includes at least one of calcium petroleum sulfonate, barium petroleum sulfonate, and barium dinonylnaphthalene sulfonate.

8. The rapid quenching oil according to any one of claims 1 to 7, characterized in that: The kinematic viscosity of the base oil at 40° C. is lower than 25 cSt.

9. A method for preparing a rapid quenching oil according to any one of claims 1 to 8, characterized in that: include, The base oil, antioxidant, dispersant and rust inhibitor are stirred and mixed at elevated temperature, and then a low-temperature quenching agent, a high-temperature quenching agent and a surfactant are added and continued to be stirred and mixed to obtain a rapid quenching oil.

10. The method for preparing rapid quenching oil according to claim 9, characterized in that: The temperature is increased to 60-100° C. at a rate of 0.2-0.5° C. / s.

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