Regulator for solid quenching oil as well as preparation method and application of regulator

Abstract

The invention discloses a regulator for solid quenching oil as well as a preparation method and application of the regulator. The regulator for the solid quenching oil comprises the following components in parts by weight: 70-95 parts of a cooling performance improver; 3 to 30 parts of an antioxidant; the low-temperature antioxidant is selected from at least one of T501, BHT (butylated hydroxytoluene), T511 and di-tert-butyl mixed phenol; the high-temperature antioxidant is selected from at least one of solid T531 and solid T534. Wherein the antioxidant comprises a high-temperature antioxidant and a low-temperature antioxidant. Compared with a liquid quenching oil regulator, the solid quenching oil regulator disclosed by the invention has the advantages of being easy to transport, weigh and add. When the solid quenching oil regulator disclosed by the invention is added into aged quenching oil, the use performance of the oil can be improved, and the cooling performance and the thermal oxidation stability of the aged quenching oil are improved.

Description

Technical Field

[0001] The invention relates to a solid quenching oil regulator and a preparation method and application thereof, belonging to the technical field of quenching reagents. Background Art

[0002] Quenching refers to a heat treatment process in which steel is heated to a temperature above the Ac3 or Ac1 point, maintained for a certain period of time, and then cooled at an appropriate rate to obtain a martensite and (or) bainite structure. It is an important part of mechanical manufacturing. The purpose of quenching is to improve the hardness, strength, and wear resistance to improve the performance of parts. In the quenching process, quenching oil plays an important role as a cooling medium. The Chinese invention patent application disclosure CN1078489A discloses an isothermal graded quenching oil composition, the main components of which include a mineral base oil, a cooling agent, a rust inhibitor, a brightener, and an antioxidant; Chinese patent application CN103710083A discloses an isothermal graded quenching oil composition, which further improves the cooling performance, thermal oxidation stability, and brightness of the isothermal graded quenching oil, and has a certain short-term rust resistance.

[0003] As the quenching oil is used for a long time, it will naturally age, including deterioration of cooling performance and thermal oxidation stability. These problems sometimes occur simultaneously, and sometimes occur separately, usually resulting in a decline in the quality of the quenched workpieces, or even unqualified workpieces. The solution to this problem is usually to replace part or all of the oil in use, but this will bring huge cost increases. Sometimes the change in the performance of the oil in use caused by the replacement of the quenching oil may cause changes in the working conditions, forcing heat treatment companies to spend time exploring and adjusting equipment parameters, increasing the investment of time and energy. Adjusting the oil in use can also be used to solve the problem of oil aging.

[0004] The Chinese invention patent application publication specification CN102978356A discloses a quenching oil regeneration method, comprising the following steps: a) settling or filtering the quenching oil to be treated; b) adding an acid value reducing agent to the quenching oil treated in step a), and fully contacting for 0.5 to 10 hours at 65 to 95° C.; wherein the acid value reducing agent is selected from at least one of an oxide, hydroxide or carbonate of an alkali metal or alkaline earth metal, and the amount added is 0.5 to 3.0% of the weight of the quenching oil to be treated; c) adding an adsorption aid to the quenching oil treated in step b), and contacting at 65 to 95° C. After full contact for 0.5 to 10 hours, the quenching oil is filtered; wherein the adsorption aid is selected from at least one of activated clay or diatomaceous earth, and the amount added is 5 to 15% of the weight of the quenching oil to be treated; d) the quenching oil treated in step c) is circulated and stirred at 80 to 100° C. for 0.5 to 10 hours to remove trace moisture in the quenching oil, and the moisture content is controlled to be no more than 0.03% by weight; e) a functional regulator is added to the quenching oil treated in step d), and the regenerated quenching oil is obtained after stirring evenly; wherein the amount of the functional regulator added is 0.5 to 15% of the weight of the quenching oil to be treated.

[0005] The existing method of adding quenching oil or quenching oil function regulator is mainly to add liquid substances, which are not convenient for transportation, weighing and addition compared with solid substances. The quenching oil regeneration method disclosed in the Chinese invention patent application publication specification CN102978356A mainly adds solid substances, but the process is cumbersome and the quenching oil needs to be filtered and recovered after treatment. The filtered treatment agent will become industrial waste, which requires increasing waste treatment costs. Therefore, it is of great practical and economic significance to develop a quenching oil function regulator composition that can adjust the aged quenching oil and does not need to be filtered and recovered. Summary of the invention

[0006] In view of the problem that the quenching oil in the prior art ages during use, resulting in performance degradation, and the prior art does not have a method for adjusting the quenching oil using a solid regulator that does not require filtration and recovery, the present invention provides a solid quenching oil regulator and a preparation method and application thereof. The solid quenching oil regulator of the present invention is added to the aged quenching oil to improve the performance of the used oil, and significantly improve the cooling performance and thermal oxidation stability of the aged quenching oil. In addition to adjusting the aged used oil, the quenching oil regulator of the present invention can also be used to adjust quenching oil products that do not match the working conditions.

[0007] The first aspect of the present invention provides a solid quenching oil regulator, which includes the following components in parts by weight: 70 to 95 parts of a cooling performance improver; 5 to 30 parts of an antioxidant; wherein the antioxidant includes a high-temperature antioxidant and a low-temperature antioxidant; the low-temperature antioxidant is selected from at least one of T501, BHT, T511, and di-tert-butyl mixed phenol; the high-temperature antioxidant is selected from at least one of solid T531 and solid T534.

[0008] According to some embodiments of the solid quenching oil conditioner of the present invention, preferably, the weight ratio of the high temperature antioxidant to the low temperature antioxidant is 1:0.1 to 10:1, preferably 1:0.15 to 5:1.

[0009] According to some embodiments of the solid quenching oil regulator of the present invention, preferably, the cooling performance improver is selected from at least one of white resin and solid petroleum resin (usually with a high degree of polymerization).

[0010] In the present invention, the cooling performance improver and antioxidant can be obtained commercially.

[0011] The second aspect of the present invention provides a method for preparing the above-mentioned solid quenching oil regulator, comprising: fully mixing and grinding a cooling performance improver and an antioxidant.

[0012] According to some embodiments of the preparation method of the present invention, preferably, the grinding particle size is 80-140 mesh.

[0013] According to some specific embodiments of the preparation method of the present invention, the preparation method of the solid quenching oil conditioning agent includes:

[0014] (1) Prepare raw materials according to the following components in parts by weight: 70 to 95 parts of cooling performance improver; 5 to 30 parts of antioxidant.

[0015] (2) adding the cooling performance improver and the antioxidant into a grinder and grinding them to 80-140 meshes to obtain better oil solubility;

[0016] (3) Take out the solid powder mixture that is fully ground and mixed, which is the solid quenching oil regulator.

[0017] The third aspect of the present invention provides the use of the above-mentioned solid quenching oil regulator or the above-mentioned preparation method in adjusting the performance of aged quenching oil.

[0018] The aging refers to the deterioration of the cooling performance and thermal oxidation stability of the quenching oil. These problems may occur simultaneously or individually. These problems usually cause the quality of the quenched workpiece to decline, or even produce unqualified workpieces.

[0019] A fourth aspect of the present invention provides a method for adjusting the performance of aged quenching oil, comprising: adding the above-mentioned solid quenching oil regulator to the aged quenching oil, preferably, the added amount is 2 mass % to 20 mass %.

[0020] Aged superspeed quenching oil usually refers to used superspeed quenching oil, and its maximum cooling rate (40℃) is generally lower than 90℃ / s.

[0021] In the aged quenching oil with degraded performance, adding solid quenching oil functional regulator at a ratio of 2wt% to 20wt% can significantly improve the various properties of the aged quenching oil. In terms of cooling performance, adding it to the aged ultra-speed quenching oil at a ratio of 5% by mass can increase the maximum cooling rate of the quenching oil from 80℃ / s to more than 95℃ / s, significantly improving the cooling performance of the ultra-speed quenching oil. In terms of thermal oxidation stability, adding it to the aged quenching oil at a ratio of 5% by mass can increase the 150℃ rotating oxygen bomb of the quenching oil from 50min to more than 105min, significantly improving the thermal oxidation stability of the quenching oil. After adding the solid quenching oil functional regulator, the cooling performance and thermal oxidation stability indicators of the quenching oil can be significantly improved, which is conducive to improving the oil in use at a lower cost.

[0022] Beneficial effects of the present invention:

[0023] (1) The solid quenching oil regulator of the present invention can significantly improve the cooling performance and thermal oxidation stability of the quenching oil, which is beneficial to improving the hardenability and hardenability of the workpiece during the quenching process and increasing the service life of the quenching oil.

[0024] (2) The solid-state regulator for quenching oil of the present invention can effectively improve the comprehensive performance of aged quenching oil. The solid-state regulator is easy to transport, weigh and add, and the addition amount is small. The addition method is simple, and there is no need to filter the quenching oil or recover the solid matter after adding. Compared with adjusting the used oil with new oil or liquid quenching oil regulator, or adjusting the quenching oil with a solid regulator that needs to be filtered and recovered, the present invention invests less time and cost, and no industrial waste is generated during the process. DETAILED DESCRIPTION

[0025] In order to make the present invention more easily understood, the present invention will be described in detail below in conjunction with embodiments. These embodiments are only for illustration and are not intended to limit the application scope of the present invention.

[0026] The above raw materials in the present invention can be prepared in-house or commercially available, and the present invention is not particularly limited thereto.

[0027] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention clearer, the present invention is further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain this patent in detail and do not limit the scope of protection of the present invention in any way. Unless otherwise defined, the technical terms used in the following embodiments have the same meanings as those generally understood by technicians in the field to which the present invention belongs. The reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the raw materials, instruments and equipment used in the following examples, etc., can all be purchased on the market or can be obtained by existing methods; the reagent dosage, unless otherwise specified, is the reagent dosage in conventional experimental operations; the experimental methods, unless otherwise specified, are all conventional methods.

[0028] Sources of raw materials in the embodiments of the present invention:

[0029] White resin, purchased from Qisheng Trading Company, brand 525;

[0030] Solid petroleum resin, purchased from Ruisheng Chemical Co., Ltd., brand C5;

[0031] T501, purchased from Lianlong New Materials Co., Ltd.;

[0032] BHT, purchased from Jiangsu Maida New Materials Co., Ltd.;

[0033] T511, purchased from Zhejiang Jinhai Chemical Co., Ltd.;

[0034] Di-tert-butyl mixed phenol, purchased from Beijing Chemical Plant No. 3;

[0035] Solid T531, purchased from Nanjing Chemical Plant;

[0036] Solid T534 was purchased from PetroChina Kunlun Additives.

[0037] Example 1

[0038] Solid quenching oil conditioning agent, composed of the following components:

[0039] Cooling performance improver: white resin, 40 parts; solid petroleum resin, 40 parts;

[0040] Antioxidant: T501, 10 parts; T531, 10 parts.

[0041] Preparation method of solid quenching oil regulator: prepare raw materials according to the weight proportions of the above components, add cooling performance improver and antioxidant into a grinder and grind to 80-140 mesh to obtain better oil solubility, take out the fully ground and mixed solid powder mixture, and obtain solid quenching oil regulator 1#.

[0042] Example 2

[0043] Solid quenching oil conditioning agent, composed of the following components:

[0044] Cooling performance improver: white resin, 20 parts; solid petroleum resin, 65 parts.

[0045] Antioxidant: BHT, 10 parts; solid T534, 5 parts.

[0046] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator 2# is obtained.

[0047] Example 3

[0048] Solid quenching oil conditioning agent, composed of the following components:

[0049] Cooling performance improver: white resin, 70 parts.

[0050] Antioxidant: di-tert-butyl mixed phenol, 20 parts; solid T534, 10 parts.

[0051] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator 3# is obtained.

[0052] Example 4

[0053] Solid quenching oil conditioning agent, composed of the following components:

[0054] Cooling performance improver: solid petroleum resin, 95 parts.

[0055] Antioxidant: di-tert-butyl mixed phenol, 3 parts; solid T531, 2 parts.

[0056] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator 4# is obtained.

[0057] Example 5

[0058] Solid quenching oil conditioning agent, composed of the following components:

[0059] Cooling performance improver: white resin, 50 parts; solid petroleum resin, 25 parts.

[0060] Antioxidant: BHT, 20 parts; solid T534, 5 parts.

[0061] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator 5# is obtained.

[0062] Example 6

[0063] Solid quenching oil conditioning agent, composed of the following components:

[0064] Cooling performance improver: white resin, 40 parts; solid petroleum resin, 40 parts.

[0065] Antioxidant: T501, 10 parts; T511, 5 parts; solid T531, 5 parts.

[0066] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator 6# is obtained.

[0067] Example 7

[0068] Solid quenching oil conditioning agent, composed of the following components:

[0069] Cooling performance improver: white resin, 30 parts; petroleum resin, 40 parts.

[0070] Antioxidant: BHT, 10 parts; solid T531, 10 parts; solid T534, 10 parts.

[0071] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator 7# is obtained.

[0072] Comparative Example 1

[0073] Solid quenching oil conditioning agent, composed of the following components:

[0074] Antioxidant: T501, 20 parts; T511, 20 parts; di-tert-butyl mixed phenol, 20 parts; solid T531, 20 parts, solid T534, 20 parts.

[0075] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator A is obtained.

[0076] Comparative Example 2

[0077] Solid quenching oil conditioning agent, composed of the following components:

[0078] Cooling performance improver: white resin, 50 parts; solid petroleum resin, 50 parts.

[0079] Preparation method of solid quenching oil regulator: According to the method of Example 1, a solid quenching oil regulator B is obtained.

[0080] Comparative Example 3

[0081] Solid quenching oil conditioning agent, composed of the following components:

[0082] Cooling performance improver: white resin, 40 parts; solid petroleum resin, 30 parts.

[0083] Antioxidant: T501, 10 parts; T511, 10 parts; di-tert-butyl mixed phenol, 10 parts.

[0084] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator C is obtained.

[0085] Comparative Example 4

[0086] Solid quenching oil conditioning agent, composed of the following components:

[0087] Cooling performance improver: white resin, 40 parts; solid petroleum resin, 30 parts;

[0088] Antioxidant: solid T531, 15 parts; solid T534, 15 parts.

[0089] Preparation method of solid quenching oil regulator: According to the method of Example 1, solid quenching oil regulator D is obtained.

[0090] Comparative Example 5

[0091] The quenching oil was prepared according to Example 1 of patent document CN103710083A to obtain a solid quenching oil conditioning agent E.

[0092] Test Case

[0093] The aged ultra-speed quenching oil used in this test refers to the used U8121 ultra-speed quenching oil, and its maximum cooling rate (40°C) is lower than 90°C / s.

[0094] The solid quenching oil regulators prepared in Examples 1-7 and Comparative Examples 1-5 were added to the aged super-speed quenching oil at a mass fraction of 5% to improve the use effect of the aged quenching oil. The results are shown in Table 1.

[0095] (1) The maximum cooling rate test method is based on ISO 9950.

[0096] (2) The test method of the rotating oxygen bomb is carried out in accordance with SH / T 0193.

[0097] Table 1

[0098]

[0099]

[0100] By comparing the maximum cooling rates (40°C) before and after adding the solid quenching oil functional regulator in Examples 1 to 7, it can be seen that adding the solid quenching oil functional regulator at a mass fraction of 5% can increase the maximum cooling rate of the aged quenching oil from 80°C / s to above 95°C / s, which significantly improves the cooling performance of the quenching oil and is beneficial to improving the hardenability and hardenability of the workpiece during the quenching process.

[0101] By comparing the rotating oxygen bomb (150°C) before and after adding the solid quenching oil function regulator in Examples 1 to 7, it can be seen that adding the solid quenching oil function regulator at a mass fraction of 5% can increase the rotating oxygen bomb of the aged quenching oil from 50 min to more than 105 min, which significantly improves the thermal oxidation stability of the quenching oil and is beneficial to increasing the service life of the quenching oil.

[0102] By comparing the maximum cooling rate (40°C) before and after adding the solid quenching oil functional regulator to Example 1, it can be seen that adding 5% by mass fraction of the comparative example cannot increase the maximum cooling rate (40°C) of the aged quenching oil, indicating that the improvement in the cooling performance of the quenching oil in Examples 1 to 7 is the effect brought about by the cooling performance improver in the solid quenching oil functional regulator.

[0103] By comparing the rotating oxygen bomb (150°C) before and after adding the solid quenching oil functional adjuster in Comparative Example 2, it can be seen that adding 5% by mass fraction of the comparative example cannot improve the rotating oxygen bomb value of the aged quenching oil, indicating that the improvement in the thermal oxidation stability of the quenching oil in Examples 1 to 7 is the effect brought about by the antioxidant in the solid quenching oil functional adjuster.

[0104] By comparing the rotating oxygen bomb (150°C) before and after adding the solid quenching oil functional regulator in Comparative Example 3, it can be seen that the addition of 5% by mass of the comparative example has limited effect on improving the rotating oxygen bomb value of the aged quenching oil, indicating that the improvement of the thermal oxidation stability of the quenching oil in Examples 1 to 7 is related to the high-temperature antioxidant in the solid quenching oil functional regulator.

[0105] By comparing the rotating oxygen bomb (150°C) before and after adding the solid quenching oil functional regulator in Comparative Example 4, it can be seen that the addition of 5% by mass of the comparative example has limited effect on improving the rotating oxygen bomb value of the aged quenching oil, indicating that the improvement of the thermal oxidation stability of the quenching oil in Examples 1 to 7 is related to the low-temperature antioxidant in the solid quenching oil functional regulator.

[0106] Compared with Comparative Examples 1-5, the solid quenching oil conditioner of the present invention has more excellent performance.

[0107] The above experimental results show that the use of solid quenching oil functional regulator can effectively improve the comprehensive performance of aged quenching oil and significantly improve the cooling performance and thermal oxidation stability of quenching oil.

[0108] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this field, under the technical enlightenment provided by the present invention, as common knowledge in the field, other equivalent variations and improvements can also be made, which should also be regarded as the protection scope of the present invention.

Claims

1. A solid quenching oil regulator, comprising components, by weight: 70 to 95 parts of a cooling performance improver and 5 to 30 parts of an antioxidant; the antioxidant comprises a high-temperature antioxidant and a low-temperature antioxidant; the low-temperature antioxidant is selected from at least one of T501, BHT, T511, and di-tert-butyl mixed phenol; the high-temperature antioxidant is selected from at least one of solid T531 and solid T534.

2. The solid quenching oil conditioning agent according to claim 1, characterized in that: The weight ratio of the high temperature antioxidant to the low temperature antioxidant is 1:0.1 to 10:

1.

3. The solid quenching oil conditioning agent according to claim 1, characterized in that: The weight ratio of the high temperature antioxidant to the low temperature antioxidant is 1:0.15 to 5:

1.

4. The solid quenching oil conditioning agent according to claim 1, characterized in that: The cooling performance improver is selected from at least one of white resin and solid petroleum resin.

5. The method for preparing the solid quenching oil conditioning agent according to any one of claims 1 to 4, comprising: The cooling performance improver and the antioxidant are mixed and then ground to obtain the solid quenching oil conditioner.

6. The method for preparing the solid quenching oil conditioning agent according to claim 5, characterized in that: The particle size after grinding is 80 to 140 meshes.

7. Use of the solid quenching oil regulator according to any one of claims 1 to 4 or the solid quenching oil regulator prepared by the preparation method according to claim 5 or 6 in adjusting the performance of aged quenching oil.

8. Methods for adjusting the properties of aged quenching oil, comprising: The solid quenching oil regulator according to any one of claims 1 to 4 or the solid quenching oil regulator prepared by the preparation method according to claim 5 or 6 is added to the aged quenching oil.

9. The method for adjusting the properties of aged quenching oil according to claim 8, characterized in that: The amount of the solid quenching oil regulator added is 2% to 20% of the mass of the aged quenching oil.

Images