WO2019006660A1 - 一种冷速稳定性能优异的超速淬火油组合物及其制备方法 - Google Patents

一种冷速稳定性能优异的超速淬火油组合物及其制备方法 Download PDF

Info

Publication number
WO2019006660A1
WO2019006660A1 PCT/CN2017/091673 CN2017091673W WO2019006660A1 WO 2019006660 A1 WO2019006660 A1 WO 2019006660A1 CN 2017091673 W CN2017091673 W CN 2017091673W WO 2019006660 A1 WO2019006660 A1 WO 2019006660A1
Authority
WO
WIPO (PCT)
Prior art keywords
stability
quenching
quenching oil
mineral oil
oil composition
Prior art date
Application number
PCT/CN2017/091673
Other languages
English (en)
French (fr)
Inventor
方建
Original Assignee
江苏鑫露新材料股份有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 江苏鑫露新材料股份有限公司 filed Critical 江苏鑫露新材料股份有限公司
Priority to PCT/CN2017/091673 priority Critical patent/WO2019006660A1/zh
Publication of WO2019006660A1 publication Critical patent/WO2019006660A1/zh

Links

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
    • C21D1/58—Oils
    • 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

Definitions

  • the invention relates to a quenching oil for metal heat treatment, in particular to an over-speed quenching oil composition excellent in cold-speed stability performance, which is suitable for quenching and strengthening requirements of various high-strength workpieces, and the invention relates to an over-speed quenching oil with excellent speed stability performance.
  • a method of preparing a composition is a method of preparing a composition.
  • the metallographic structure of the metal can be changed, so that the mechanical strength of the metal material can be improved by an order of magnitude; the excellent comprehensive performance of the hard surface and the toughness of the core can be obtained, and the mechanical component can be resisted. Impact performance, anti-adhesive wear and anti-fatigue wear are greatly improved; the service life of key mechanical components is increased by hundreds or even thousands of times.
  • One of the quenching media used in the quenching process is quenching oil.
  • the working principle of quenching oil is to remove heat from the surface of the red hot metal workpiece, so that the workpiece can be cooled rapidly and the corresponding metallographic structure can be obtained, thereby obtaining excellent comprehensive mechanical properties.
  • the cooling rate of the quenching oil is a key indicator of the good metal structure and mechanical properties of the quenched workpiece. For a workpiece of a specific material and size, there is a critical requirement for the cooling rate of the quenching oil. The cooling rate of the quenching oil is only higher than this critical value, and the quenched workpiece can obtain rational mechanical properties; otherwise, the mechanical properties of the quenched workpiece Will be unqualified, there will be defective products.
  • Overspeed quenching oil is the fastest quenching oil type in quenching oil. It is used for quenching requirements that require high surface hardness and good core toughness at the same time. It can be used for quenching of medium and low carbon alloy steels or relatively large-sized workpieces. It can be obtained (relative to the use of other types of quenching oil) for deeper hardening. Layer, higher surface hardness and finer metallographic structure. Compared with the quenching liquid, the quenching strength is more mild, and the quenched workpiece is not easily deformed and cracked. Therefore, it is widely used in the quenching process of high-strength parts. It is widely used in the quenching treatment of key components such as bridges, wind power, automobiles, engineering machinery and equipment, such as fasteners, gears, shafts, bearings, bushings, etc.
  • the red hot workpiece exposed to the quenching oil has a temperature of up to 850 °C, and its use environment is extremely harsh. Such a harsh use environment will cause changes in the structure of the oil material (cracking, sludge formation, carbon deposit), causing changes in cooling rate. Because of its ultra-fast cooling rate, ultra-speed oil is often used in applications with larger workpiece sizes, so it is more affected by thermal shock. The cooling rate of the quenching oil and the change of the cooling rate distribution will make the quenched workpiece unable to obtain the corresponding mechanical strength requirements, and may also cause deformation over tolerance. The cooling rate stability of the quenching oil is therefore extremely important. How to improve the cooling rate stability of quenching oil is the goal of the continuous efforts of quenching oil manufacturers.
  • the shortcomings of the existing over-speed quenching oil First, the cooling rate is falling fast. The performance is as follows: the maximum cooling rate decreases, the maximum cold temperature decreases, and the vapor film phase time is prolonged, which may cause poor metallographic structure of the workpiece, insufficient hardness, uneven hardness, and soft spots.
  • the existing ultra-speed oil cooling performance is unstable, and the rapid cooling rate is mainly due to the fact that the composition of the over-speed oil composition is susceptible to decay, cracking, etc. under the combined influence of the high temperature thermal shock of the workpiece and the catalytic action of the metal. The reason can be divided into three aspects: 1. The stability of the high temperature additive is insufficient, the cracking temperature is low, and the cracking decays rapidly during the quenching application; 2.
  • the problem of the composition compounding causes the cracking decay of the high temperature refrigerant; 3
  • the consumption of the selected self-consumed foaming type low-temperature refrigerant causes a decrease in the maximum cooling rate.
  • the selection of some raw materials for the over-speed quenching oil composition causes difficulty in separating the oil and water of the over-speed quenching oil, and it is difficult to recycle the used oil after the cleaning.
  • the present invention provides a cold in view of the current situation and the reasons for the insufficient cooling rate stability of the existing overspeed quenching oil.
  • the quenching oil composition is selected from the group consisting of high-stability additives; the temperature of the high-temperature refrigerant is rapidly reduced by the combination of the quenching oil composition, and the cracking decay of the high-temperature refrigerant is slowed down; the boiling of the composition is lowered by the selection of the special surface additive.
  • Additional pressure to promote gasification near boiling temperature use corresponding additives to passivate the catalytic aging effect of various metal materials in the quenching oil tank on quenching oil, decompose the peroxide generated by the decay of quenching oil, trap free radicals, cut off quenching
  • the oil aging reaction chain relieves and inhibits the aging process of quenching oil from the source and prolongs its service life.
  • the selected raw materials of the composition do not cause difficulty in separating the quenching oil and water.
  • An object of the present invention is to provide an over-speed quenching oil composition excellent in cold-speed stability performance in view of the deficiencies in the prior art, which has the characteristics of extremely fast cooling rate, and particularly excellent cooling rate stability.
  • an over-speed quenching oil composition excellent in cooling speed stability comprising the following components by weight:
  • Alkyl sulfonate metal salt 0.1 to 5%
  • the refined mineral oil is a mixture of refined paraffin-based mineral oil and refined intermediate-based mineral oil, wherein the paraffin-based mineral oil accounts for 90-10% of the total mass of the refined mineral oil, and the refined intermediate-based mineral oil accounts for refined minerals. 10 to 90% of the total mass of the oil.
  • the petroleum resin is a C 5 , C 9 or propane petroleum pitch resin.
  • the petroleum resin has a molecular weight of 1,000 to 15,000.
  • the shielding bisphenol is a sub-based hindered phenol.
  • the methyl amino thioformate is methyl dimethyl thioformate.
  • the metal alkylsulfonate is one or two of a metal salt of a octadecylsulfonate and a metal salt of a octadecylbenzenesulfonate;
  • the metal ion of the salt is potassium ion, sodium ion, or lithium ion.
  • octadecylsulfonic acid metal salt is a 2-mercapto-octadecylsulfonic acid metal salt.
  • the metal salt of octadecylbenzenesulfonic acid is a metal salt of 2-mercapto-octadecylbenzenesulfonate.
  • the invention also provides a preparation method of an over-speed quenching oil composition excellent in cold-speed stability performance, comprising the following steps:
  • the invention has the advantages that the quenching composition of the invention has the characteristics of extremely fast cooling speed, in particular, excellent cooling speed stability; after quenching with the quenching oil of the invention, the surface hardness of the workpiece is high and uniform, and the hardened layer is deep and deformed. The amount is small, the metallographic structure and mechanical properties are good, the workpiece performance is good, the defect rate is lowered, the quenching process is stable and easy to maintain; when the optimization, matching and quantity optimization of various raw material components of the quenching oil composition of the invention are sufficient
  • the oil-water separation property of the quenching oil is taken into consideration, and therefore, the quenching oil and water of the present invention is easy to separate, and the waste oil is recovered by post-cleaning for recycling and reuse.
  • An over-speed quenching oil composition excellent in cold-speed stability performance according to the present invention comprises the following components by weight:
  • 40 parts of mineral oil is refined into the first reactor, and the temperature is uniformly stirred to 80-100 ° C; 10 parts of a propane petroleum pitch resin having a molecular weight of 2000 is added, and 3 parts of the sub-based hindered phenol are stirred until uniformly dissolved; and the second reaction is filtered. 40 parts of refined mineral oil mixed with 90% paraffinic mineral oil and 10% refined intermediate mineral oil, and cooled to 60 ° C, 1 part of methyl dimethyl thioformate, alkyl thiodi 1 part of the azole and 5 parts of the octadecyl sulfonic acid metal salt were uniformly stirred.
  • 40 parts of mineral oil is refined into the first reactor, and the temperature is uniformly stirred to 80-100 ° C; 1 part of a propane petroleum pitch resin having a molecular weight of 8000, 5 parts of a sub-based hindered phenol, stirred until uniformly dissolved; and filtered to a second reaction 45 parts of refined mineral oil mixed with 50% paraffinic mineral oil and 50% refined intermediate mineral oil, and cooled to 60 ° C, 3 parts of methyl dimethyl thioformate, alkyl thiodi 1 part of the azole, 5 parts of the alkyl sulfonate was stirred evenly.
  • 40 parts of mineral oil is refined into the first reactor, and the temperature is uniformly stirred to 80-100 ° C; 2 parts of C5 petroleum resin having a molecular weight of 10,000, 0.1 part of sub-based hindered phenol, stirred until homogeneously dissolved; and filtered to the second reactor 50 parts of refined mineral oil mixed with 10% paraffinic mineral oil and 90% refined intermediate mineral oil, and cooled to 60 ° C, 0.01 parts of methyl monothiocarbamate, alkyl thiadiazole 5 parts, 1.5 parts of octadecylbenzenesulfonate and 1.5 parts of octadecylsulfonate were stirred uniformly.
  • 40 parts of mineral oil is refined into the first reactor, and the temperature is uniformly stirred to 80-100 ° C; 1 part of C9 petroleum resin having a molecular weight of 15000, 0.5 parts of sub-based hindered phenol, stirred until homogeneously dissolved; and filtered to the second reactor Adding 58 parts of refined mineral oil mixed with 50% paraffinic mineral oil and 50% refined intermediate mineral oil, and cooling to 60 ° C, adding 1 part of methyl monothiocarbamate, alkyl thiadiazole 0.001 parts, 0.1 parts of octadecylbenzenesulfonate was stirred well.
  • the maximum cooling rate is from 110 ° C / s to 78 ° C / s, the cooling rate is reduced by about 30%, the maximum cold temperature is from 620 ° C or more, down to 520 ° C, cooling rate
  • the distribution changed significantly; after 24 hours of water separation, 82.5% of the oil was still severe, difficult to separate, and the water was separated, 92.5% of the water and emulsified, and the waste oil recovered after washing was basically difficult to recycle. use.
  • the maximum cooling rate decreased from 110 ° C / s to 82 ° C / s, the cooling rate decreased by about 25%, the maximum cold temperature decreased from 620 ° C to 565 ° C, and the cooling rate distribution also changed significantly; In the 24h water separation process, 33% of the oil is still difficult to reuse directly, which contains 417,000ppm of water.
  • the above two sets of comparative examples the cooling performance changes greatly, the application of these two sets of comparative quenching oil, the probability of quenching workpiece defective products is high.
  • the overspeed quenching oil prepared by the embodiment of the invention has excellent cooling rate stability.
  • the maximum cooling rate is maintained above 110 ° C / s, and the maximum cooling rate is maintained above 620 ° C, and their surface is cooled and cooled.
  • the speed distribution is quite stable; the performance stability of the quenched product in the quenching application is improved, the fluctuation of the performance of the quenched workpiece is reduced, and the quenching pass rate is improved.
  • the oil-water separation performance of the embodiment of the invention is good, and the collected waste oil is cleaned afterwards, which is convenient for recycling.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

一种冷速稳定性能优异的超速淬火油组合物，包括以下重量百分比的组分：精制矿物油80～98％、石油树脂1～10％、屏蔽双酚0.1～5％、胺基硫代甲酸甲酯0.01～3％、烷基噻二唑0.001～5％、烷基磺酸盐0.1～5％。该淬火油组合物具有冷速极快的特点，特别是冷却性能及冷速分布特性稳定，采用该淬火油淬火后，工件表面硬度高且均匀，淬硬层深，变形量小，金相组织及机械性能好，淬火工件机械强度性能波动小，淬火工件合格率高，淬火工艺维护简单；该组合物油泥、积碳生成倾向小，使用寿命长，淬火后工件清洁光亮；该组合物油水分离性能好，后清洗回收废油便于回收再利用。

Description

一种冷速稳定性能优异的超速淬火油组合物及其制备方法 一种冷速稳定性能优异的超速淬火油组合物及其制备方法
技术领域
本发明涉及一种金属热处理用淬火油，具体涉及一种冷速稳定性能优异的超速淬火油组合物，适用于多种高强度工件淬火强化需求，本发明还涉及速稳定性能优异的超速淬火油组合物的制备方法。
背景技术
通过淬火及相应的热处理工艺，改变金属内部金相组织，可以使金属材质的机械强度性能一个数量级左右的提升；可以获得外表硬、而心部韧的优异综合性能，可以使机械零部件的抗冲击性能、抗黏着磨损及抗疲劳磨损获得极大的提升；使关键机械部件的使用寿命获得数百倍甚至数千倍的提高。淬火工艺所用到的淬火介质之一就是淬火油。
淬火油的工作原理，是从红热的金属工件表面移走热量，使工件迅速降温，获取相应金相组织，从而获得优异的综合机械性能。淬火油的冷却速度，是淬火工件获得良好金属组织和机械性能的一项关键指标。对于某一特定材质、尺寸的工件，对淬火油的冷却速度有一个临界要求，淬火油的冷却速度只有高于这一临界值，淬火工件才能获得理性的机械性能；否则，淬火工件的机械性能将不合格，出现次品。
超速淬火油是淬火油中冷速最快的淬火油类型。多用于需要同时获得高表面硬度和良好心部韧性的淬火要求，可用于中低碳合金钢、或者尺寸相对较大的工件的淬火，可以获得（相对于利用其他类型淬火油）更深的淬硬层、更高的表面硬度和更为细腻金相组织。与淬火液相比呢，其淬火强度又更为温和，淬火工件不易变形和开裂。因而在高强度零件淬火工艺中广泛应用。如在桥梁、风电、汽车、工程机械设备等领域的关键零部件（如紧固件、齿轮、轴、轴承、轴套等等）的淬火处理中起着重要的作用，而被广泛使用。
淬火油接触到的红热工件温度高达850℃左右，其使用环境异常的苛刻。这样苛刻的使用环境将会引起油品物质结构的变化（裂解、形成油泥、产生积碳），从而引起冷速的变化。超速油由于其冷速超快，多用于工件尺寸更大的应用环境，因而其受到的热冲击的影响更大。淬火油冷速的下滑，冷速分布的变化，将会使得淬火工件无法获得相应的机械强度要求，亦有可能引起变形超差。淬火油的冷速稳定性因而便显得异常重要。如何提高淬火油的冷速稳定性是淬火油制造商持续努力的目标。
现有超速淬火油的不足：一是冷速下滑快。多表现为，最大冷速下降，最大冷温降低，蒸气膜阶段时间延长，会引起工件金相组织不良，硬度不足，硬度不均匀，出现软点等问题。现有超速油冷却性能不稳定，冷速下降快的原因主要是：超速油组合物成分在工件高温热冲击作用以及金属的催化作用的共同影响下，易发生衰变、裂解等变化。其原因可分为三个方面进行说明：1、高温添加剂的稳定性不足，裂解温度低，在淬火应用过程中裂解衰退快；2、组合物配合的问题引起高温催冷剂的裂解衰退；3、所选用自消耗起泡型低温催冷剂的消耗引起最大冷速的衰退。二是一些超速淬火油组合物原料的选用问题，引起超速淬火油的油水分离困难，后清洗回收废油难以回收利用。
为了满足工件高淬火机械性能及高淬火机械稳定性对冷速稳定性能优异的超速淬火油应用的需求，针对现有超速淬火油冷速稳定性不足的现状及其原因，本发明提供一种冷速稳定性优异的超速淬火油组合物及其制备方法。该淬火油组合物选用：高稳定性的添加剂；通过淬火油组合物的配合迅速降低高温催冷剂的温度，减缓高温催冷剂的裂解衰退；通过特种表面添加剂的选用，降低组合物沸腾过热附加压力，促进临近沸腾温度时的气化；选用相应添加剂钝化淬火油槽中各种金属材质对淬火油的催化老化作用，分解淬火油的衰变产生的过氧化物，捕灭自由基，切断淬火油老化反应链，从源头上缓解与抑制淬火油的老化过程，延长其使用寿命。选用的组合物原料不会引起淬火油油水分离困难。
发明内容
本发明的目的在于针对现有技术中的不足，提供一种冷速稳定性能优异的超速淬火油组合物，具有冷速极快的特点，特别是冷速稳定性能优异。
为解决上述技术问题，本发明采用的技术方案为：一种冷速稳定性能优异的超速淬火油组合物，包括以下重量百分比的组分：
精制矿物油 80～98%
石油树脂 1～10%
屏蔽双酚 0.1～5%
胺基硫代甲酸甲酯 0.01～3%
烷基噻二唑 0.001～5%
烷基磺酸金属盐 0.1～5%
进一步的，所述精制矿物油由精制石蜡基矿物油和精制中间基矿物油混合而成，其中，石蜡基矿物油占精制矿物油总质量的90～10%，精制中间基矿物油占精制矿物油总质量的10～90%。
进一步的，所述的石油树脂为C5、C9或丙烷石油沥青树脂。
进一步的，所述的石油树脂的分子量为1000～15000。
进一步的，所述的屏蔽双酚为亚撑基受阻酚。
优选的，所述的胺基硫代甲酸甲酯为双胺基硫代甲酸甲酯。
进一步的，所述的烷基磺酸金属盐为二十八碳烷基磺酸金属盐和二十八碳烷基苯磺酸金属盐中的一种或两种；所述烷基磺酸金属盐的金属离子为钾离子、钠离子、或锂离子。
进一步的，所述二十八碳烷基磺酸金属盐为2-癸基-十八烷基磺酸金属盐。
进一步的，所述二十八碳烷基苯磺酸金属盐为2-癸基-十八烷基苯磺酸金属盐。
本发明还提供一种 冷速稳定性能优异的超速淬火油组合物的制备方法，包括以下步骤：
（1）将精制矿物油总质量的50%加入第一反应器中，搅拌升温至80～100℃；
（2）按比例向精制矿物油中加入石油树脂、屏蔽双酚，恒定在80～100℃，继续搅拌至均匀，过滤至第二反应器；
（3）向第二反应器中加入剩余精制矿物油，并降温至60℃，然后按比例加入胺基硫代甲酸甲酯、烷基噻二唑，烷基磺酸盐，循环搅拌均匀，得到所述高稳定性超速淬火油组合物。
本发明的有益效果：本发明的淬火组合物具有冷速极快的特点，特别是冷速稳定性能优异；采用本发明的淬火油淬火后，工件表面硬度高且均匀，淬硬层深，变形量小，金相组织及机械性能好，工件性能稳定性好，降低次品率，淬火工艺稳定易于维护；本发明淬火油组合物各种原料成分的优选、匹配及量的优化时，充分的兼顾到淬火油的油水分离性，因而，本发明淬火油油水易于分离，后清洗回收废油便于回收再利用。
具体实施方式
本发明的一种冷速稳定性能优异的超速淬火油组合物，包括以下重量百分比的组分：
精制矿物油 80～98%
石油树脂 1～10%
屏蔽双酚 0.1～5%
胺基硫代甲酸甲酯 0.01～3%
烷基噻二唑 0.001～5%
烷基磺酸盐 0.1～5%
下面结合具体实施例对本发明的技术方案作详细说明。
实施例1
向第一反应器精制矿物油40份，均匀搅拌升温至80-100℃；加入分子量为2000的丙烷石油沥青树脂10份，亚撑基受阻酚3份，搅拌至溶解均匀；过滤至第二反应器，加入由90%石蜡基矿物油和10%精制中间基矿物油混合而成的精制矿物油40份，并降温至60℃，加入双胺基硫代甲酸甲酯1份，烷基噻二唑1份，二十八碳烷基磺酸金属盐5份搅拌均匀。
实施例2
向第一反应器精制矿物油40份，均匀搅拌升温至80-100℃；加入分子量为8000的丙烷石油沥青树脂1份，亚撑基受阻酚5份，搅拌至溶解均匀；过滤至第二反应器，加入由50%石蜡基矿物油和50%精制中间基矿物油混合而成的精制矿物油45份，并降温至60℃，加入双胺基硫代甲酸甲酯3份，烷基噻二唑1份，烷基磺酸盐5份搅拌均匀。
实施例3
向第一反应器精制矿物油40份，均匀搅拌升温至80-100℃；加入分子量为10000的C5石油树脂2份，亚撑基受阻酚0.1份，搅拌至溶解均匀；过滤至第二反应器，加入由10%石蜡基矿物油和90%精制中间基矿物油混合而成的精制矿物油50份，并降温至60℃，加入单胺基硫代甲酸甲酯0.01份，烷基噻二唑5份，二十八碳烷基苯磺酸盐1.5份和二十八碳烷基磺酸盐1.5份搅拌均匀。
实施例4
向第一反应器精制矿物油40份，均匀搅拌升温至80-100℃；加入分子量为15000的C9石油树脂1份，亚撑基受阻酚0.5份，搅拌至溶解均匀；过滤至第二反应器，加入由50%石蜡基矿物油和50%精制中间基矿物油混合而成的精制矿物油58份，并降温至60℃，加入单胺基硫代甲酸甲酯1份，烷基噻二唑0.001份，二十八碳烷基苯磺酸盐0.1份搅拌均匀。
对比例1
市场上淬火油1
对比例2
市场上淬火油2
表一实施例1-4及对比例1和2的产品性能指标
项目 试验方法 实施例 1 实施例 2 实施例 3 实施例 4 对比例 1 对比例 2
最大冷速 ISO9950 ≥ 110 ℃ /s ≥ 110 ℃ /s ≥ 110 ℃ /s ≥ 110 ℃ /s ≥ 110 ℃ /s ≥ 110 ℃ /s
最大冷温 ISO9950 ≥ 620 ℃ ≥ 620 ℃ ≥ 620 ℃ ≥ 620 ℃ ≥ 620 ℃ ≥ 620 ℃
油水分离时间 ASTM D1401 24h 24h 24h 24h 24h 24h
油层 ASTM D1401 40ml 40ml 40ml 40ml 7ml 30ml
水层 ASTM D1401 40ml
清澈		 40ml
清澈		 40ml
清澈		 40ml
清澈		 3ml 33ml
乳化层 ASTM D1401 无 无 无 无 70ml
乳白色
33ml 油被乳化		 15ml
其中含有 10ml 油和 7ml 水
老化后最大冷速 ISO9950 ≥ 110 ≥ 110 ≥ 110 ≥ 110 78 82
老化后最大冷温 ISO9950 ≥ 620 ℃ ≥ 620 ℃ ≥ 620 ℃ ≥ 620 ℃ 520 ℃ 565 ℃
由上表可以看出，对比例1，最大冷速从110℃/s以上，降至78℃/s，冷速下降了30%左右，最大冷温从620℃以上，下降至520℃，冷速分布发生明显改变；经过24h的分水过程，仍有82.5%的油被严重，难以分离，分出来的水很少，92.5%的水和形成乳化状，其后清洗回收的废油基本难以回收利用。对比例2，最大冷速从110℃/s以上，降至82℃/s，冷速下降了25%左右，最大冷温从620℃以上，下降至565℃，冷速分布发生亦明显改变；经过24h的分水过程，仍有33%油难以直接回用，其中含有417000ppm的水。以上两组对比例，冷却性能变化大，应用这两组对比例淬火油，淬火工件次品几率高。本发明实施例制备的冷速稳定性优异的超速淬火油，老化之后，最大冷速皆维持在110℃/s之上，最大冷速亦皆维持在620℃以上，表面它们的冷速及冷速分布相当稳定；提高了淬火应用中，淬火产品的性能稳定性，减小淬火工件性能的波动，提高淬火合格率。而且本发明实施例油水分离性能良好，后清洗收集的废油，便于回收利用。
上述实施例仅用以说明本发明的技术方案，而非对本发明的构思和保护范围进行限定，本发明的普通技术人员对本发明的技术方案进行修改或者等同替换，而不脱离技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围中。

Claims (10)

  1. 一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述组合物包括以下重量百分比的组分：
    精制矿物油 80～98%
    石油树脂 1～10%
    屏蔽双酚 0.1～5%
    胺基硫代甲酸甲酯 0.01～3%
    烷基噻二唑 0.001～5%
    烷基磺酸金属盐 0.1～5%。
  2. 根据权利要求1所述的一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述精制矿物油由精制石蜡基矿物油和精制中间基矿物油混合而成，其中，石蜡基矿物油占精制矿物油总质量的90～10%，精制中间基矿物油占精制矿物油总质量的10～90%。
  3. 根据权利要求1所述的一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述的石油树脂为C5、C9或丙烷石油沥青树脂。
  4. 根据权利要求1或3所述的一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述的石油树脂的分子量为1000～15000。
  5. 根据权利要求1所述的一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述的屏蔽双酚为亚撑基受阻酚。
  6. 根据权利要求1所述的一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述的胺基硫代甲酸甲酯为双胺基硫代甲酸甲酯。
  7. 根据权利要求1所述的一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述的烷基磺酸金属盐为二十八碳烷基磺酸金属盐和二十八碳烷基苯磺酸金属盐中的一种或两种；所述烷基磺酸金属盐的金属离子为钾离子、钠离子、或锂离子。
  8. 根据权利要求6所述的一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述二十八碳烷基磺酸金属盐为2-癸基-十八烷基磺酸金属盐。
  9. 根据权利要求6所述的一种冷速稳定性能优异的超速淬火油组合物，其特征在于：所述二十八碳烷基苯磺酸金属盐为2-癸基-十八烷基苯磺酸金属盐。
  10. 一种冷速稳定性能优异的超速淬火油组合物的制备方法，其特征在于：所述方法包括以下步骤：
    （1）将精制矿物油总质量的50%加入第一反应器中，搅拌升温至80～100℃；
    （2）按比例向精制矿物油中加入石油树脂、屏蔽双酚，恒定在80～100℃，继续搅拌至均匀，过滤至第二反应器；
    （3）向第二反应器中加入剩余精制矿物油，并降温至60℃，然后按比例加入胺基硫代甲酸甲酯、烷基噻二唑，烷基磺酸盐，循环搅拌均匀，得到所述高稳定性超速淬火油组合物。
PCT/CN2017/091673 2017-07-04 2017-07-04 一种冷速稳定性能优异的超速淬火油组合物及其制备方法 WO2019006660A1 (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2017/091673 WO2019006660A1 (zh) 2017-07-04 2017-07-04 一种冷速稳定性能优异的超速淬火油组合物及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2017/091673 WO2019006660A1 (zh) 2017-07-04 2017-07-04 一种冷速稳定性能优异的超速淬火油组合物及其制备方法

Publications (1)

Publication Number Publication Date
WO2019006660A1 true WO2019006660A1 (zh) 2019-01-10

Family

ID=64949618

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2017/091673 WO2019006660A1 (zh) 2017-07-04 2017-07-04 一种冷速稳定性能优异的超速淬火油组合物及其制备方法

Country Status (1)

Country Link
WO (1) WO2019006660A1 (zh)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0305114A1 (en) * 1987-08-26 1989-03-01 Nippon Oil Co. Ltd. Heat treating oil
CN1078489A (zh) * 1992-05-15 1993-11-17 中国石油化工总公司大连石油化工公司 分级淬火油组合物
CN102212662A (zh) * 2011-06-09 2011-10-12 上海德润宝特种润滑剂有限公司 一种特快速淬火油及其制备方法
CN103981340A (zh) * 2014-05-26 2014-08-13 江苏鑫露新材料股份有限公司 一种便于回收利用的高速淬火油组合物及其制备方法
CN104017953A (zh) * 2014-05-26 2014-09-03 江苏鑫露新材料股份有限公司 一种冷速稳定性能优异的超速淬火油组合物及其制备方法
CN105821186A (zh) * 2016-04-28 2016-08-03 昌利锻造有限公司 一种换挡连杆用淬火油
CN106591547A (zh) * 2015-10-19 2017-04-26 中国石油化工股份有限公司 一种淬火油组合物及其制造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0305114A1 (en) * 1987-08-26 1989-03-01 Nippon Oil Co. Ltd. Heat treating oil
CN1078489A (zh) * 1992-05-15 1993-11-17 中国石油化工总公司大连石油化工公司 分级淬火油组合物
CN102212662A (zh) * 2011-06-09 2011-10-12 上海德润宝特种润滑剂有限公司 一种特快速淬火油及其制备方法
CN103981340A (zh) * 2014-05-26 2014-08-13 江苏鑫露新材料股份有限公司 一种便于回收利用的高速淬火油组合物及其制备方法
CN104017953A (zh) * 2014-05-26 2014-09-03 江苏鑫露新材料股份有限公司 一种冷速稳定性能优异的超速淬火油组合物及其制备方法
CN106591547A (zh) * 2015-10-19 2017-04-26 中国石油化工股份有限公司 一种淬火油组合物及其制造方法
CN105821186A (zh) * 2016-04-28 2016-08-03 昌利锻造有限公司 一种换挡连杆用淬火油

Similar Documents

Publication Publication Date Title
CA1139081A (fr) Fabrication de silicate de sodium
CN108165295B (zh) 一种用于炼油过程延迟焦化的液体增收剂
WO2021203542A1 (zh) 一种冷速稳定的超速光亮淬火油
CN109022713B (zh) 抗乳化型淬火油组合物及其用途
WO2019006660A1 (zh) 一种冷速稳定性能优异的超速淬火油组合物及其制备方法
CN109554563B (zh) 一种降低复杂多元黄铜合金杂质元素镍的方法
CN101260337B (zh) 一种金属表面改性材料及其制备方法
CN104893683A (zh) 一种抗结焦烷基苯合成导热油及其制备方法
CN103667628A (zh) 热处理方法
CN104017953A (zh) 一种冷速稳定性能优异的超速淬火油组合物及其制备方法
CN105018238A (zh) 蓝宝石衬底晶片清洗液
CN103667630A (zh) 热处理油组合物及其制备方法
CN102180655B (zh) 一种坩埚及其生产工艺
WO2017127988A1 (zh) 一种用于炼油工艺过程的阻垢剂及其制备方法
EP0908505B1 (en) Method for operating an ethylene production plant comprising the addition of an anti-aging additive composition to a quench oil.
CN112501398A (zh) 抗乳化型超速淬火油组合物、制备方法及其用途
CN104451057A (zh) 一种防腐蚀淬火油及其制备方法
CN112538559A (zh) 一种自紧垫片、自紧螺母的加工工艺
CN117265218A (zh) 一种精密齿轮专用淬火油、制备及使用方法
CN112522492B (zh) 一种自紧螺母及自紧垫片的热处理工艺
CN111410937B (zh) 一种基于改性石墨烯的导热油及其制备方法
KR890000447B1 (ko) 조경유 회수설비의 부식억제제
CN110315285A (zh) 一种汽车用高强耐磨紧固件的制备方法
CN115651742B (zh) 磷化反应型金刚线拉拔油及制备方法和应用
CN110295369B (zh) 一种缓蚀复合物、缓蚀剂、缓蚀阻焦剂及制备方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17916815

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 17916815

Country of ref document: EP

Kind code of ref document: A1