A method for preparing a neutralization-free modified amine ethoxy compound lubricant

Abstract

This invention relates to the field of lubricant preparation technology and provides a method for preparing a neutralization-free modified amine ethoxylated compound lubricant. The method includes the preparation of oligomeric amides and alkoxylated adducts. An oligomer is formed by condensing a dimer acid with diethylenetriamine to form an amide. Subsequently, the oligomer is modified with ethylene oxide and propylene oxide, alkoxylating the secondary amino groups in the diethylenetriamine. The alkoxylated secondary amino groups act as an alkaline neutralizer, while the dimer acid replaces the fatty acid as a lubricant. By adjusting the ethylene oxide-propylene oxide ratio and polymerization structure, products with emulsifying functions for semi-synthetic cutting fluids and low-foaming products for fully synthetic cutting fluids can be synthesized. This reduces preparation costs and environmental pollution, and allows for the preparation of high-performance adducts suitable for different application areas. It also improves product quality and stability, resulting in a promising market.

Description

Technical Field

[0001] This invention belongs to the field of lubricant preparation technology, and particularly relates to a method for preparing a neutralization-free modified amine ethoxy compound lubricant. Background Technology

[0002] Metalworking cutting fluids offer stable and outstanding performance, suitable for various cutting and grinding operations on a wide range of materials. Their excellent chemical and mechanical lubrication properties meet the most demanding cutting and grinding requirements. There are many types of metalworking fluids; broadly speaking, they can be categorized into four types based on composition: pure oil, soluble oil, chemical fluids (fully synthetic fluids), and semi-chemical fluids (semi-synthetic fluids). Currently, fully synthetic and semi-synthetic cutting fluids are the most commonly used on the market. Their main components are alkanolamines as neutralizing agents and macromolecular polyethers and fatty acids as lubricants.

[0003] Given the demands of green chemistry and energy conservation, and considering the odor of small-molecule fatty acids and alcohol amines, especially the harm to human health caused by the widespread use of inexpensive diethanolamine, some alternatives have been introduced to the market, such as diisopropanolamine and diethylene glycolamine. These alternatives have certain lubricating properties, but their lubrication and antioxidant properties are generally poor, making it difficult to meet the lubrication requirements of various mechanical equipment under extreme conditions such as high temperature and high load. Furthermore, in order to achieve better lubrication, the dosage ratio will be increased, which will increase the cost of use and the possibility of pollution. They have significant limitations and shortcomings in large-scale production and practical application, making it difficult to promote and apply them widely. Summary of the Invention

[0004] This invention provides a method for preparing a neutralization-free modified amine ethoxy compound lubricant, aiming to address the problems of existing neutralizing agents that use large quantities of inexpensive alternatives such as diethanolamine, which poses health risks. Furthermore, while diethanolamine does possess some lubricating properties, its lubrication and antioxidant effects are generally limited, making it difficult to meet the lubrication requirements of various mechanical equipment under extreme conditions such as high temperature and high load. Additionally, achieving better lubrication results requires increasing the dosage, which increases usage costs and the potential for pollution. These limitations hinder its widespread application and large-scale production.

[0005] This invention is achieved through a method for preparing a neutralization-free modified amine ethoxylated compound lubricant, comprising: preparing an oligomeric amide;

[0006] (1) Raw material preparation: Weigh dimer acid and diethylenetriamine according to a molar ratio of 1:1.1-1:1.5;

[0007] (2) Mixing process: The weighed dimer acid and diethylenetriamine are mixed to obtain a mixture of dimer acid and diethylenetriamine;

[0008] ① You can use a balance or electronic scale to weigh the dimer acid and diethylenetriamine accurately, and then mix them thoroughly with a mixer or stirrer to obtain a homogeneous mixture;

[0009] (3) Heating process: The mixture of dimer acid and diethylenetriamine is placed in the reactor and heated to a reaction temperature of 160°C at a uniform rate within 4 hours under the protection of nitrogen.

[0010] (4) Heat preservation process: After the reaction temperature reaches the specified value, keep it at the temperature for 3 hours to allow the reaction to proceed fully;

[0011] ① The reaction can be judged to be complete by monitoring changes in the physical properties of the reaction mixture, such as viscosity and color.

[0012] (5) Cooling process: Allow the reaction mixture to cool naturally to room temperature;

[0013] (6) Separation process: Separate the mixture after reaction to obtain oligomeric amides;

[0014] ① Extraction: Taking advantage of the fact that oligomeric amides have high solubility in a certain solvent and low solubility in other substances, oligomeric amides are separated from the reaction mixture. Commonly used solvents include acetone and ethanol.

[0015] Preferably, a method for preparing a neutralization-free modified amine ethoxylate lubricant includes: oligomeric amide processing:

[0016] (1) Washing process: Wash the oligomer amide with an appropriate amount of solvent to remove other impurities;

[0017] ① Washing solvent: Choose a solvent that is insoluble or has very low solubility in oligomeric amides, such as ethanol or acetone;

[0018] ② Washing concentration: Determined based on the nature and content of the impurities. If the impurity content is high, a higher concentration of washing solution may be required.

[0019] ③ Washing temperature: It usually needs to be higher than the boiling point of the solvent so that the solvent can fully dissolve and diffuse the impurities; the temperature should not be too high to avoid thermal decomposition or melting of the oligomeric amide;

[0020] ④ Washing time: long enough for impurities to fully dissolve and diffuse into the solvent.

[0021] (2) Drying process: The washed oligomer amide is dried to remove moisture and other volatile substances.

[0022] ① The drying of oligomeric amides should be carried out in a sealed container to avoid oxidation and contamination;

[0023] ② Drying temperature: below the melting point of the oligomeric amide to avoid melting and crystallization;

[0024] ③ Drying humidity: The drying humidity should be controlled within an appropriate range; if the humidity is too high, the oligomer amide may absorb moisture and affect the drying effect; if the humidity is too low, the oligomer amide may be over-dried and damaged.

[0025] ④ Drying time: Determined based on the thickness of the oligomeric amide, moisture content, and drying conditions to avoid over-drying and damage.

[0026] Preferably, a method for preparing a neutralization-free modified amine ethoxylated compound lubricant includes: preparing an alkoxylated adduct:

[0027] (1) Material transfer: The oligomeric amide is transferred to the polymerization reactor, which is a large pressure vessel to control the reaction temperature as needed;

[0028] (2) Vacuum removal of small molecule compounds: Create a vacuum environment to remove any small molecule substances that may be present; to promote the polymerization reaction and ensure the purity and quality of the final product;

[0029] (3) Heat to the reaction temperature: Raise the temperature inside the polymerization reactor to 140°C;

[0030] (4) Chemical reaction: After reaching the set temperature, ethylene oxide and propylene oxide are introduced into the polymerization reactor to react with the oligomer amide; the oligomer amide combines with ethylene oxide and propylene oxide to obtain alkoxylated adducts.

[0031] Preferably, a method for preparing a neutralization-free modified amine ethoxylated compound lubricant, wherein the alkoxylated adduct can modify the hydrophilicity and hydrophobicity of the cutting fluid by adjusting the HLB value of the additive, thereby optimizing its performance.

[0032] Preferably, in a method for preparing a neutralization-free modified amine ethoxy compound lubricant, the molar ratio of ethylene oxide to dimer acid is 1:3-1:16; and the molar ratio of propylene oxide to oligomer is 1:2-1:8.

[0033] Preferably, a method for preparing a neutralization-free modified amine ethoxylated compound lubricant, wherein the method for introducing ethylene oxide and propylene oxide is a block polyether method, the block polyether method comprising:

[0034] (1)EP: First ethylene oxide, then propylene oxide:

[0035] ① Ethylene oxide is introduced into the polymerization reactor to react with oligomeric amides to form block polyethers. Then, propylene oxide is introduced into the reactor to react with the remaining oligomeric amides to form the final adduct.

[0036] Preferably, a method for preparing a neutralization-free modified amine ethoxylate lubricant, wherein the block polyether method further includes:

[0037] (1) PE: First propylene oxide, then ethylene oxide;

[0038] ① Propylene oxide is introduced into the polymerization reactor to react with oligomeric amides to form block polyethers. Then, ethylene oxide is introduced into the reactor to react with the remaining oligomeric amides to form the final adduct.

[0039] Preferably, a method for preparing a neutralization-free modified amine ethoxylate lubricant, wherein the block polyether method further includes:

[0040] (1) Mix ethylene oxide and propylene oxide and carry out random copolymerization reaction;

[0041] ① Ethylene oxide and propylene oxide are introduced into the polymerization reactor simultaneously or sequentially to react with oligomeric amides to form the final adduct.

[0042] Compared with the prior art, the embodiments of this application have the following main advantages:

[0043] This method involves condensing a dimer acid with diethylenetriamine to form an amide, creating an oligomer. The oligomer is then modified with ethylene oxide and propylene oxide, alkoxylating the secondary amino groups in the diethylenetriamine. These alkoxylated secondary amino groups act as an alkaline neutralizer, while the dimer acid replaces the fatty acid as a lubricant. By adjusting the ethylene oxide-propylene oxide ratio and polymerization structure, products with emulsifying properties for semi-synthetic cutting fluids and low-foaming products for fully synthetic cutting fluids can be synthesized. This reduces preparation costs and environmental pollution, allowing for the production of high-performance adducts suitable for various applications. It also improves product quality and stability, resulting in a promising market. Attached Figure Description

[0044] Figure 1 This is a flowchart illustrating the present invention;

[0045] Figure 2 These are schematic diagrams illustrating specific embodiments and comparisons of the present invention; Detailed Implementation

[0046] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used herein in the specification of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having," and any variations thereof, in the specification, claims, and foregoing drawings of this application are intended to cover non-exclusive inclusion. The terms "first," "second," etc., in the specification, claims, or foregoing drawings of this application are used to distinguish different objects, not to describe a particular order.

[0047] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.

[0048] This invention provides a method for preparing a neutralization-free modified amine ethoxylated compound lubricant, such as... Figure 1-2 As shown, this includes: preparation of oligomeric amides:

[0049] (1) Raw material preparation: Weigh dimer acid and diethylenetriamine according to a molar ratio of 1:1.1-1:1.5;

[0050] (2) Mixing process: The weighed dimer acid and diethylenetriamine are mixed to obtain a mixture of dimer acid and diethylenetriamine;

[0051] ① You can use a balance or electronic scale to weigh the dimer acid and diethylenetriamine accurately, and then mix them thoroughly with a mixer or stirrer to obtain a homogeneous mixture;

[0052] (3) Heating process: The mixture of dimer acid and diethylenetriamine is placed in the reactor and heated to a reaction temperature of 160°C at a uniform rate within 4 hours under the protection of nitrogen.

[0053] (4) Heat preservation process: After the reaction temperature reaches the specified value, keep it at the temperature for 3 hours to allow the reaction to proceed fully;

[0054] ① The reaction can be judged to be complete by monitoring changes in the physical properties of the reaction mixture, such as viscosity and color.

[0055] (5) Cooling process: Allow the reaction mixture to cool naturally to room temperature;

[0056] (6) Separation process: Separate the mixture after reaction to obtain oligomeric amides;

[0057] ① Extraction: Taking advantage of the fact that oligomeric amides have high solubility in a certain solvent and low solubility in other substances, oligomeric amides are separated from the reaction mixture. Commonly used solvents include acetone and ethanol.

[0058] It should be noted that existing neutralizing agents, which largely use inexpensive alternatives like diethanolamine, pose health risks. While diethanolamine does possess some lubricating properties, its lubrication and antioxidant effects are generally poor, failing to meet the lubrication requirements of various mechanical equipment under extreme conditions such as high temperature and high load. Furthermore, achieving better lubrication requires increasing the dosage, which increases costs and the potential for pollution. These limitations hinder its widespread adoption in large-scale production and practical applications. This proposed solution addresses this issue by condensing dimer acid with diethylenetriamine to form an amide, creating an oligomer. This oligomer is then modified with ethylene oxide and propylene oxide, alkoxylating the secondary amino groups in diethylenetriamine. The alkoxylated secondary amino groups act as an alkaline neutralizer, while the dimer acid replaces fatty acids as a lubricant. By adjusting the ethylene oxide-propylene oxide ratio and polymerization structure, products with emulsifying functions for semi-synthetic cutting fluids and low-foaming products for fully synthetic cutting fluids can be synthesized. This reduces production costs and environmental pollution while improving product quality and stability.

[0059] Specifically, in this embodiment, a dimer acid and diethylenetriamine with a molar ratio of 1:1.5 are mixed and heated to 160°C at a uniform rate over 4 hours, during which nitrogen is blown in for dehydration. After reaching the temperature, the mixture is kept at that temperature for 3 hours to prepare an oligomeric amide of dimer acid and diethylenetriamine. The material is then transferred to a polymerization reactor without the addition of any catalyst. After removing small molecule compounds by vacuuming, the temperature is raised to 140°C. An addition reaction is first carried out by introducing dimer acid and propylene oxide in a molar ratio of 1:2. After the pressure remains constant, an addition reaction is carried out by introducing ethylene oxide in a molar ratio of 1:16 to obtain a water-soluble compound, which can be used for the fully synthetic cutting fluid high-foaming, high-cloud-point lubricant.

[0060] In a further preferred embodiment of the present invention, such as Figure 1-2 As shown, a dimer acid and diethylenetriamine were mixed in a molar ratio of 1:1.1 and heated to 160°C at a uniform rate over 4 hours, during which nitrogen was blown in for dehydration. After reaching the temperature, the mixture was held at that temperature for 3 hours to prepare an oligomeric amide of dimer acid and diethylenetriamine. The material was then transferred to a polymerization reactor without the addition of any catalyst. After removing small molecule compounds by vacuuming, the temperature was raised to 140°C to prepare a mixture of ethylene oxide and propylene oxide in a ratio of dimer acid:propylene oxide:ethylene oxide of 1:8:16. This yielded a water-soluble compound with low foaming properties. This compound is used as a low-foaming, low-cloud-point lubricant for fully synthetic cutting fluids.

[0061] In this embodiment, dimer acid and diethylenetriamine are mixed in a molar ratio of 1:1.3 and heated to 160°C at a constant rate over 4 hours, during which nitrogen is blown in for dehydration. After reaching the temperature, the mixture is kept at that temperature for 3 hours to prepare an oligomeric amide of dimer acid and diethylenetriamine. The material is then transferred to a polymerization reactor without the addition of any catalyst. After removing small molecule compounds by vacuuming, the temperature is raised to 140°C. An addition reaction is first carried out by introducing dimer acid and ethylene oxide in a molar ratio of 1:3. Once the pressure remains constant, an addition reaction is carried out by introducing propylene oxide in a molar ratio of 1:5 to obtain a stable emulsion that produces blue fluorescence when emulsified in water. This emulsion is used as a low-foaming, water-dispersible lubricant with a certain emulsifying power in semi-synthetic cutting fluids.

[0062] It should be noted that, for the sake of simplicity, the foregoing embodiments are all described as a series of actions. However, those skilled in the art should understand that the present invention is not limited to the described order of actions, as some steps may be performed in other orders or simultaneously according to the present invention. Furthermore, those skilled in the art should also understand that the embodiments described in the specification are preferred embodiments, and the actions and modules involved are not necessarily essential to the present invention.

[0063] It should be understood that the disclosed apparatus can be implemented in other ways, given the several embodiments provided in this application. For example, the apparatus embodiments described above are merely illustrative. For instance, the division of units described above may be implemented in other ways in practice. For example, multiple units or components may be combined or integrated into another system, or some features may be ignored or not executed. Furthermore, the coupling or communication connections shown or discussed may be through some interfaces; indirect coupling or communication connections between devices or units may be telecommunications or other forms.

[0064] The units described above as separate components may or may not be physically separate. The components shown as units may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the units can be selected to achieve the purpose of this embodiment according to actual needs.

[0065] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit the scope of protection of the invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on these embodiments, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can still combine, add, delete, or otherwise adjust the features of the various embodiments of the present invention according to the circumstances without conflict or creative effort, thereby obtaining different technical solutions that do not fundamentally depart from the concept of the present invention. These technical solutions also fall within the scope of protection of the present invention.

Claims

1. The application of a neutralization-free modified amine ethoxy compound as a lubricant in semi-synthetic or fully synthetic cutting fluids, characterized in that, The preparation method of the compound includes: preparation of oligomeric amides: (1) Raw material preparation: Weigh dimer acid and diethylenetriamine according to a molar ratio of 1:1.1-1:1.5; (2) Mixing process: The weighed dimer acid and diethylenetriamine are mixed to obtain a mixture of dimer acid and diethylenetriamine; ① Use a balance or electronic scale to weigh the dimer acid and diethylenetriamine accurately, and then mix them thoroughly together using a mixer to obtain a homogeneous mixture; (3) Heating process: The mixture of dimer acid and diethylenetriamine is placed in the reactor and heated to a reaction temperature of 160°C at a uniform rate within 4 hours under the protection of nitrogen. (4) Heat preservation process: After the reaction temperature reaches the specified value, keep it warm for 3 hours to allow the reaction to proceed fully; ① During the reaction process, the viscosity and color changes of the reaction mixture are monitored to determine whether the reaction is proceeding fully; (5) Cooling process: Allow the reaction mixture to cool naturally to room temperature; (6) Separation process: Separate the mixture after reaction to obtain oligomeric amides; ① Extraction: Taking advantage of the high solubility of oligomeric amides in solvents and the low solubility of other substances, the oligomeric amides are separated from the reaction mixture. The solvents are selected from acetone and ethanol. Oligomeric amide processing: (1) Washing process: Wash the oligomer amide with an appropriate amount of solvent to remove other impurities; (2) Drying process: The washed oligomer amide is dried to remove moisture and other volatile substances; Preparation of alkoxylated adducts: (1) Material transfer: The oligomeric amide is transferred to the polymerization reactor, which is a large pressure vessel to control the reaction temperature as needed; (2) Vacuum removal of small molecule compounds: Create a vacuum environment to remove any small molecule substances that may be present; to promote the polymerization reaction and ensure the purity and quality of the final product; (3) Heat to the reaction temperature: Raise the temperature inside the polymerization reactor to 140°C; (4) Chemical reaction: After reaching the set temperature, ethylene oxide and propylene oxide are introduced into the polymerization reactor to react with the oligomer amide; the oligomer amide combines with ethylene oxide and propylene oxide to obtain alkoxylated adducts.

2. The application of the neutralization-free modified amine ethoxy compound as described in claim 1 as a lubricant in semi-synthetic or fully synthetic cutting fluids, characterized in that, The molar ratio of ethylene oxide to dimer acid is 1:3-1:16; the molar ratio of propylene oxide to oligomer is 1:2-1:

8.

3. The application of the neutralization-free modified amine ethoxy compound as described in claim 2 as a lubricant in semi-synthetic or fully synthetic cutting fluids, characterized in that... The method for introducing ethylene oxide and propylene oxide includes: (1) Ethylene oxide first, then propylene oxide: ① Ethylene oxide is introduced into the polymerization reactor to react with oligomeric amides to form block polyethers. Then, propylene oxide is introduced into the reactor to react with the remaining oligomeric amides to form the final adduct.

4. The application of the neutralization-free modified amine ethoxy compound as described in claim 2 as a lubricant in semi-synthetic or fully synthetic cutting fluids, characterized in that... The method for introducing ethylene oxide and propylene oxide includes: (1) Propylene oxide first, then ethylene oxide; ① Propylene oxide is introduced into the polymerization reactor to react with oligomeric amides to form block polyethers. Then, ethylene oxide is introduced into the reactor to react with the remaining oligomeric amides to form the final adduct.

5. The application of the neutralization-free modified amine ethoxy compound as described in claim 2 as a lubricant in semi-synthetic or fully synthetic cutting fluids, characterized in that... The method for introducing ethylene oxide and propylene oxide includes: (1) Mix ethylene oxide and propylene oxide and carry out random copolymerization reaction; ① Ethylene oxide and propylene oxide are introduced into the polymerization reactor simultaneously or sequentially to react with oligomeric amides to form the final adduct.

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