Drawing oil applied to drawing of aluminum-based fine wire and preparation method of drawing oil

Abstract

The invention discloses drawing oil applied to aluminum-based fine wire drawing and a preparation method of the drawing oil, and belongs to the technical field of drawing oil processing, and the drawing oil specifically comprises a modifier, alcohol ammonia modified fluorine-containing polysiloxane, a thickener, an additive and base oil. The alcohol-ammonia-modified fluorine-containing polysiloxane and the thickening agent are used for enhancing and modifying the modified base oil, so that the extreme pressure resistance and the wear resistance of the drawing oil are effectively improved, the drawing breakage rate of 0.1 mm aluminum-based fine wires is reduced, and the production rate of the aluminum-based fine wires is increased.

Description

Technical Field

[0001] The invention relates to the technical field of wire drawing oil processing, and in particular to wire drawing oil used for aluminum-based fine wire drawing and a preparation method thereof. Background Art

[0002] The manufacturing process of enameled wire is composed of a series of different production processes, among which the wire drawing process is a very important process in the entire manufacturing process. Since the specifications of enameled wire are very diverse, the conductor material needs to be drawn into different sizes according to different requirements at any time during the manufacturing process. This drawing production process is the wire drawing production process. Wire drawing oil is the most important raw and auxiliary material in wire drawing production. It plays the role of lubrication, cleaning, cooling, and anti-oxidation during the drawing process, and provides quality assurance for the semi-finished products after drawing. Therefore, the quality of wire drawing oil directly affects the stability of the wire drawing manufacturing process and the quality of the semi-finished products after drawing.

[0003] The wire drawing process can be divided into large drawing, medium drawing, small drawing, micro drawing and other categories according to the type of wire drawing equipment and the size of the drawn aluminum wire. The aluminum-based wire drawing oil commonly used in the industry can be well applied to large drawing, medium drawing and small drawing. The micro-drawing size is mostly defined as aluminum wire below 0.18mm. The high-temperature stability of traditional wire drawing oil is insufficient. The wire drawing oil is easily oxidized and decomposed under the high temperature generated by high-speed wire drawing, resulting in oil film rupture, causing oxidation or local adhesive wear on the aluminum wire surface, and its extreme pressure-anti-wear performance is poor. Although sulfur / phosphorus additives can improve the extreme pressure properties, the aluminum sulfide film generated by the reaction of its active ingredients on the aluminum surface is highly brittle and easy to peel off after long-term use, which aggravates abrasive wear. In addition, it is difficult for lubricating wire drawing oil to form a continuous and uniform lubricating film in the submicron die gap, resulting in a high wire breakage rate of aluminum wire below 0.1mm, which seriously restricts the production rate and indirectly increases the manufacturing cost. Summary of the invention

[0004] The purpose of the present invention is to provide a wire drawing oil for use in aluminum-based fine wire drawing and a preparation method thereof, so as to solve the technical problems that the wire drawing oil for aluminum-based fine wire drawing in the prior art has poor extreme pressure resistance, wear resistance and surface lubrication performance, resulting in a high wire breakage rate during the drawing of aluminum-based fine wires, and the production rate needs to be further improved.

[0005] The object of the present invention can be achieved by the following technical scheme: a wire drawing oil used for aluminum-based fine wire drawing comprises the following components in parts by weight: 15-20 parts of a modifier, 10-13 parts of an alcohol-amine modified fluorinated polysiloxane, 5-7 parts of a thickener, 3-5 parts of an additive and 80-90 parts of a base oil;

[0006] The base oil is neopentyl polyol ester;

[0007] The modifier is composed of imidazole solution, triethanolamine borate and triethanolamine oleate soap in a weight ratio of 2:5:2, and the imidazole solution is composed of imidazolium ion salt and isopropanol in a weight ratio of 2g:3mL.

[0008] Further, the alcohol-ammonia modified fluorinated polysiloxane is processed by the following steps:

[0009] A1, stirring and mixing fluorinated polysiloxane, isopropanol and 1,2-epoxy-5-hexene, raising the temperature of the reaction system to 76-82° C., adding a platinum catalyst to the reaction system, keeping the temperature for 5-6 hours, and post-treating to obtain epoxidized fluorinated polysiloxane;

[0010] The synthetic reaction equation of epoxidized fluorinated polysiloxane is:

[0011]

[0012]

[0013] The synthetic reaction mechanism of epoxidized fluorinated polysiloxane is:

[0014] During the reaction, under the action of a catalyst, the olefin on the 1,2-epoxy-5-hexene molecule reacts with the silicon-hydrogen on the fluorinated polysiloxane molecule to modify the epoxy group on the fluorinated polysiloxane molecule to prepare an epoxidized fluorinated polysiloxane.

[0015] A2. The epoxidized fluorinated polysiloxane, isopropanol and N,N-bis(2-hydroxyethyl)ethylenediamine are stirred and mixed, the temperature of the reaction system is raised to 70-80° C., the reaction is kept warm for 4-5 hours, and post-treated to obtain alcohol-amine modified fluorinated polysiloxane.

[0016] The synthetic reaction equation of alcohol-ammonia modified fluorinated polysiloxane is:

[0017]

[0018] Where R 1 for:

[0019] The synthetic reaction mechanism of alcohol-ammonia modified fluorinated polysiloxane is:

[0020] During the reaction, the amino group on the N,N-bis(2-hydroxyethyl)ethylenediamine molecule is used as the active reaction site, and undergoes ring-opening condensation with the epoxy group on the epoxidized fluorinated polysiloxane molecule at high temperature to form a polyhydroxy modification, thereby preparing an alcohol-amine modified fluorinated polysiloxane.

[0021] Furthermore, in step A1, the amount ratio of the fluorinated polysiloxane, isopropanol, 1,2-epoxy-5-hexene and platinum catalyst is 5g:100mL:0.6g:0.02g, the platinum catalyst is chloroplatinic acid, and the post-treatment includes: after the reaction is completed, the temperature of the reaction system is kept at 76-82°C, and low-boiling substances are removed under reduced pressure to obtain epoxidized fluorinated polysiloxane; in step A2, the amount ratio of the epoxidized fluorinated polysiloxane, isopropanol and N,N-bis(2-hydroxyethyl)ethylenediamine is 5g:10mL:1g, and the post-treatment includes: after the reaction is completed, the reaction system is kept at 70-80°C, low-boiling substances are removed under reduced pressure, the temperature of the reaction system is lowered to room temperature, purified water is added to the reaction system, stirred and dispersed for 20-30min, allowed to stand for separation, the upper solution is washed 3 times with purified water, the upper solution is dried with anhydrous sodium sulfate for 4h, and filtered to obtain alcohol-ammonia-modified fluorinated polysiloxane.

[0022] Furthermore, the preparation method of fluorinated polysiloxane is as follows: D4, D3F, D4H and 1,1,3,3-tetramethyldisiloxane are stirred and mixed, a catalyst is added to the reaction system, the temperature of the reaction system is increased to 70-80°C, the reaction is kept warm for 6-8h, and post-processed to obtain fluorinated polysiloxane.

[0023] The synthetic reaction equation of fluorinated polysiloxane is:

[0024]

[0025] The synthetic reaction mechanism of fluorinated polysiloxane is:

[0026] During the reaction, under the action of the catalyst, the siloxane rings of D4, D3F and D4H are opened to form linear polysiloxane chains with randomly distributed fluorine / hydrogen side groups. Tetramethyldisiloxane is used as a capping agent to limit the chain length, thereby preparing fluorine- and silicon-hydrogen-modified fluorine-containing polysiloxane.

[0027] Furthermore, the weight ratio of D4, D3F, D4H, 1,1,3,3-tetramethyldisiloxane and acid catalyst is 6:4:3:1:0.3, the acid catalyst is 85-95wt% sulfuric acid, and the post-treatment includes: after the reaction is completed, the temperature of the reaction system is lowered to room temperature, 3wt% sodium carbonate aqueous solution is added to the reaction system, the pH of the system is adjusted to 6-7, the liquid is allowed to stand and separate, the upper solution is washed twice with saturated sodium carbonate and then washed three times with purified water, the upper solution is dried with anhydrous sodium sulfate for 4 hours, and filtered to obtain fluorine-containing polysiloxane.

[0028] Furthermore, the preparation method of the thickener is: under the protection of an inert atmosphere, 4,4'-diaminodiphenylmethane, blocked ammonia and tetrahydrofuran are stirred and mixed, the temperature of the reaction system is increased to 40-50°C, toluene diisocyanate is added to the reaction system, the reaction is kept warm for 60-80 minutes, and post-processed to obtain the thickener.

[0029] The synthetic reaction equation of thickener is:

[0030]

[0031] Where R 2 for: , , , , Any of .

[0032] The synthetic reaction mechanism of thickener is:

[0033] During the reaction, the amino group on the 4,4'-diaminodiphenylmethane molecule reacts with the isocyanate group on the toluene diisocyanate molecule to form a polyurethane molecule with a long chain end. The blocked ammonia acts as a chain terminator to limit chain growth, thereby preparing a thickener.

[0034] Furthermore, the dosage ratio of the 4,4'-diaminodiphenylmethane, the blocked ammonia and the toluene diisocyanate is 5mol:2mol:6mol, the dosage ratio of the 4,4'-diaminodiphenylmethane and tetrahydrofuran is 1g:5mL, the blocked ammonia is 6-aminohexanoic acid ethyl ester, and the post-treatment comprises: after the reaction is completed, the reaction system is kept at 40-50°C, and the tetrahydrofuran is removed under reduced pressure to obtain a thickener.

[0035] Furthermore, the preparation method of the imidazolium ion salt is as follows: 3,5-dihydroxybenzoic acid, sodium bicarbonate, and anhydrous ethanol are stirred and mixed until the system is dissolved, the temperature of the reaction system is increased to 40-50°C, 1-butyl-3-methylimidazole chloride solution is added dropwise to the reaction system, and after the addition is completed, the reaction is carried out at room temperature for 20-24 hours, and post-processed to obtain the imidazolium ion salt.

[0036] The synthetic reaction mechanism of imidazolium ion salt is:

[0037] During the reaction, the carboxyl protons of 3,5-dihydroxybenzoic acid are neutralized by sodium bicarbonate to form sodium carboxylate, which enhances the nucleophilicity of the carboxylate radical. The carboxylate radical oxygen attacks the C2 position of 1-butyl-3-methylimidazole chloride. - It is replaced as a leaving group to form an imidazolium ion salt and generate NaCl as a by-product.

[0038] Furthermore, the dosage ratio of the 3,5-dihydroxybenzoic acid, sodium bicarbonate and 1-butyl-3-methylimidazole chloride is 1 mol:1.2 mol:1 mol, the dosage ratio of the 3,5-dihydroxybenzoic acid and anhydrous ethanol is 1 g:5 mL, the 1-butyl-3-methylimidazole chloride solution is composed of 1-butyl-3-methylimidazole chloride and anhydrous ethanol at 1 g:2 mL, and the post-treatment comprises: after the reaction is completed, the temperature of the reaction system is reduced to 5-10°C, filtered, and the filtrate is transferred to a rotary evaporator with a water bath temperature of 50-60°C, and low boiling points are removed under reduced pressure to obtain an imidazolium ion salt.

[0039] The present invention also provides a method for preparing a wire drawing oil used for aluminum-based fine wire drawing, comprising the following steps:

[0040] S1, mixing the base oil and the modifier to obtain a modified base oil;

[0041] S2. Evenly mix the alcohol-ammonia modified fluorinated polysiloxane, thickener, additive and modified base oil to obtain wire drawing oil.

[0042] The present invention has the following beneficial effects:

[0043] 1. The aluminum-based fine wire drawing oil of the present invention uses neopentyl polyol ester as the base oil, which has a highly branched neopentyl structure. This structure gives it high thermal stability, low pour point and high viscosity index. Branching reduces the crystallization tendency of ester molecules and ensures low-temperature fluidity. At the same time, the viscosity decreases slowly at high temperatures to adapt to temperature fluctuations in the wire drawing process. The ester group forms a physical lubricating film on the aluminum surface through polar adsorption to reduce direct contact between metals. The imidazole cation in the modifier forms a dense organic film on the aluminum surface through electrostatic adsorption. The phenolic hydroxyl group of 3,5-dihydroxybenzoic acid is combined with the aluminum oxide layer through hydrogen bonds or chemical bonds to enhance the adsorption strength. The BO bond in triethanolamine borate is hydrolyzed under the action of friction heat to generate boric acid, which reacts with aluminum. The surface reaction forms aluminum borate or boron oxide compounds to reduce the friction coefficient. In addition, borate esters can also cooperate with imidazole salts to form a composite lubricating film such as BN coordination bonds to enhance the high temperature resistance of the film. The long-chain alkyl (C18) of oleic acid soap is arranged in a direction in the oil phase to form a micellar structure, which helps to disperse the imidazole salts and borates, prevent agglomeration, and assist in the uniform spreading of the lubricating film. The non-polar side chains of neopentyl polyol esters provide the main lubricating phase, while the polar components of the modifier are enriched on the metal surface to form a gradient lubricating layer to meet the lubrication needs of different pressure stages. After the weak adsorption film of the ester group is destroyed at high temperature, the imidazole salts and borates quickly fill the defects through chemical adsorption / reaction, thereby realizing the dynamic repair of the lubricating film and reducing the wear spot diameter and wire breakage rate.

[0044] 2. The wire drawing oil for aluminum-based fine wire drawing of the present invention comprises a thickener which is a polyurethane-type polymer generated by a condensation reaction of 4,4'-diaminodiphenylmethane, 6-aminoethyl caproate and toluene diisocyanate. The rigid aromatic ring structure in the molecular structure enhances the rigidity and thermal stability of the molecular chain. The ethyl caproate segment imparts flexibility and extensibility to form a "hard segment-soft segment" alternating block structure. The thickener molecules are bonded by hydrogen bonds to construct a three-dimensional physical cross-linked network. The rigid aromatic rings on the thickener molecular chains form a physical barrier under high pressure to hinder the direct contact of micro-convexities on the metal surface and delay the occurrence of bite. The flexible segments of the thickener are oriented in the sliding direction under the action of friction shear force to form a directional lubricating layer with a low friction coefficient. The thickener can form a composite extreme pressure film together with imidazole salts and borates in the modifier. The hydrogen bond cross-linked network of the thickener captures wear particles through hydrogen bonds to prevent secondary abrasive wear. Under the action of external force, the hydrogen bond network breaks preferentially and absorbs energy to reduce stress concentration and reduce the wire breakage rate.

[0045] 3. The aluminum-based fine wire drawing oil of the present invention comprises a fluorinated polysiloxane modified with alcohol ammonia, through a ring-opening reaction between N,N-bis(2-hydroxyethyl)ethylenediamine and a fluorinated polysiloxane modified with epoxy groups, to form a polar branched chain containing hydroxyl groups and amino groups on the long polysiloxane molecular chain. 3 The groups form a low surface energy lubrication layer on the aluminum surface to reduce the tendency of metal-to-metal adhesion. The flexibility of the Si-O-Si main chain absorbs impact energy through conformational changes and delays the rupture of the extreme pressure film. The hydroxyl / amino group enhances the adhesion of the boundary lubrication film through chemical adsorption. In addition, the amino group adsorbs aluminum chips through electrostatic action. It cooperates with the thickener and modified base oil to quickly clean the aluminum powder and aluminum mud produced by drawing from the surface of the wire and the drawing die during the wire drawing process to prevent their aggregation and wear, thereby greatly reducing the die breakage caused by the accumulation of residual aluminum mud, further enhancing the lubrication and drawing performance of the drawing oil on the aluminum wire, making it more suitable for the drawing and forming of aluminum-based fine wires. DETAILED DESCRIPTION

[0046] The technical scheme of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than 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.

[0047] In the present application, neopentyl polyol ester was selected from Jining Huipeng Chemical Co., Ltd., CAS No. 65461-8945-7, and hydroxyl value was 5 mgKOH / g;

[0048] In the present application, D4 is octamethylcyclotetrasiloxane, CAS number is 556-67-2;

[0049] In the present application, D3F is 1,3,5-trimethyl-1,3,5-tris(3,3,3-trifluoropropyl)cyclotrisiloxane, CAS number 2374-14-3;

[0050] In the present application, D4H is 1,3,5,7-tetramethylcyclotetrasiloxane, CAS number is 2370-88-9;

[0051] In this application, the sulfurized fatty acid ester is selected from Jinzhou Chenghua New Materials Co., Ltd., CAS No. 68390-93-2, model T1015;

[0052] In the present application, monoalkenyl succinimide is selected from Jinzhou Chenghua New Materials Co., Ltd., model T-151, kinematic viscosity (100°C) 178.5, total base number 48 mgKOH / g;

[0053] In this application, the CAS number of dodecanedioic acid is 693-23-2;

[0054] In this application, the CAS number of triethanolamine borate is 206-003-5;

[0055] In the present application, the CAS number of triethanolamine oleate soap is 10277-04-0.

[0056] Example 1

[0057] This embodiment provides a method for preparing a fluorinated polysiloxane modified with alcohol and ammonia for wire drawing oil used in aluminum-based fine wire drawing, comprising the following steps:

[0058] A1. Preparation of fluorinated polysiloxane

[0059] Weigh: 60g of D4, 40g of D3F, 30g of D4H and 10g of 1,1,3,3-tetramethyldisiloxane, add to a reaction flask and stir for 10min, add 3g of 85wt% sulfuric acid to the reaction flask, raise the temperature of the reaction flask to 70°C, keep warm for 6h, lower the temperature of the reaction flask to room temperature, add 3wt% sodium carbonate aqueous solution to the reaction flask, adjust the pH of the system to 6, let stand and separate, wash the upper solution with saturated sodium carbonate twice and then with purified water three times, dry the upper solution with anhydrous sodium sulfate for 4h, filter, and obtain fluorinated polysiloxane.

[0060] A2. Preparation of Epoxidized Fluorinated Polysiloxane

[0061] Weigh: 100 g of fluorinated polysiloxane, 2000 mL of isopropanol and 12 g of 1,2-epoxy-5-hexene, add into a reaction flask and stir, raise the temperature of the reaction flask to 76°C, add 0.4 g of chloroplatinic acid into the reaction flask, keep the temperature for 5 hours, keep the temperature of the reaction flask at 76°C, remove low-boiling substances under reduced pressure, and obtain epoxidized fluorinated polysiloxane.

[0062] A3. Preparation of alcohol-ammonia modified fluorinated polysiloxane

[0063] Weigh: 100 g of epoxidized fluorinated polysiloxane, 200 mL of isopropanol and 20 g of N,N-bis(2-hydroxyethyl)ethylenediamine, add to a reaction flask and stir, raise the temperature of the reaction flask to 70°C, keep warm for 4 hours, keep the reaction flask at 70°C, remove low boiling points under reduced pressure, lower the temperature of the reaction flask to room temperature, add 300 mL of purified water to the reaction flask, stir and disperse for 20 minutes, let stand to separate, wash the upper solution with purified water 3 times, dry the upper solution with anhydrous sodium sulfate for 4 hours, filter, and obtain alcohol-amine modified fluorinated polysiloxane.

[0064] Example 2

[0065] This embodiment provides a method for preparing a fluorinated polysiloxane modified with alcohol and ammonia for wire drawing oil used in aluminum-based fine wire drawing, comprising the following steps:

[0066] A1. Preparation of fluorinated polysiloxane

[0067] Weigh: 60g of D4, 40g of D3F, 30g of D4H and 10g of 1,1,3,3-tetramethyldisiloxane, add to a reaction flask and stir for 13min, add 3g of 90wt% sulfuric acid to the reaction flask, raise the temperature of the reaction flask to 75°C, keep warm for 7h, lower the temperature of the reaction flask to room temperature, add 3wt% aqueous sodium carbonate solution to the reaction flask, adjust the pH of the system to 6.5, let stand and separate, wash the upper solution with saturated sodium carbonate twice and then with purified water three times, dry the upper solution with anhydrous sodium sulfate for 4h, filter, and obtain fluorinated polysiloxane.

[0068] A2. Preparation of Epoxidized Fluorinated Polysiloxane

[0069] Weigh: 100 g of fluorinated polysiloxane, 2000 mL of isopropanol and 12 g of 1,2-epoxy-5-hexene, add into a reaction flask and stir, raise the temperature of the reaction flask to 79°C, add 0.4 g of chloroplatinic acid into the reaction flask, keep the temperature for 5.5 h, keep the temperature of the reaction flask at 79°C, remove low-boiling substances under reduced pressure, and obtain epoxidized fluorinated polysiloxane.

[0070] A3. Preparation of alcohol-ammonia modified fluorinated polysiloxane

[0071] Weigh: 100 g of epoxidized fluorinated polysiloxane, 200 mL of isopropanol and 20 g of N,N-bis(2-hydroxyethyl)ethylenediamine, add to a reaction flask and stir, raise the temperature of the reaction flask to 75°C, keep the reaction warm for 4.5 hours, keep the reaction flask warm at 75°C, remove low boiling points under reduced pressure, lower the temperature of the reaction flask to room temperature, add 300 mL of purified water to the reaction flask, stir and disperse for 25 minutes, stand and separate, wash the upper solution with purified water 3 times, dry the upper solution with anhydrous sodium sulfate for 4 hours, filter, and obtain alcohol-amine modified fluorinated polysiloxane.

[0072] Example 3

[0073] This embodiment provides a method for preparing a fluorinated polysiloxane modified with alcohol and ammonia for wire drawing oil used in aluminum-based fine wire drawing, comprising the following steps:

[0074] A1. Preparation of fluorinated polysiloxane

[0075] Weigh: 60g of D4, 40g of D3F, 30g of D4H and 10g of 1,1,3,3-tetramethyldisiloxane, add to a reaction flask and stir for 15min, add 3g of 95wt% sulfuric acid to the reaction flask, raise the temperature of the reaction flask to 80°C, keep warm for 8h, lower the temperature of the reaction flask to room temperature, add 3wt% aqueous sodium carbonate solution to the reaction flask, adjust the pH of the system to 7, let stand and separate, wash the upper solution with saturated sodium carbonate twice and then with purified water three times, dry the upper solution with anhydrous sodium sulfate for 4h, filter, and obtain fluorinated polysiloxane.

[0076] A2. Preparation of Epoxidized Fluorinated Polysiloxane

[0077] Weigh: 100 g of fluorinated polysiloxane, 2000 mL of isopropanol and 12 g of 1,2-epoxy-5-hexene, add into a reaction flask and stir, raise the temperature of the reaction flask to 82°C, add 0.4 g of chloroplatinic acid into the reaction flask, keep the temperature for 6 hours, keep the temperature of the reaction flask at 82°C, remove low-boiling substances under reduced pressure, and obtain epoxidized fluorinated polysiloxane.

[0078] A3. Preparation of alcohol-ammonia modified fluorinated polysiloxane

[0079] Weigh: 100 g of epoxidized fluorinated polysiloxane, 200 mL of isopropanol and 20 g of N,N-bis(2-hydroxyethyl)ethylenediamine, add to a reaction flask and stir, raise the temperature of the reaction flask to 80°C, keep the reaction warm for 5 hours, keep the reaction flask warm at 80°C, remove low boiling points under reduced pressure, lower the temperature of the reaction flask to room temperature, add 300 mL of purified water to the reaction flask, stir and disperse for 30 minutes, let stand to separate, wash the upper solution with purified water 3 times, dry the upper solution with anhydrous sodium sulfate for 4 hours, filter, and obtain alcohol-amine modified fluorinated polysiloxane.

[0080] Example 4

[0081] This embodiment provides a method for preparing a wire drawing oil used for aluminum-based fine wire drawing, comprising the following steps:

[0082] S1. Preparation of modifier

[0083] Weigh: 17.5 g of 1-butyl-3-methylimidazole chloride and 35 mL of anhydrous ethanol, mix well to obtain a 1-butyl-3-methylimidazole chloride solution for later use;

[0084] Weigh: 15.4 g of 3,5-dihydroxybenzoic acid, 10.1 g of sodium bicarbonate, and 77 mL of anhydrous ethanol, add them to a reaction flask and stir until the system is dissolved. The temperature of the reaction flask is raised to 40°C, and 1-butyl-3-methylimidazole chloride solution is added dropwise to the reaction system. After the addition is complete, react at room temperature for 20 h. The temperature of the reaction flask is lowered to 5°C, and the filtrate is filtered. The filtrate is transferred to a rotary evaporator at a water bath temperature of 50°C, and low-boiling substances are evaporated under reduced pressure to obtain imidazolium ion salt;

[0085] Add imidazolium ion salt and isopropanol in a ratio of 2 g:3 mL into a reaction bottle and stir until the system is dissolved to obtain an imidazole solution;

[0086] The imidazole solution, triethanolamine borate and triethanolamine oleate soap were uniformly mixed in a weight ratio of 2:5:2 to obtain a modifier.

[0087] S2. Preparation of thickener

[0088] Weigh: 99.2 g of 4,4'-diaminodiphenylmethane, 31.8 g of ethyl 6-aminohexanoate and 496 mL of tetrahydrofuran, add into a reaction bottle protected by argon and stir, raise the temperature of the reaction bottle to 40°C, add 104.5 g of toluene diisocyanate into the reaction bottle, keep warm and react for 60 minutes, keep the reaction bottle at 40°C, remove tetrahydrofuran under reduced pressure, and obtain a thickener.

[0089] S3. Preparation of modified base oil

[0090] Weigh out by weight: 80 parts of neopentyl polyol ester and 15 parts of the modifier in step S1 and mix them evenly to obtain a modified base oil.

[0091] S4. Prepare wire drawing oil.

[0092] Dibutyl hydroxytoluene, sulfide fatty acid ester, monoolefin succinimide and dodecanedioic acid are uniformly mixed in a weight ratio of 3:2:1:2 to obtain an additive auxiliary agent for standby use;

[0093] Weigh by weight: 10 parts of the alcohol-amine modified fluorinated polysiloxane prepared in Example 1, 5 parts of a thickener, 3 parts of an additive and 95 parts of a modified base oil, and mix them evenly to obtain a wire drawing oil.

[0094] Example 5

[0095] This embodiment provides a method for preparing a wire drawing oil used for aluminum-based fine wire drawing, comprising the following steps:

[0096] S1. Preparation of modifier

[0097] Weigh: 17.5 g of 1-butyl-3-methylimidazole chloride and 35 mL of anhydrous ethanol, mix well to obtain a 1-butyl-3-methylimidazole chloride solution for later use;

[0098] Weigh: 15.4 g of 3,5-dihydroxybenzoic acid, 10.1 g of sodium bicarbonate, and 77 mL of anhydrous ethanol, add them to a reaction flask and stir until the system is dissolved. The temperature of the reaction flask is raised to 45°C, and 1-butyl-3-methylimidazole chloride solution is added dropwise to the reaction system. After the addition is complete, react at room temperature for 22 hours. The temperature of the reaction flask is lowered to 7°C, and the filtrate is filtered. The filtrate is transferred to a rotary evaporator with a water bath temperature of 55°C, and low-boiling substances are evaporated under reduced pressure to obtain imidazolium ion salt;

[0099] Add imidazolium ion salt and isopropanol in a ratio of 2 g:3 mL into a reaction bottle and stir until the system is dissolved to obtain an imidazole solution;

[0100] The imidazole solution, triethanolamine borate and triethanolamine oleate soap were uniformly mixed in a weight ratio of 2:5:2 to obtain a modifier.

[0101] S2. Preparation of thickener

[0102] Weigh: 99.2 g of 4,4'-diaminodiphenylmethane, 31.8 g of ethyl 6-aminohexanoate and 496 mL of tetrahydrofuran, add into a reaction bottle protected by argon and stir, raise the temperature of the reaction bottle to 45°C, add 104.5 g of toluene diisocyanate into the reaction bottle, keep warm and react for 70 minutes, keep the reaction bottle at 45°C, remove tetrahydrofuran under reduced pressure, and obtain a thickener.

[0103] S3. Preparation of modified base oil

[0104] Weigh out by weight: 85 parts of neopentyl polyol ester and 17 parts of the modifier in step S1 and mix them evenly to obtain a modified base oil.

[0105] S4. Preparation of wire drawing oil

[0106] Dibutyl hydroxytoluene, sulfide fatty acid ester, monoolefin succinimide and dodecanedioic acid are uniformly mixed in a weight ratio of 3:2:1:2 to obtain an additive auxiliary agent for standby use;

[0107] Weigh by weight: 12 parts of the alcohol-amine modified fluorinated polysiloxane prepared in Example 2, 6 parts of a thickener, 4 parts of an additive and 102 parts of a modified base oil, mix well to obtain a wire drawing oil.

[0108] Example 6

[0109] This embodiment provides a method for preparing a wire drawing oil used for aluminum-based fine wire drawing, comprising the following steps:

[0110] S1. Preparation of modifier

[0111] Weigh: 17.5 g of 1-butyl-3-methylimidazole chloride and 35 mL of anhydrous ethanol, mix well to obtain a 1-butyl-3-methylimidazole chloride solution for later use;

[0112] Weigh: 15.4 g of 3,5-dihydroxybenzoic acid, 10.1 g of sodium bicarbonate, and 77 mL of anhydrous ethanol, add them to a reaction flask and stir until the system is dissolved. The temperature of the reaction flask is raised to 50°C, and 1-butyl-3-methylimidazole chloride solution is added dropwise to the reaction system. After the addition is complete, react at room temperature for 24 hours. The temperature of the reaction flask is lowered to 10°C, and the filtrate is filtered. The filtrate is transferred to a rotary evaporator with a water bath temperature of 60°C, and low-boiling substances are evaporated under reduced pressure to obtain imidazolium ion salt;

[0113] Add imidazolium ion salt and isopropanol in a ratio of 2 g:3 mL into a reaction bottle and stir until the system is dissolved to obtain an imidazole solution;

[0114] The imidazole solution, triethanolamine borate and triethanolamine oleate soap were uniformly mixed in a weight ratio of 2:5:2 to obtain a modifier.

[0115] S2. Preparation of thickener

[0116] Weigh: 99.2 g of 4,4'-diaminodiphenylmethane, 31.8 g of ethyl 6-aminohexanoate and 496 mL of tetrahydrofuran, add into a reaction bottle protected by argon and stir, raise the temperature of the reaction bottle to 50°C, add 104.5 g of toluene diisocyanate into the reaction bottle, keep warm and react for 80 minutes, keep the reaction bottle at 50°C, remove tetrahydrofuran under reduced pressure, and obtain a thickener.

[0117] S3. Preparation of modified base oil

[0118] Weigh by weight: 90 parts of neopentyl polyol ester and 20 parts of the modifier in step S1 are mixed evenly to obtain a modified base oil.

[0119] S4. Preparation of wire drawing oil

[0120] Dibutyl hydroxytoluene, sulfide fatty acid ester, monoolefin succinimide and dodecanedioic acid are uniformly mixed in a weight ratio of 3:2:1:2 to obtain an additive auxiliary agent for standby use;

[0121] Weigh by weight: 13 parts of the alcohol-amine modified fluorinated polysiloxane prepared in Example 3, 7 parts of a thickener, 5 parts of an additive and 110 parts of a modified base oil, mix well to obtain a wire drawing oil.

[0122] Comparative Example 1

[0123] The difference between this comparative example and Example 6 is that when preparing the alcoholamine modified fluorinated polysiloxane, steps A2-A3 are omitted, and the alcoholamine modified fluorinated polysiloxane is replaced by the fluorinated polysiloxane prepared in step A1.

[0124] Comparative Example 2

[0125] The difference between this comparative example and Example 6 is that no imidazole solution is added to the modifier in step S1.

[0126] Comparative Example 3

[0127] The difference between this comparative example and Example 6 is that the 6-aminocaproic acid ethyl ester in step S2 is replaced by n-propylamine in an equimolar amount.

[0128] Comparative Example 4

[0129] The difference between this comparative example and Example 6 is that neopentyl polyol ester is used as the wire drawing oil.

[0130] Performance Testing:

[0131] The maximum no-seizure load and wear spot diameter of the wire drawing oil samples prepared in Examples 4-6 and Comparative Examples 1-4 were measured with reference to the standard GB / T 3142-2019 "Determination of the load-bearing capacity of lubricants by four-ball method";

[0132] The wire drawing oils prepared in Examples 4-6 and Comparative Examples 1-4 were used on a Changzhou Dingtian DG150-24 dual frequency conversion tension-free rod fine drawing machine to draw 0.1 mm aluminum wires. The wire drawing speed and the wire breakage rate per 100 tons of the wire drawing operation were statistically analyzed. The specific test results are shown in Table 1 below:

[0133] Table 1-Performance test data of the sample

[0134]

[0135] Data Analysis:

[0136] A comparative analysis of the data in Table 1 above shows that the wire drawing oil prepared by the present invention has a maximum no-seizure load of 768.6 N, a wear spot diameter reduced to 0.307 mm, a wire drawing speed of 2000 m / min, and a 100-ton wire breakage rate reduced to 1.0%. All performance test data are better than those of the control example, that is, the present invention modifies the base oil with a modifier containing an imidazolium ion salt, and then enhances and modifies it with an alcohol-ammonia-modified fluorinated polysiloxane and a thickener, which not only effectively increases the extreme pressure resistance and wear resistance of the wire drawing oil, but also reduces the wire breakage rate of 0.1 mm aluminum-based fine wires, thereby increasing the production rate of aluminum-based fine wires.

[0137] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. Wire drawing oil used for aluminum-based fine wire drawing, characterized in that: The invention comprises the following components in parts by weight: 15-20 parts of a modifier, 10-13 parts of an alcohol-amine modified fluorinated polysiloxane, 5-7 parts of a thickener, 3-5 parts of an additive and 80-90 parts of a base oil; The base oil is neopentyl polyol ester; The modifier is composed of imidazole solution, triethanolamine borate and triethanolamine oleate soap in a weight ratio of 2:5:2, and the imidazole solution is composed of imidazolium ion salt and isopropanol in a weight ratio of 2g:3mL.

2. The wire drawing oil used for aluminum-based fine wire drawing according to claim 1, characterized in that: The alcohol-amine modified fluorinated polysiloxane is processed by the following steps: A1, stirring and mixing fluorinated polysiloxane, isopropanol and 1,2-epoxy-5-hexene, raising the temperature of the reaction system to 76-82° C., adding a platinum catalyst to the reaction system, keeping the temperature for 5-6 hours, and post-treating to obtain epoxidized fluorinated polysiloxane; A2. The epoxidized fluorinated polysiloxane, isopropanol and N,N-bis(2-hydroxyethyl)ethylenediamine are stirred and mixed, the temperature of the reaction system is raised to 70-80° C., the reaction is kept warm for 4-5 hours, and post-treated to obtain alcohol-amine modified fluorinated polysiloxane.

3. The wire drawing oil for aluminum-based fine wire drawing according to claim 2, characterized in that: In step A1, the amount ratio of the fluorinated polysiloxane, isopropanol, 1,2-epoxy-5-hexene and platinum catalyst is 5g:100mL:0.6g:0.02g, and the platinum catalyst is chloroplatinic acid; in step A2, the amount ratio of the epoxidized fluorinated polysiloxane, isopropanol and N,N-bis(2-hydroxyethyl)ethylenediamine is 5g:10mL:1g.

4. The wire drawing oil for aluminum-based fine wire drawing according to claim 2, characterized in that: The preparation method of fluorinated polysiloxane is as follows: D4, D3F, D4H and 1,1,3,3-tetramethyldisiloxane are stirred and mixed, a catalyst is added to the reaction system, the temperature of the reaction system is increased to 70-80°C, the reaction is kept warm for 6-8h, and post-processed to obtain fluorinated polysiloxane.

5. The wire drawing oil for aluminum-based fine wire drawing according to claim 4, characterized in that: The weight ratio of D4, D3F, D4H, 1,1,3,3-tetramethyldisiloxane and the acid catalyst is 6:4:3:1:0.3, and the acid catalyst is 85-95wt% sulfuric acid.

6. The wire drawing oil for aluminum-based fine wire drawing according to claim 1, characterized in that: The preparation method of the thickener is as follows: under the protection of an inert atmosphere, 4,4'-diaminodiphenylmethane, blocked ammonia and tetrahydrofuran are stirred and mixed, the temperature of the reaction system is increased to 40-50°C, toluene diisocyanate is added to the reaction system, the reaction is kept warm for 60-80 minutes, and post-processed to obtain the thickener.

7. The wire drawing oil for aluminum-based fine wire drawing according to claim 6, characterized in that: The usage ratio of the 4,4'-diaminodiphenylmethane, blocked ammonia and toluene diisocyanate is 5 mol:2 mol:6 mol, the usage ratio of the 4,4'-diaminodiphenylmethane and tetrahydrofuran is 1 g:5 mL, and the blocked ammonia is 6-aminohexanoic acid ethyl ester.

8. The wire drawing oil for aluminum-based fine wire drawing according to claim 1, characterized in that: The preparation method of the imidazolium ion salt is as follows: 3,5-dihydroxybenzoic acid, sodium bicarbonate and anhydrous ethanol are stirred and mixed until the system is dissolved, the temperature of the reaction system is increased to 40-50° C., 1-butyl-3-methylimidazole chloride solution is added dropwise to the reaction system, and after the addition is completed, the reaction is carried out at room temperature for 20-24 hours, and post-processing is performed to obtain the imidazolium ion salt.

9. The wire drawing oil for aluminum-based fine wire drawing according to claim 8, characterized in that: The dosage ratio of the 3,5-dihydroxybenzoic acid, sodium bicarbonate and 1-butyl-3-methylimidazole chloride is 1 mol:1.2 mol:1 mol, the dosage ratio of the 3,5-dihydroxybenzoic acid and anhydrous ethanol is 1 g:5 mL, and the 1-butyl-3-methylimidazole chloride solution is composed of 1-butyl-3-methylimidazole chloride and anhydrous ethanol at 1 g:2 mL.

10. A method for preparing a wire drawing oil for aluminum-based fine wire drawing according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1, mixing the base oil and the modifier to obtain a modified base oil; S2. Evenly mix the alcohol-ammonia modified fluorinated polysiloxane, thickener, additive and modified base oil to obtain wire drawing oil.

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