Ultrahigh-temperature-resistant room-temperature curing release agent for forging and forming titanium alloy and preparation method thereof

Abstract

The invention relates to the field of release agents, and provides an ultrahigh-temperature-resistant room-temperature curing release agent for titanium alloy forging and forming and a preparation method thereof.The release agent is prepared from, by weight, 70-90 parts of organic silicon resin, 5-15 parts of modified molybdenum disulfide, 2-6 parts of ultrahigh-temperature-resistant filler, 1-5 parts of surfactant and 2-6 parts of curing agent; 0.5-3 parts of a silver-based catalyst, and 100-200 parts of deionized water. The ultrahigh-temperature-resistant room-temperature curing release agent for forging and forming of the titanium alloy, provided by the invention, has the characteristics of good lubricity and ultrahigh temperature resistance, and has a relatively good commercial application value.

Description

Technical Field

[0001] The invention relates to the field of mold release agents, and in particular to an ultra-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing and a preparation method thereof. Background Art

[0002] A release agent is a functional substance between the mold and the finished product, which can make the surface of an object easy to release, smooth and clean. It is widely used in various molding operations such as metal die-casting, polyurethane foam and elastomers, and injection molding of thermoplastics. Among them, metal die-casting release agents are mainly used in various molding operations of metal materials such as aluminum alloys, magnesium alloys, zinc alloys, and titanium alloys, and metal die-casting release agents need to have greater tensile strength, good chemical resistance, high temperature resistance and other properties.

[0003] Silicone resin has good heat resistance and weather resistance, so it is widely used as a base material in the field of release agents. However, silicone rubber still has some unresolved defects. For example, if silicone resin is exposed to high temperature environment for a long time, it is prone to aging, which seriously limits the application of silicone resin in some ultra-high temperature environments; and the existing die-casting release agents generally have problems such as insufficient lubrication performance, poor stability at high temperature or poor dispersibility.

[0004] Patent CN 108907072A discloses a high-temperature resistant metal die-casting release agent and a preparation method thereof. The metal die-casting release agent prepared in the application includes ingredients such as oxidized polyethylene wax, organic modified silicone oil, xanthan gum and preservatives, and has the advantages of emulsion stability, excellent corrosion resistance and high temperature resistance. However, the application does not solve the problem that xanthan gum is easy to agglomerate and has poor dispersibility, which may lead to a decrease in the high temperature resistance of the release agent; Patent CN 117305008A discloses a water-based die-casting release agent and a preparation method thereof. The die-casting release agent includes ingredients such as petroleum solvent oil, lubricant, emulsifier, antioxidant and bactericide, wherein the lubricant is at least one of ozokerite, beeswax and oxidized polyethylene wax, but the high temperature resistance of the wax itself is not high enough and is easily oxidized, and cannot meet the use requirements in ultra-high temperature environments.

[0005] Therefore, there is an urgent need in the market for an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming with good lubricity and ultra-high temperature resistance. Summary of the invention

[0006] In view of the problems existing in the prior art, the present invention uses silicone resin as the base material of the release agent, adds modified molybdenum disulfide, ultra-high temperature resistant filler and surfactant, and synthesizes an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and pressing under the action of a curing agent and a silver-based catalyst. The release agent has good lubricity and ultra-high temperature resistance.

[0007] In order to achieve the above object, the technical solution adopted by the present invention is as follows:

[0008] On the one hand, the present invention provides an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and pressing. The release agent comprises the following raw materials in parts by weight: 70-90 parts of silicone resin, 5-15 parts of modified molybdenum disulfide, 2-6 parts of ultra-high temperature resistant filler, 1-5 parts of surfactant, 2-6 parts of curing agent, 0.5-3 parts of silver-based catalyst, and 100-200 parts of deionized water.

[0009] Wherein, the surfactant is Tween 20 or Tween 80.

[0010] In some embodiments of the present invention, the silicone resin is methyl silicone resin or methylphenyl silicone resin.

[0011] In some embodiments of the present invention, the method for preparing the modified molybdenum disulfide comprises the following steps:

[0012] (1) placing kaolin in a reaction container, adding a sodium hydroxide aqueous solution, stirring, centrifuging, washing, filtering, taking a precipitate, drying, and grinding to obtain modified kaolin for later use;

[0013] (2) taking the modified kaolin of step (1), adding deionized water, stirring, ultrasonicating, sequentially adding ammonium molybdate and thiourea, stirring, ultrasonicating, heating to 210-220° C., stirring, cooling to room temperature, filtering, taking solid, washing, drying, grinding, and obtaining a modified kaolin-molybdenum disulfide composite material for later use;

[0014] (3) 5-bromo-2-carboxythiophene, N-methylformamide and cuprous bromide are sequentially added to a methanol solution of sodium methoxide, refluxed under an inert atmosphere, extracted, and the organic phase is collected to obtain product 1 for later use;

[0015] (4) adding the product 1 of step (3), 3-bromo-1-propanol and sodium sulfite to toluene in sequence, heating to 90-110° C. under an inert atmosphere, washing, collecting the aqueous phase, and drying to obtain the product 2 for later use;

[0016] (5) adding the product 2 of step (4) to tetrahydrofuran, adding a trimethylamine aqueous solution, stirring, distilling, washing, and drying to obtain a product 3 for standby use;

[0017] (6) adding the product 3 of step (5) and ferric chloride to chloroform in sequence, stirring under an inert atmosphere, filtering, drying the solid, adding hydrazine hydrate, precipitating, and drying to obtain polythiophene for later use;

[0018] (7) The modified kaolin-molybdenum disulfide composite material of step (2) and the polythiophene of step (6) are sequentially added into deionized water, ultrasonicated, allowed to stand, centrifuged, and freeze-dried to obtain modified molybdenum disulfide.

[0019] Wherein, in the step (1), the concentration of the sodium hydroxide aqueous solution is 4-6 mol / L; the mass ratio of 5-bromo-2-carboxythiophene, 3-bromo-1-propanol and trimethylamine in the trimethylamine aqueous solution is 1:(1.2-1.5):(0.08-0.1).

[0020] Preferably, in step (1), the concentration of the sodium hydroxide aqueous solution is 5 mol / L; the mass ratio of 5-bromo-2-carboxythiophene, 3-bromo-1-propanol and trimethylamine in the trimethylamine aqueous solution is 1:1.38:0.09.

[0021] In some embodiments of the present invention, in step (2), the mass ratio of modified kaolin and ammonium molybdate is (0.06-0.1):1.

[0022] Preferably, in step (2), the mass ratio of modified kaolin to ammonium molybdate is 0.08:1.

[0023] In some embodiments of the present invention, in step (7), the mass ratio of the modified kaolin-molybdenum disulfide composite material to polythiophene is 1:(0.08-0.12).

[0024] Preferably, in step (7), the mass ratio of the modified kaolin-molybdenum disulfide composite material to polythiophene is 1:0.1.

[0025] Molybdenum disulfide is widely used in release agents due to its good lubricity, chemical stability, wear resistance and temperature stability. However, due to its high surface energy, molybdenum disulfide is prone to agglomeration and has poor dispersion in release agents, resulting in a decrease in its lubricating effect in release agents.

[0026] On the one hand, the applicant uses kaolin modified by alkaline solution to modify molybdenum disulfide to obtain a modified kaolin-molybdenum disulfide composite material. Kaolin is a natural aluminum silicate mineral material with low price, wide source, large specific surface area, safety and environmental protection. It is an ideal carrier material for molybdenum disulfide. The applicant uses an aqueous solution of sodium hydroxide with a suitable concentration to modify kaolin, so that the modified kaolin can expose more active sites and have higher reaction activity. Furthermore, the aqueous solution of sodium hydroxide will destroy the silicon-oxygen tetrahedral units on the outer surface of kaolin, causing a large number of defects on its outer surface, thereby making the defects on the outer surface and the Al-OH on the inner surface serve as nucleation sites for molybdenum disulfide, which can adsorb a large number of molybdate ions and then react with thiourea. The hydrogen sulfide gas produced by hydrolysis reacts to generate molybdenum disulfide, and the generated molybdenum disulfide is highly dispersed in the inner cavity and outer surface of kaolin, which greatly improves the dispersibility of molybdenum disulfide in the release agent; on the other hand, the applicant synthesized polythiophene using 5-bromo-2-carboxythiophene with a carboxyl group as a raw material, and through the control of reaction conditions and the selection of substances, the polythiophene contains a quaternary ammonium salt structure and has good antibacterial properties, and the polythiophene is combined with a modified kaolin-molybdenum disulfide composite material through electrostatic action to obtain modified molybdenum disulfide, so that the modified molybdenum disulfide has good lubricity and antibacterial effect; further, the carboxyl group in polythiophene and the hydroxyl group in kaolin may also produce a certain cross-linking effect, thereby improving the stability of the modified molybdenum disulfide.

[0027] In some embodiments of the present invention, the method for preparing the ultrahigh temperature resistant filler comprises the following steps:

[0028] 1) Sc 2 O 3 and ZrO 2 Mix, add deionized water, ball mill, add deionized water, ball mill, dry, sieve, sinter, and obtain a mixture for use;

[0029] 2) The mixture of step 1) and isopropyl tri(dioctyl pyrophosphate acyloxy) titanate are mixed, anhydrous ethanol is added, the mixture is heated to 70-80° C., stirred, washed, and dried to obtain an ultrahigh temperature resistant filler.

[0030] In some embodiments of the present invention, in step 1), ZrO 2 and Sc 2 O 3 The mass ratio is 1:(0.06-0.1).

[0031] Preferably, in step 1), ZrO 2 and Sc 2 O 3 The mass ratio is 1:0.081.

[0032] In some embodiments of the present invention, in step 2), the ratio of the mixture to isopropyl tri(dioctyl pyrophosphate) titanate is 1 g: (0.6-1) ml.

[0033] Preferably, in the step 2), the ratio of the mixture to isopropyl tri(dioctyl pyrophosphate) titanate is 1 g:0.8 ml.

[0034] Zirconia (ZrO 2 ), as a ceramic material, has outstanding properties such as high temperature resistance and high strength, and can meet the use requirements of release agents at ultra-high temperatures above 900°C. However, there are still some problems with the zirconia material itself. On the one hand, zirconia is relatively brittle, and the phase change problem of zirconia may cause the toughness of zirconia to decrease; on the other hand, zirconia powder is easy to agglomerate and thus affect the uniformity of the internal structure, ultimately making the filler uneven and reducing the impact strength. These problems will affect the high temperature resistance of zirconia.

[0035] On the one hand, the applicant adopts Sc 2 O 3 to ZrO 2 Doping, the Sc ion radius is similar to the Zr ion radius, which can form a denser ceramic structure, thereby effectively improving the ZrO 2 toughness and phase-stable structure in high temperature and corrosive environment; on the other hand, the applicant uses titanate coupling agent isopropyl tri (dioctyl pyrophosphate acyloxy) titanate to Sc 2 O 3 Doped ZrO 2 The (mixture) is surface modified to finally obtain an ultra-high temperature resistant filler. The addition of isopropyl tri(dioctyl pyrophosphate acyloxy) titanate improves the dispersibility of the ultra-high temperature resistant filler, and the pyrophosphate in isopropyl tri(dioctyl pyrophosphate acyloxy) titanate may also have a certain chelating effect with the curing agent triethanolamine, so that the ultra-high temperature resistant filler can be stably dispersed in the release agent, further improving the high temperature resistance of the release agent.

[0036] In some embodiments of the present invention, the curing agent is triethanolamine.

[0037] Another aspect of the present invention further provides a method for preparing the ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and pressing as described in the above technical solution, comprising the following steps:

[0038] S1. Add silicone resin, modified molybdenum disulfide, ultrahigh temperature resistant filler and surfactant into deionized water in sequence, stir for 25-35 minutes, and obtain a mixed solution for standby use;

[0039] S2. Add the curing agent and the silver-based catalyst to the mixed solution of step S1 in sequence, and stir for 15-25 minutes to obtain an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging.

[0040] Compared with the prior art, the present invention has the following beneficial effects:

[0041] (1) The present invention uses silicone resin as the base material of the release agent, adds modified molybdenum disulfide, ultrahigh temperature resistant filler and surfactant, and synthesizes an ultrahigh temperature resistant room temperature curing release agent for titanium alloy forging and pressing under the action of a curing agent and a silver-based catalyst. Through the synergistic effect of the various components, the release agent has the advantages of good lubricity and ultrahigh temperature resistance.

[0042] (2) The present invention uses molybdenum disulfide as the main component of the lubricant, uses alkaline solution modified kaolin as a carrier of molybdenum disulfide, and introduces polythiophene with a quaternary ammonium salt structure synthesized using 5-bromo-2-carboxythiophene as a raw material to synthesize modified molybdenum disulfide, so that the modified molybdenum disulfide has good antibacterial properties, stability and dispersibility.

[0043] (3) The present invention uses zirconium oxide, a ceramic material having ultrahigh temperature resistance, as a matrix and performs Sc 2 O 3 Doping and surface modification of isopropyl tri(dioctyl pyrophosphate) titanate solve the phase change problem and poor dispersion problem of zirconium oxide.

[0044] (4) The release agent prepared by the present invention has excellent lubricity and ultra-high temperature resistance, can be widely used in the field of titanium alloy forging and forming, and has good commercial application value. DETAILED DESCRIPTION

[0045] The present invention will be described below in conjunction with specific embodiments. It should be noted that the following embodiments are examples of the present invention and are only used to illustrate the present invention, but not to limit the present invention. Other combinations and various modifications within the concept of the present invention may be performed without departing from the spirit or scope of the present invention.

[0046] In the following embodiments and comparative examples, except for modified molybdenum disulfide and ultra-high temperature resistant fillers, the remaining compound monomers and related reagents used can be purchased from the market. Among them, the model of methyl silicone resin is IOTA 6070, purchased from Anhui IOTA Silicone Oil Co., Ltd.; the model of methyl phenyl silicone resin is IOTA 6156C, purchased from Anhui IOTA Silicone Oil Co., Ltd.; kaolin is purchased from Shijiazhuang Baijiang Mineral Products Co., Ltd.; the average particle size of zirconium oxide is 60nm, purchased from Beijing Dekedao Gold Technology Co., Ltd.; the silver-based catalyst is silver powder purchased from Shaanxi Kaida Chemical Co., Ltd.; the titanium alloy plate is purchased from Shenzhen Pacific Mold Steel Co., Ltd.

[0047] Preparation Example 1

[0048] The synthetic method of modified molybdenum disulfide A comprises the following steps:

[0049] (1) 2 g of kaolin was placed in a reaction container, 100 ml of 5 mol / L sodium hydroxide aqueous solution was added, the mixture was stirred for 24 h, centrifuged, washed until the pH of the supernatant was 7, filtered, the precipitate was taken, dried at 60° C. for 12 h, and ground to obtain modified kaolin for later use;

[0050] (2) Take 0.8 g of the modified kaolin of step (1), add 50 ml of deionized water, stir for 15 min, ultrasonicate, add 10 g of ammonium molybdate and 114 g of thiourea in sequence, stir for 30 min, ultrasonicate for 30 min, heat to 215 ° C, stir for 24 h, cool to room temperature, filter, take the solid, wash with deionized water 3 times, dry at 60 ° C for 12 h, grind, and obtain a modified kaolin-molybdenum disulfide composite material for use;

[0051] (3) 10 g of 5-bromo-2-carboxythiophene, 30 ml of N-methylformamide and 2 g of cuprous bromide were added to 20 ml of 28 wt% methanol solution of sodium methoxide in sequence. 2 Reflux for 72 h under atmosphere, extract with ether, collect the organic phase, and obtain product 1 for later use;

[0052] (4) The product 1 of step (3), 13.8 g of 3-bromo-1-propanol and 5 g of sodium sulfite were added to 50 ml of toluene in sequence and heated to 40 °C. 2 The mixture was heated to 100°C under an atmosphere, washed with deionized water three times, the aqueous phase was collected, and dried at 60°C for 12 h to obtain product 2 for later use;

[0053] (5) Add the product 2 of step (4) to 40 ml of tetrahydrofuran, add 30 ml of 30 wt% trimethylamine aqueous solution, stir for 24 h, distill, wash with deionized water 3 times, and dry at 60° C. for 12 h to obtain product 3 for use;

[0054] (6) The product 3 of step (5) and 16.2 g of ferric chloride were added to 50 ml of chloroform in sequence under N 2 Stir for 24 hours under atmosphere, filter, dry the solid at 60°C for 12 hours, add 3 g of hydrazine hydrate, add 30 ml of saturated tetrabutylammonium chloride acetone solution to precipitate, dry at 60°C for 12 hours to obtain polythiophene for use;

[0055] (7) 10 g of the modified kaolin-molybdenum disulfide composite material of step (2) and 1 g of the polythiophene of step (6) were added to 100 ml of deionized water, ultrasonicated for 6 h, allowed to stand for 2 h, centrifuged, and freeze-dried at -40 ° C for 12 h to obtain modified molybdenum disulfide A.

[0056] Preparation Example 2

[0057] The specific implementation method of modified molybdenum disulfide B is the same as that of modified molybdenum disulfide A, except that in step (2), the mass of modified kaolin is replaced by 0.4 g.

[0058] Preparation Example 3

[0059] The specific implementation method of modified molybdenum disulfide C is the same as that of modified molybdenum disulfide A, except that in step (7), the mass of polythiophene is replaced by 0.6 g.

[0060] Preparation Example 4

[0061] The synthesis method of the ultrahigh temperature resistant filler A comprises the following steps:

[0062] 1) 3g Sc 2 O 3 and 37g ZrO 2 Mix, add 50 ml of deionized water, ball mill at 65 r / min for 24 h, add 10 ml of deionized water, ball mill at 2700 r / min for 3 h, dry at 80 ° C for 24 h, pass through 80 mesh sieve, sinter at 1400 ° C for 4 h to obtain a mixture for use;

[0063] 2) 5 g of the mixture of step 1) and 4 ml of isopropyl tri(dioctyl pyrophosphate) titanate were mixed, 20 ml of anhydrous ethanol was added, the mixture was heated to 75° C., stirred for 30 min, washed with anhydrous ethanol and deionized water three times in sequence, and dried at 75° C. for 12 h to obtain ultrahigh temperature resistant filler A.

[0064] Preparation Example 5

[0065] The specific implementation method of ultrahigh temperature resistant filler B is the same as that of ultrahigh temperature resistant filler A, except that: in step 1), Sc 2 O 3 The mass of is replaced with 1.5g.

[0066] Preparation Example 6

[0067] The specific implementation of the ultrahigh temperature resistant filler C is the same as that of the ultrahigh temperature resistant filler A, except that in step 2), the volume of isopropyl tri(dioctyl pyrophosphate) titanate is replaced with 2 ml.

[0068] Example 1

[0069] A super-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing, comprising the following raw materials in parts by weight: 80 parts of methyl silicone resin, 10 parts of modified molybdenum disulfide A, 4 parts of super-high temperature resistant filler A, 3 parts of Tween 20, 4 parts of triethanolamine, 1.75 parts of silver-based catalyst and 150 parts of deionized water.

[0070] The preparation method of the ultra-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing in this embodiment comprises the following steps:

[0071] S1, adding methyl silicone resin, modified molybdenum disulfide A, ultrahigh temperature resistant filler A and Tween 20 into deionized water in sequence, stirring for 30 minutes to obtain a mixed solution for standby use;

[0072] S2. Add triethanolamine and a silver-based catalyst to the mixed solution of step S1 in sequence, and stir for 20 minutes to obtain an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging.

[0073] Example 2

[0074] A super-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing, comprising the following raw materials in parts by weight: 70 parts of methylphenyl silicone resin, 10 parts of modified molybdenum disulfide A, 2 parts of super-high temperature resistant filler A, 1 part of Tween 80, 2 parts of triethanolamine, 0.5 parts of silver-based catalyst and 100 parts of deionized water.

[0075] The preparation method of the ultra-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing in this embodiment comprises the following steps:

[0076] S1, adding methyl phenyl silicone resin, modified molybdenum disulfide A, ultrahigh temperature resistant filler A and Tween 80 into deionized water in sequence, stirring for 25 minutes to obtain a mixed solution for standby use;

[0077] S2. Add triethanolamine and a silver-based catalyst to the mixed solution of step S1 in sequence, and stir for 15 minutes to obtain an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging.

[0078] Example 3

[0079] A super-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing, comprising the following raw materials in parts by weight: 90 parts of methyl silicone resin, 10 parts of modified molybdenum disulfide A, 6 parts of super-high temperature resistant filler A, 5 parts of Tween 80, 6 parts of triethanolamine, 3 parts of silver-based catalyst and 200 parts of deionized water.

[0080] The preparation method of the ultra-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing in this embodiment comprises the following steps:

[0081] S1, add methyl silicone resin, modified molybdenum disulfide A, ultrahigh temperature resistant filler A and Tween 80 into deionized water in sequence, stir for 35 minutes, and obtain a mixed solution for standby use;

[0082] S2. Add triethanolamine and a silver-based catalyst to the mixed solution of step S1 in sequence, and stir for 25 minutes to obtain an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging.

[0083] Example 4

[0084] A super-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing, comprising the following raw materials in parts by weight: 75 parts of methyl silicone resin, 5 parts of modified molybdenum disulfide A, 4 parts of super-high temperature resistant filler A, 2 parts of Tween 80, 3 parts of triethanolamine, 1 part of silver-based catalyst, and 120 parts of deionized water.

[0085] The preparation method of the ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and pressing in this embodiment is the same as that in Example 1.

[0086] Example 5

[0087] A super-high temperature resistant room temperature curing mold release agent for titanium alloy forging and pressing, comprising the following raw materials in parts by weight: 85 parts of methylphenyl silicone resin, 15 parts of modified molybdenum disulfide A, 4 parts of super-high temperature resistant filler A, 4 parts of Tween 20, 5 parts of triethanolamine, 2 parts of silver-based catalyst, and 180 parts of deionized water.

[0088] The preparation method of the ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and pressing in this embodiment is the same as that in Example 1.

[0089] Example 6

[0090] This embodiment provides an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming and a preparation method thereof. The specific implementation method is the same as that of Example 1, except that modified molybdenum disulfide B replaces modified molybdenum disulfide A in equal amounts.

[0091] Example 7

[0092] This embodiment provides an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming and a preparation method thereof. The specific implementation method is the same as that of Example 1, except that modified molybdenum disulfide C replaces modified molybdenum disulfide A in equal amounts.

[0093] Example 8

[0094] This embodiment provides an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming and a preparation method thereof. The specific implementation method is the same as that of Example 1, except that the ultra-high temperature resistant filler B replaces the ultra-high temperature resistant filler A in equal amounts.

[0095] Example 9

[0096] This embodiment provides an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming and a preparation method thereof. The specific implementation method is the same as that of Example 1, except that the ultra-high temperature resistant filler C replaces the ultra-high temperature resistant filler A in equal amounts.

[0097] Example 10

[0098] This embodiment provides an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming and a preparation method thereof. The specific implementation method is the same as that of Example 1, except that an equal amount of zirconium oxide is used to replace the ultra-high temperature resistant filler A.

[0099] Comparative Example 1

[0100] This comparative example provides an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming and a preparation method thereof. The specific implementation method is the same as that of Example 1, except that an equal amount of molybdenum disulfide is used to replace modified molybdenum disulfide A.

[0101] Performance Testing

[0102] The lubricity and high temperature resistance of the ultra-high temperature resistant room temperature curing release agents for titanium alloy forging and pressing of the above-mentioned Examples 1-10 and Comparative Example 1 were tested, and the test results are shown in Table 1.

[0103] The release agents obtained in the examples and comparative examples were coated on a titanium alloy plate with a thickness of 20 μm, and the lubricity and high temperature resistance were tested after standing at room temperature for 24 hours.

[0104] (1) Lubricity

[0105] The lubricity of the release agent is determined by testing the friction coefficient. The smaller the friction coefficient, the better the lubricity. Refer to ASTM D1894-14.

[0106] (2) High temperature resistance

[0107] The thermal stability of the release agent is determined by testing with a thermogravimetric analyzer (TGA), with the decomposition temperature recorded as the high temperature resistance temperature. The higher the decomposition temperature, the better the high temperature resistance.

[0108] Table 1

[0109] Group Friction coefficient High temperature resistance (℃) Example 1 0.1105 1100 Example 2 0.1180 1090 Example 3 0.1200 1085 Example 4 0.1175 1087 Example 5 0.1170 1083 Example 6 0.1301 920 Example 7 0.1340 918 Example 8 0.1250 903 Example 9 0.1265 900 Example 10 0.1270 880 Comparative Example 1 0.1432 890

[0110] It can be seen from the data in Table 1 that the ultra-high temperature resistant room temperature curing mold release agent for titanium alloy forging and forming in Examples 1-5 of the present invention has a relatively small friction coefficient as a whole and can withstand temperatures above 1000°C, that is, it has high lubricity and ultra-high temperature resistance. Among them, Examples 6-7 respectively changed the amount of carrier modified kaolin and polythiophene added during the synthesis of lubricant modified molybdenum disulfide, which reduced the dispersibility of modified molybdenum disulfide, showed an increase in friction coefficient, that is, a significant decrease in lubrication, and caused a decrease in the high temperature resistance of the mold release agent; Examples 8-9 changed the amount of Sc in the ultra-high temperature resistant filler to reduce ... 2 O 3 And the addition ratio of isopropyl tri(dioctyl pyrophosphate) titanate, the toughness of zirconium dioxide is not well improved and the agglomeration phenomenon is aggravated, which leads to a decrease in the high temperature resistance of zirconium dioxide, thereby causing a significant decrease in the high temperature resistance of the release agent, but has little effect on the lubricity; Example 10 is to select zirconium oxide to replace the ultra-high temperature resistant filler A in equal amounts. The test found that the high temperature resistance of the release agent showed poor results, but had little effect on the lubricity; Comparative Example 1 is to replace the modified molybdenum disulfide A with molybdenum disulfide in equal amounts. The test found that the lubricity and high temperature resistance of the release agent both showed poor results.

[0111] The above implementation modes are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with this technology to understand the content of the present invention and implement it, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. A super-high temperature resistant room temperature curing release agent for titanium alloy forging, characterized in that: The release agent comprises the following raw materials in parts by weight: 70-90 parts of silicone resin, 5-15 parts of modified molybdenum disulfide, 2-6 parts of ultrahigh temperature resistant filler, 1-5 parts of surfactant, 2-6 parts of curing agent, 0.5-3 parts of silver-based catalyst, and 100-200 parts of deionized water.

2. The ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming according to claim 1, characterized in that: The organic silicone resin is methyl silicone resin or methylphenyl silicone resin.

3. The ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming according to claim 1, characterized in that: The preparation method of the modified molybdenum disulfide comprises the following steps: (1) placing kaolin in a reaction container, adding a sodium hydroxide aqueous solution, stirring, centrifuging, washing, filtering, taking a precipitate, drying, and grinding to obtain modified kaolin for later use; (2) taking the modified kaolin of step (1), adding deionized water, stirring, ultrasonicating, sequentially adding ammonium molybdate and thiourea, stirring, ultrasonicating, heating to 210-220° C., stirring, cooling to room temperature, filtering, taking solid, washing, drying, grinding, and obtaining a modified kaolin-molybdenum disulfide composite material for later use; (3) 5-bromo-2-carboxythiophene, N-methylformamide and cuprous bromide are sequentially added to a methanol solution of sodium methoxide, refluxed under an inert atmosphere, extracted, and the organic phase is collected to obtain product 1 for later use; (4) adding the product 1 of step (3), 3-bromo-1-propanol and sodium sulfite to toluene in sequence, heating to 90-110° C. under an inert atmosphere, washing, collecting the aqueous phase, and drying to obtain the product 2 for later use; (5) adding the product 2 of step (4) to tetrahydrofuran, adding a trimethylamine aqueous solution, stirring, distilling, washing, and drying to obtain a product 3 for standby use; (6) adding the product 3 of step (5) and ferric chloride to chloroform in sequence, stirring under an inert atmosphere, filtering, drying the solid, adding hydrazine hydrate, precipitating, and drying to obtain polythiophene for later use; (7) The modified kaolin-molybdenum disulfide composite material of step (2) and the polythiophene of step (6) are sequentially added into deionized water, ultrasonicated, allowed to stand, centrifuged, and freeze-dried to obtain modified molybdenum disulfide.

4. The ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming according to claim 3, characterized in that: In the step (2), the mass ratio of modified kaolin and ammonium molybdate is (0.06-0.1):

1.

5. The ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming according to claim 3, characterized in that: In the step (7), the mass ratio of the modified kaolin-molybdenum disulfide composite material to polythiophene is 1:(0.08-0.12).

6. The ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and forming according to claim 1, characterized in that: The preparation method of the ultrahigh temperature resistant filler comprises the following steps: 1) mixing Sc2O3 and ZrO2, adding deionized water, ball milling, adding deionized water, ball milling, drying, sieving, sintering, and obtaining a mixture for use; 2) The mixture of step 1) and isopropyl tri(dioctyl pyrophosphate acyloxy) titanate are mixed, anhydrous ethanol is added, the mixture is heated to 70-80° C., stirred, washed, and dried to obtain an ultrahigh temperature resistant filler.

7. The ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and press forming according to claim 6, characterized in that: In the step 1), the mass ratio of ZrO2 to Sc2O3 is 1:(0.06-0.1).

8. The ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and press forming according to claim 6, characterized in that: In the step 2), the ratio of the mixture to isopropyl tri(dioctyl pyrophosphate) titanate is 1 g: (0.6-1) ml.

9. The ultra-high temperature resistant room temperature curing release agent for titanium alloy forging and press forming according to claim 1, characterized in that: The curing agent is triethanolamine.

10. A method for preparing a super-high temperature resistant room temperature curing release agent for titanium alloy forging and pressing according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1. Add silicone resin, modified molybdenum disulfide, ultrahigh temperature resistant filler and surfactant into deionized water in sequence, stir for 25-35 minutes, and obtain a mixed solution for standby use; S2. Add the curing agent and the silver-based catalyst to the mixed solution of step S1 in sequence, and stir for 15-25 minutes to obtain an ultra-high temperature resistant room temperature curing release agent for titanium alloy forging.