An antiseptic ointment and a method of preparing the same

Abstract

This invention provides a preservative paste and its preparation method. The preservative paste comprises the following components in parts by weight: 1 part lithium-based grease, 0.2-0.4 parts petrolatum, 0.1-0.2 parts cerium polyisobutylene oxide, 0.1-0.2 parts talc, 0.05-0.1 parts porous quartz powder, 0.01-0.03 parts defoamer, 0.01-0.03 parts wetting and dispersing agent, 0.01-0.03 parts pentaerythritol diphosphite (bis(2,4-di-tert-butylphenol)), and 0.01-0.05 parts alkylpyridine quaternary ammonium salt. The preservative paste provided by this invention, by adding polyisobutylene, flake talc, porous quartz powder, defoamer, wetting agent, pentaerythritol diphosphite (2,4-di-tert-butylphenol), and alkylpyridine quaternary ammonium salt, results in a preservative paste with superior temperature resistance, aging resistance, and resistance to media corrosion.

Description

Technical Field

[0001] This invention relates to the field of metal corrosion protection technology, and more specifically, to a corrosion-preserving paste and its preparation method. Background Technology

[0002] As a primary structural material, steel suffers increasing economic losses and safety risks annually due to corrosion. Corrosion protection and repair of in-service steel structures are receiving growing attention. However, for complex steel structures, offshore platforms, and in-service pipelines in environments with limited construction conditions, conventional coating repairs often yield unsatisfactory results due to high surface treatment requirements and complex construction procedures. Conventional anti-corrosion pastes suffer from shortcomings such as poor aging resistance, low-temperature resistance, and poor adhesion. In particular, they cannot convert water during wet application, leading to corrosion and impacting the safe operation of in-service steel structures. Summary of the Invention

[0003] In view of this, the present invention proposes a preservative paste and its preparation method, aiming to solve the problems of existing preservative pastes having unsatisfactory aging resistance, high temperature resistance, poor adhesion, and inability to achieve water conversion.

[0004] In one aspect, the present invention provides an antiseptic paste comprising the following components in parts by weight: 1 part lithium-based grease, 0.2 to 0.4 parts petrolatum, 0.1 to 0.2 parts cerium polyisobutylene oxide, 0.1 to 0.2 parts talc, 0.05 to 0.1 parts porous quartz powder, 0.01 to 0.03 parts defoamer, 0.01 to 0.03 parts wetting and dispersing agent, 0.01 to 0.03 parts antioxidant, and 0.01 to 0.05 parts corrosion inhibitor.

[0005] Furthermore, in the above-mentioned preservative paste, the defoamer is a polyether siloxane copolymer; and / or the wetting and dispersing agent is a high molecular weight fatty acid derivative solution; and / or the antioxidant is bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite; and / or the corrosion inhibitor is an alkylpyridine quaternary ammonium salt.

[0006] Furthermore, in the above-mentioned preservative paste, the polyisobutylene cerium alcohol is synthesized by modification of highly reactive polyisobutylene with a molecular weight of 1000-3000, and its molecular formula is as follows: The structure of OR is as follows: The value of n ranges from 19 to 52.

[0007] On the other hand, the present invention also proposes a method for preparing a preservative paste, comprising the following steps: Step 1: Modify polyisobutylene to obtain polyisobutylene cerium alcohol; Step 2: Disperse and mix 1 part lithium-based grease, 0.2-0.4 parts petrolatum, 0.1-0.2 parts cerium polyisobutylene oxide, 0.1-0.2 parts flake talc, 0.05-0.1 parts porous quartz powder, 0.01-0.03 parts defoamer, 0.01-0.03 parts wetting and dispersing agent, 0.01-0.03 parts antioxidant, and 0.01-0.05 parts corrosion inhibitor to obtain an antiseptic paste.

[0008] Furthermore, in the above-mentioned method for preparing the preservative paste, step 1 includes the following steps: In the polyisobutylene catalytic oxidation step, polyisobutylene and the first catalyst are added to a reaction vessel, heated and stirred, and oxygen is introduced. Under the action of the catalyst, α-carbon atoms are oxidized to produce polyisobutylene aldehyde. In the catalytic hydrogenation step of polyisobutylene aldehyde, the polyisobutylene aldehyde and the second catalyst are added to a reaction vessel, heated and stirred to produce polyisobutylene alcohol. The synthesis steps of polyisobutylene alcohol cerium are as follows: CeCl3 is added to polyisobutylene alcohol, the pH is adjusted to alkaline, and the mixture is heated and stirred. Polyisobutylene alcohol and CeCl3 react to produce polyisobutylene alcohol cerium.

[0009] Furthermore, in the above-mentioned method for preparing the preservative paste, in the polyisobutylene catalytic oxidation step, the first catalyst is CuO; the amount of CuO added accounts for 2-5% of the mass ratio of the reactants.

[0010] Furthermore, in the above-mentioned method for preparing the preservative paste, in the polyisobutylene catalytic oxidation step, the reaction temperature of the polyisobutylene catalytic oxidation is 220-250℃, the reaction time is 2-3h, the stirring speed is 60-80 rpm, and the oxygen pressure is 1.3-1.5MPa.

[0011] Furthermore, in the above-mentioned method for preparing the preservative paste, in the step of catalytic hydrogenation of polyisobutylene aldehyde, the second catalyst is Os / ZnO, and the amount of Os and ZnO added accounts for 1-3% of the mass ratio of the reactants; the reaction temperature of catalytic hydrogenation of polyisobutylene aldehyde is 130-150℃, the reaction time is 3-4h, the stirring speed is 40-60 rpm, and the hydrogen pressure is 3.0-4.0MPa.

[0012] Furthermore, in the above-mentioned method for preparing the preservative paste, in the polyisobutylene cerium synthesis step, the molar ratio of polyisobutylene ethanol to CeCl3 is 3:(0.8-1.2).

[0013] Furthermore, in the above-mentioned method for preparing the preservative paste, in the polyisobutylene cerium synthesis step, ammonia gas is introduced to adjust the pH of the reaction system to 8-10.

[0014] Furthermore, in the above-mentioned method for preparing the preservative paste, in the polyisobutylene cerium synthesis step, the reaction temperature is 60-80℃, the reaction time is 2-3h, and the stirring speed is 60-80 rpm.

[0015] The preservative paste provided by this invention, by adding cerium polyisobutylene oxide, flake talc, porous quartz powder, defoamer, wetting agent, pentaerythritol diphosphite (2,4-di-tert-butylphenol), and alkylpyridine quaternary ammonium salt, results in a preservative paste with superior temperature resistance, aging resistance, and resistance to media corrosion. Detailed Implementation

[0016] Exemplary embodiments of this disclosure will now be described in more detail. These embodiments are provided to enable a more thorough understanding of this disclosure and to fully convey the scope of this disclosure to those skilled in the art. It should be noted that, unless otherwise specified, the embodiments and features described herein can be combined with each other.

[0017] The preservative paste of this invention comprises the following components in parts by weight: 1 part lithium-based grease, 0.2 to 0.4 parts petrolatum, 0.1 to 0.2 parts cerium polyisobutylene oxide, 0.1 to 0.2 parts talc, 0.05 to 0.1 parts porous quartz powder, 0.01 to 0.03 parts defoamer, 0.01 to 0.03 parts wetting and dispersing agent, 0.01 to 0.03 parts antioxidant, and 0.01 to 0.05 parts corrosion inhibitor.

[0018] Specifically, one part of lithium-based grease is used as the base grease for the preservative paste. If too little is added, it will not be able to wet the filler, affecting the anti-corrosion performance. If too much is added, it will increase the cost of the preservative paste and reduce its adhesion.

[0019] 0.2 to 0.4 parts of petroleum jelly, as an auxiliary oil in preservatives, can improve the water resistance of preservatives. Adding too little will not improve water resistance, while adding too much will affect the basic properties of the preservative.

[0020] Add 0.1 to 0.2 parts of talc powder. In practice, flake talc powder can be used to improve the water resistance of the preservative. Adding too little will not improve the water resistance of the preservative, while adding too much will affect the performance of the preservative.

[0021] Porous quartz powder (0.05–0.1 parts) improves the viscosity and adhesion of the preservative paste. Adding too little will not improve viscosity or adhesion, while adding too much will result in poor preservative performance. Defoamer (0.01–0.03 parts) is selected from polyether siloxane copolymer. Adding too little will not defoam, while adding too much will negatively impact the preservative paste's performance.

[0022] High molecular weight fatty acid derivative solutions can be used as wetting and dispersing agents. Adding too little will not achieve the desired wetting and dispersing effect, while adding too much will negatively impact the performance of the preservative. In this embodiment, TEGO245 is selected as the wetting and dispersing agent.

[0023] The antioxidant is pentaerythritol diphosphite (2,4-di-tert-butylphenol). Adding too little will not improve the antioxidant properties of the preservative, while adding too much will affect the performance of the preservative.

[0024] The corrosion inhibitor is an alkylpyridine quaternary ammonium salt. Adding too little will not inhibit corrosion, while adding too much will affect the performance of the preservative. Preferably, the pyridine quaternary ammonium salt is tetradecyl bromopyridine.

[0025] Porous quartz powder has a fine particle size of approximately 5 μm, uniform particle distribution, and a large specific surface area (approximately 8.3 m²). 2 The powdered quartz ( / g) has a nearly spherical and non-angular structure. Electron microscopy images show its surface is entirely composed of nanoscale mesopores, with an average pore size of approximately 8.8 nm. Porous quartz powder can improve the viscosity and adhesion of preservative pastes. Adding too little will not improve viscosity or adhesion, while adding too much will result in poor preservative performance.

[0026] The addition of 0.1-0.2 parts of cerium polyisobutylene oxide (CBE) improves the heat aging resistance of the preservative paste. Furthermore, alkoxides are readily hydrolyzed; during wet application, water preferentially reacts with the alkoxide, achieving water conversion and preventing further metal corrosion. Adding too little CBE will not improve the preservative paste's performance, while adding too much will increase costs and negatively impact its performance. In this embodiment, each cerium atom in the selected CBE is bonded to three alkoxy groups, resulting in higher reaction efficiency with water and better absorption of moisture, thus preventing metal corrosion.

[0027] In this embodiment of the invention, lithium-based grease is used as the base oil of the preservative paste, which plays a role in film formation and moisture isolation. The high hydrophobicity of petrolatum improves the water resistance of the base oil. Porous quartz and talc improve the viscosity of the base oil and increase the adhesion of the preservative paste to the substrate surface. High molecular weight fatty acid derivative solution improves the wetting effect of the preservative paste on the substrate surface. Bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite improves the aging resistance of the preservative paste. Alkylpyridine quaternary ammonium salt can inhibit corrosion. Polyisobutylene cerium can improve the heat aging resistance of the preservative paste. Moreover, alkoxides are easily hydrolyzed. When applied in wet conditions, water preferentially reacts with alkoxides, realizing the conversion of water and avoiding further corrosion of metals.

[0028] In practice, the preparation method of cerium polyisobutylene alcohol includes the following steps: In the catalytic oxidation step of polyisobutylene, highly active polyisobutylene and a first catalyst are added to a reaction vessel, heated and stirred, and oxygen is introduced. Under the action of the catalyst, α-carbon atoms are oxidized to produce polyisobutylene aldehyde. The molecular weight of polyisobutylene is 1000-3000, and the first catalyst is CuO. The amount of CuO added accounts for 2-5% of the total weight of the reactants, preferably 3%, which can effectively reduce the generation of by-products. The reaction temperature of polyisobutylene catalytic oxidation is 220-250℃, the reaction time is 2-3h, the stirring speed is 60-80 rpm, and the oxygen pressure is 1.3-1.5MPa.

[0029] In the catalytic hydrogenation step of polyisobutylene aldehyde, polyisobutylene aldehyde and a second catalyst are added to a reaction vessel, heated and stirred to undergo a catalytic hydrogenation reaction to generate polyisobutylene alcohol; wherein, the second catalyst is Os / ZnO, and the amount of Os and ZnO added accounts for 1-3% of the total mass ratio of the reactants, preferably 1.5%; the reaction temperature of polyisobutylene aldehyde catalytic hydrogenation is 130-150℃, the reaction time is 3-4h, the stirring speed is 40-60 rpm, and the hydrogen pressure is 3.0-4.0MPa.

[0030] The synthesis steps for polyisobutylene alcohol cerium are as follows: CeCl3 is added to polyisobutylene alcohol, the pH is adjusted to alkaline, and the mixture is heated and stirred to react the polyisobutylene alcohol with CeCl3 to produce polyisobutylene alcohol cerium. The molar ratio of polyisobutylene alcohol to CeCl3 is 3:(0.8–1.2). Ammonia gas is introduced to adjust the pH of the reaction system to 8–10, the reaction temperature is 60–80℃, the reaction time is 2–3 hours, and the stirring speed is 60–80 rpm.

[0031] The lithium-based grease, petrolatum, polyisobutylene, flake talc, porous quartz powder, polyether siloxane copolymer, high molecular weight fatty acid derivative solution, bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite, alkylpyridine quaternary ammonium salt, CeCl3, CuO, Os, ZnO, hydrogen, oxygen, and ammonia used in the embodiments of this invention were all purchased from Tianjin Jiangtian Chemical Technology Co., Ltd.

[0032] This invention also provides a method for preparing a preservative paste, comprising the following steps: Step S1: Modify polyisobutylene to obtain polyisobutylene cerium alcohol; Specifically, it includes the following sub-steps: In sub-step S101, polyisobutylene and the first catalyst are added to the reaction vessel, heated and stirred, and oxygen is introduced. Under the action of the catalyst, α-carbon atoms are oxidized to generate polyisobutylene aldehyde. In sub-step S102, polyisobutylene aldehyde and the second catalyst are added to the reaction vessel, heated and stirred to undergo catalytic hydrogenation reaction to generate polyisobutylene alcohol; In sub-step S103, CeCl3 is added to polyisobutylene alcohol, the pH is adjusted to alkaline, and the mixture is heated and stirred. Polyisobutylene alcohol reacts with CeCl3 to generate cerium polyisobutylene alcohol.

[0033] In sub-step S101, the first catalyst is CuO; the amount of CuO added accounts for 2-5% of the mass of the reactants, preferably 3%; the reaction temperature for the catalytic oxidation of polyisobutylene is 220-250℃, the reaction time is 2-3h, the stirring speed is 60-80 rpm, and the oxygen pressure is 1.3-1.5MPa.

[0034] In sub-step S102, the second catalyst is a mixed catalyst of Os and ZnO with a mass ratio of 1:1. The amount of the mixed catalyst formed by Os and ZnO added accounts for 1-3% of the mass ratio of the reactants, preferably 1.5%. The reaction temperature for the catalytic hydrogenation of polyisobutylene aldehyde is 130-150℃, the reaction time is 3-4h, the stirring speed is 40-60 rpm, and the hydrogen pressure is 3.0-4.0MPa.

[0035] In sub-step S103, the molar ratio of polyisobutylene alcohol to CeCl3 is 3:(0.8-1.2); ammonia gas is introduced to adjust the pH of the reaction system to 8-10, the reaction temperature is 60-80℃, the reaction time is 2-3h, and the stirring speed is 60-80rpm.

[0036] Step S2: Disperse and mix 1 part lithium-based grease, 0.2-0.4 parts petrolatum, 0.1-0.2 parts polyisobutylene cerium, 0.1-0.2 parts flaky talc, 0.05-0.1 parts porous quartz powder, 0.01-0.03 parts defoamer, 0.01-0.03 parts high molecular weight fatty acid derivative solution, 0.01-0.03 parts antioxidant and 0.01-0.05 parts corrosion inhibitor to obtain a preservative paste.

[0037] Specifically, the dispersion and mixing method is to use a high-speed disperser, with a stirring speed of 500-700 rpm and a time of 20-35 minutes.

[0038] The present invention will be described in detail below with reference to specific embodiments: Example 1 (1) Add 100g of polyisobutylene with a molecular weight of 1000-3000 and 3g of CuO to a reaction vessel, introduce oxygen to a pressure of 1.3MPa, heat to 220℃, stir at 60rpm for 2h, and cool to room temperature to obtain polyisobutylene aldehyde. (2) Add polyisobutylene aldehyde and 2g of Os and ZnO mixed catalyst with a mass ratio of 1:1 to the reactor, introduce hydrogen gas to a pressure of 4MPa, heat to 130℃, stir at 40rpm for 3h, and cool to room temperature to obtain polyisobutylene alcohol. (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:0.8 to the reactor, introduce ammonia to adjust the pH to 8, heat to 60°C, stir at 60 rpm for 2 hours, and cool to room temperature to obtain polyisobutylene alcohol cerium.

[0039] (4) For every 1000g, add 1 part lithium-based grease, 0.2 parts petrolatum, 0.1 parts polyisobutylene cerium, 0.1 parts flake talc, 0.05 parts porous quartz powder, 0.01 parts polyether siloxane copolymer, 0.01 parts high molecular weight fatty acid derivative solution, 0.01 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite and 0.01 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 500 rpm for 20 min to form an antiseptic paste.

[0040] Example 2 (1) 100g of polyisobutylene with a molecular weight of 1000-3000 and 2.5g of CuO were added to the reactor, oxygen was introduced to a pressure of 1.4MPa, the temperature was heated to 220℃, and the mixture was stirred at 70rpm for 2.5h. The mixture was then cooled to room temperature to obtain polyisobutylene aldehyde. (2) Polyisobutylene aldehyde, 1.2g of Os and ZnO mixed catalyst in a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to a pressure of 3MPa, heated to 140℃, stirred at 50rpm for 3h, and cooled to room temperature to obtain polyisobutylene alcohol.

[0041] (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:0.9 to the reactor, introduce ammonia to adjust the pH to 8, heat to 60°C, stir at 80 rpm for 2 hours, and cool to room temperature to obtain polyisobutylene alcohol cerium. (4) For every 1000g, add 1 part lithium-based grease, 0.2 parts petrolatum, 0.15 parts polyisobutylene cerium, 0.15 parts flake talc, 0.08 parts porous quartz powder, 0.02 parts polyether siloxane copolymer, 0.02 parts high molecular weight fatty acid derivative solution, 0.02 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite and 0.02 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 600 rpm for 30 min to form an antiseptic paste.

[0042] Example 3 (1) Polyisobutylene with a molecular weight of 1000-3000 and 4g of CuO were added to the reactor, oxygen was introduced to a pressure of 1.5MPa, the temperature was heated to 220℃, and the mixture was stirred at 80rpm for 3h. After cooling to room temperature, polyisobutylene aldehyde was obtained.

[0043] (2) Polyisobutylene aldehyde and 1.2g of Os and ZnO mixed catalyst in a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to a pressure of 3MPa, heated to 150℃, stirred at 60rpm for 3h, and cooled to room temperature to obtain polyisobutylene alcohol. (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:0.8 to the reaction vessel, introduce ammonia to adjust the pH to 8, heat to 60°C, stir at 60 rpm for 2 h, and cool to room temperature to obtain polyisobutylene alcohol cerium. (4) For every 1000g, add 1 part lithium-based grease, 0.2 parts petrolatum, 0.2 parts polyisobutylene cerium, 0.2 parts flake talc, 0.1 parts porous quartz powder, 0.03 parts polyether siloxane copolymer, 0.03 parts high molecular weight fatty acid derivative solution, 0.03 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite and 0.05 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 700 rpm for 35 min to form an antiseptic paste.

[0044] Example 4 (1) 100g of polyisobutylene with a molecular weight of 1000-3000 and 4.3g of CuO were added to the reactor, oxygen was introduced to a pressure of 1.3MPa, the temperature was heated to 220℃, and the mixture was stirred at 60rpm for 2h. The mixture was then cooled to room temperature to obtain polyisobutylene aldehyde. (2) Polyisobutylene aldehyde, 2.8g of Os and ZnO mixed catalyst with a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to a pressure of 3MPa, heated to 140℃, stirred at 40rpm for 3h, and cooled to room temperature to obtain polyisobutylene alcohol. (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:0.8 to the reaction vessel, introduce ammonia to adjust the pH to 8, heat to 80°C, stir at 80 rpm for 3 hours, and cool to room temperature to obtain polyisobutylene alcohol cerium. (4) For every 1000g, add 1 part lithium-based grease, 0.3 parts petrolatum, 0.1 parts polyisobutylene cerium, 0.1 parts flake talc, 0.05 parts porous quartz powder, 0.01 parts polyether siloxane copolymer, 0.01 parts high molecular weight fatty acid derivative solution, 0.01 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite and 0.01 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 500 rpm for 20 min to form an antiseptic paste.

[0045] Example 5 (1) 100g of polyisobutylene with a molecular weight of 1000-3000 and 4.5g of CuO were added to the reactor, oxygen was introduced to a pressure of 1.4MPa, the temperature was heated to 235℃, and the mixture was stirred at 70rpm for 2h. The mixture was then cooled to room temperature to obtain polyisobutylene aldehyde. (2) Polyisobutylene aldehyde, 1.3g of Os and ZnO mixed catalyst in a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to a pressure of 3MPa, heated to 140℃, stirred at 50rpm for 3h, and cooled to room temperature to obtain polyisobutylene alcohol. (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:0.8 to the reaction vessel, introduce ammonia to adjust the pH to 9, heat to 80°C, stir at 80 rpm for 3 hours, and cool to room temperature to obtain polyisobutylene alcohol cerium; (3) For every 1000g, add 1 part lithium-based grease, 0.3 parts petrolatum, 0.15 parts polyisobutylene cerium, 0.15 parts flake talc, 0.08 parts porous quartz powder, 0.02 parts polyether siloxane copolymer, 0.02 parts high molecular weight fatty acid derivative solution, 0.02 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite and 0.02 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 600 rpm for 30 min to form an antiseptic paste.

[0046] Example 6 (1) 100g of polyisobutylene with a molecular weight of 1000-3000 and 3.1g of CuO were added to the reactor, oxygen was introduced to a pressure of 1.5MPa, the temperature was heated to 235℃, and the mixture was stirred at 80rpm for 3h. The mixture was then cooled to room temperature to obtain polyisobutylene aldehyde. (2) Polyisobutylene aldehyde, 2.2g of Os and ZnO mixed catalyst with a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to a pressure of 3MPa, heated to 150℃, stirred at 60rpm for 4h, and cooled to room temperature to obtain polyisobutylene alcohol. (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:1 to the reactor, introduce ammonia to adjust the pH to 9, heat to 80°C, stir at 80 rpm for 3 hours, and cool to room temperature to obtain polyisobutylene alcohol cerium. (4) For every 1000g, add 1 part lithium-based grease, 0.3 parts petrolatum, 0.2 parts polyisobutylene cerium, 0.2 parts flake talc, 0.1 parts porous quartz powder, 0.03 parts polyether siloxane copolymer, 0.03 parts high molecular weight fatty acid derivative solution, 0.03 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite and 0.05 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 700 rpm for 35 min to form an antiseptic paste.

[0047] Example 7 (1) 100g of polyisobutylene with a molecular weight of 1000-3000 and 2.8g of CuO were added to the reactor, oxygen was introduced to a pressure of 1.4MPa, the temperature was heated to 235℃, and the mixture was stirred at 70rpm for 2.5h. The mixture was then cooled to room temperature to obtain polyisobutylene aldehyde. (2) Polyisobutylene aldehyde and 2.4g of Os and ZnO mixed catalyst in a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to a pressure of 4MPa, heated to 140℃, stirred at 40rpm for 4h, and cooled to room temperature to obtain polyisobutylene alcohol. (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:1 to the reaction vessel, introduce ammonia to adjust the pH to 9, heat to 70°C, stir at 70 rpm for 2 h, and cool to room temperature to obtain polyisobutylene alcohol cerium. (4) For every 1000g, add 1 part lithium-based grease, 0.3 parts petrolatum, 0.15 parts polyisobutylene cerium, 0.15 parts flake talc, 0.05 parts porous quartz powder, 0.01 parts polyether siloxane copolymer, 0.01 parts high molecular weight fatty acid derivative solution, 0.01 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite, and 0.01 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 500 rpm for 20 min to form an antiseptic paste.

[0048] Example 8 (1) 100g of polyisobutylene with a molecular weight of 1000-3000 and 3.7g of CuO were added to the reactor, oxygen was introduced to a pressure of 1.5MPa, the temperature was heated to 250℃, and the mixture was stirred at 60rpm for 2h. The mixture was then cooled to room temperature to obtain polyisobutylene aldehyde. (2) Polyisobutylene aldehyde and 2.5g of Os and ZnO mixed catalyst in a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to a pressure of 4MPa, heated to 150℃, stirred at 60rpm for 4h, and cooled to room temperature to obtain polyisobutylene alcohol. (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:1 to the reactor, introduce ammonia to adjust the pH to 10, heat to 70°C, stir at 70 rpm for 2 hours, and cool to room temperature to obtain polyisobutylene alcohol cerium. (4) For every 1000g, add 1 part lithium-based grease, 0.4 parts petrolatum, 0.1 parts polyisobutylene cerium, 0.1 parts flake talc, 0.08 parts porous quartz powder, 0.02 parts polyether siloxane copolymer, 0.02 parts high molecular weight fatty acid derivative solution, 0.02 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite, and 0.02 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 600 rpm for 30 min to form an antiseptic paste.

[0049] Example 9 (1) Add 100g of polyisobutylene with a molecular weight of 1000-3000 and 3g of CuO to a reaction vessel, introduce oxygen to a pressure of 1.4MPa, heat to 250℃, stir at 70rpm for 2.5h, and cool to room temperature to obtain polyisobutylene aldehyde. (2) Polyisobutylene aldehyde and 2g of Os and ZnO mixed catalyst with a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to a pressure of 4MPa, heated to 130℃, stirred at 50rpm for 4h, and cooled to room temperature to obtain polyisobutylene alcohol.

[0050] (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:1.1 to the reaction vessel, introduce ammonia to adjust the pH to 10, heat to 70°C, stir at 70 rpm for 3 hours, and cool to room temperature to obtain polyisobutylene alcohol cerium. (4) For every 1000g, add 1 part lithium-based grease, 0.4 parts petrolatum, 0.15 parts polyisobutylene cerium, 0.15 parts flake talc, 0.1 parts porous quartz powder, 0.03 parts polyether siloxane copolymer, 0.03 parts high molecular weight fatty acid derivative solution, 0.03 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite, and 0.05 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 700 rpm for 35 min to form an antiseptic paste.

[0051] Example 10 (1) 100g of polyisobutylene with a molecular weight of 1000-3000 and 4g of CuO were added to the reactor, oxygen was introduced to 1.5MPa, heated to 250℃, stirred at 80rpm for 3h, and cooled to room temperature to obtain polyisobutylene aldehyde. (2) Polyisobutylene aldehyde and 2.5g of Os and ZnO mixed catalyst in a mass ratio of 1:1 were added to the reactor, hydrogen gas was introduced to 4MPa, heated to 130℃, stirred at 40rpm for 4h, and cooled to room temperature to obtain polyisobutylene alcohol. (3) Add polyisobutylene alcohol and CeCl3 in a molar ratio of 3:1.2 to the reaction vessel, introduce ammonia to adjust the pH to 10, heat to 70°C, stir at 70 rpm for 2 h, and cool to room temperature to obtain polyisobutylene alcohol cerium. (4) For every 1000g, add 1 part lithium-based grease, 0.4 parts petrolatum, 0.2 parts polyisobutylene cerium, 0.2 parts flake talc, 0.1 parts porous quartz powder, 0.03 parts polyether siloxane copolymer, 0.03 parts high molecular weight fatty acid derivative solution, 0.03 parts bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite, and 0.05 parts alkylpyridine quaternary ammonium salt to a high-speed disperser and disperse at 700 rpm for 35 min to form an antiseptic paste.

[0052] Comparative Example 1 Except for the omission of cerium polyisobutylene alcohol, the other steps and components are the same as in Example 1.

[0053] Comparative Example 2 Except for the amount of cerium polyisobutylene oxide (CPE) being 0.4 parts, all other steps and components are the same as in Example 1.

[0054] Comparative Example 3 In the preparation of polyisobutylene cerium, the reaction temperature for the oxidation of polyisobutylene to prepare polyisobutylene aldehyde is 150°C, and the other steps and components are the same as in Example 1.

[0055] Comparative Example 4 In the preparation of polyisobutylene cerium, the reaction temperature during the hydrogenation reduction of polyisobutylene aldehyde is 180°C, and the other steps and components are the same as in Example 1.

[0056] Comparative Example 5 In the preparation process of polyisobutylene alcohol cerium, the molar ratio of polyisobutylene alcohol to CeCl3 is 3:0.5, and other steps and components are the same as in Example 1.

[0057] Comparative Example 6 In the preparation of polyisobutylene cerium, the reaction time for the hydrogenation reduction of polyisobutylene aldehyde is 2 hours, and the other steps and components are the same as in Example 1.

[0058] The component ratios of the preservative paste prepared in the embodiments of the present invention and the preservative paste prepared in the comparative example are shown in the following table:

[0059] Furthermore, the preservative pastes prepared in Examples 1-7 and Comparative Examples 1-6 of this invention were subjected to wet coating tests. After completion, performance tests were conducted, including neutral salt spray test (3000h), 10% NaCl (50℃, 90d) immersion test, and ultraviolet aging test (3000h). The results are shown in the table below:

[0060] The data in the table above shows that: In Comparative Example 1, no polyisobutylene cerium was added, and all other steps were the same as in Example 1. The results showed that the anti-corrosion paste changed color and the specimens rusted.

[0061] In Comparative Example 2, 0.4 parts of polyisobutylene cerium were added, and the rest were the same as in Example 1. As a result, the anti-corrosion paste fell off and the specimens rusted.

[0062] In Comparative Example 3, during the preparation of polyisobutylene cerium, the reaction temperature for the oxidation of polyisobutylene to polyisobutylene aldehyde was 150°C, which is lower than the 220-250°C range of the present invention. The rest were the same as in Example 1. As a result, the anti-corrosion paste changed color and the specimen rusted.

[0063] In Comparative Example 4, during the preparation of polyisobutylene cerium, the reaction temperature during the hydrogenation reduction of polyisobutylene aldehyde was 180°C, which is higher than the reaction temperature range of 130-150°C in the embodiment of the present invention. The rest was the same as in Example 1. As a result, the anti-corrosion paste changed color and the specimen rusted.

[0064] In Comparative Example 5, during the preparation of polyisobutylene cerium, the molar ratio of polyisobutylene ethanol to CeCl3 was 3:0.5, which is less than the range of 3:(0.8~1.2) in this application. All other aspects were the same as in Example 1. As a result, the anti-corrosion paste changed color and the specimen rusted.

[0065] In Comparative Example 6, during the preparation of polyisobutylene cerium, the reaction time for the hydrogenation reduction of polyisobutylene aldehyde was 2 hours, which is less than the 3-4 hours range of this application. The rest was the same as in Example 1. As a result, the antiseptic paste changed color and the specimen rusted.

[0066] The data in the table above shows that: This invention, by adding cerium polyisobutylene oxide, flake talc, porous quartz powder, defoamer, wetting agent, pentaerythritol diphosphite (2,4-di-tert-butylphenol), and alkylpyridine quaternary ammonium salt, and controlling the ratio between the components and factors such as reaction temperature and reaction time in the preparation process, results in a preservative paste with superior temperature resistance, aging resistance, and resistance to media corrosion.

[0067] The anti-corrosion paste prepared in this embodiment of the invention has good temperature resistance, aging resistance and corrosion resistance. On-site construction requires low surface treatment (no special treatment is required for the metal surface to achieve good anti-corrosion effect). It can be applied to wet and rusty surfaces and can be used for coating repair of complex steel structures and in-service pipelines.

[0068] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.

Claims

1. A preservative paste, characterized in that, It is composed of the following components in parts by weight: 1 part lithium-based grease, 0.2-0.4 parts petrolatum, 0.1-0.2 parts cerium polyisobutylene oxide, 0.1-0.2 parts talc, 0.05-0.1 parts porous quartz powder, 0.01-0.03 parts defoamer, 0.01-0.03 parts wetting and dispersing agent, 0.01-0.03 parts antioxidant, and 0.01-0.05 parts corrosion inhibitor; wherein the cerium polyisobutylene oxide is synthesized by modifying highly active polyisobutylene with a molecular weight of 1000-3000. The preparation method of the polyisobutylene cerium alcohol includes the following steps: In the polyisobutylene catalytic oxidation step, polyisobutylene and a first catalyst are added to a reaction vessel, heated and stirred, and oxygen is introduced. Under the action of the catalyst, α-carbon atoms are oxidized to generate polyisobutylene aldehyde; the reaction temperature of the polyisobutylene catalytic oxidation is 220-250℃. In the catalytic hydrogenation step of polyisobutylene aldehyde, the polyisobutylene aldehyde and the second catalyst are added to a reaction vessel, heated and stirred to undergo a catalytic hydrogenation reaction to generate polyisobutylene alcohol; the reaction temperature of the catalytic hydrogenation of polyisobutylene aldehyde is 130-150℃, and the reaction time is 3-4h. The synthesis steps of polyisobutylene alcohol cerium are as follows: CeCl3 is added to polyisobutylene alcohol, the pH is adjusted to alkaline, and the mixture is heated and stirred. Polyisobutylene alcohol and CeCl3 react to generate polyisobutylene alcohol cerium; wherein, the molar ratio of polyisobutylene alcohol to CeCl3 is 3: (0.8~1.2).

2. The preservative paste according to claim 1, characterized in that, The molecular formula of the polyisobutylene cerium alcohol is as follows: The structure of OR is as follows: The value of n ranges from 19 to 52.

3. The preservative paste according to claim 1, characterized in that, The defoamer is a polyether siloxane copolymer; and / or the wetting and dispersing agent is a high molecular weight fatty acid derivative solution; and / or the antioxidant is bis(2,4-di-tert-butylphenol) pentaerythritol diphosphite; and / or the corrosion inhibitor is an alkylpyridine quaternary ammonium salt.

4. A method for preparing the preservative paste as described in claim 1 or 2, characterized in that, Includes the following steps: Step 1: Modify polyisobutylene to obtain the polyisobutylene cerium alcohol; Step 2: Disperse and mix the following components: 1 part lithium-based grease, 0.2-0.4 parts petrolatum, 0.1-0.2 parts cerium polyisobutylene oxide, 0.1-0.2 parts flaky talc, 0.05-0.1 parts porous quartz powder, 0.01-0.03 parts defoamer, 0.01-0.03 parts wetting and dispersing agent, 0.01-0.03 parts antioxidant, and 0.01-0.05 parts corrosion inhibitor to obtain an antiseptic paste.

5. The method for preparing the preservative paste according to claim 4, characterized in that, In the polyisobutylene catalytic oxidation step, the first catalyst is CuO; the amount of CuO added accounts for 2-5% of the mass of the reactants.

6. The method for preparing the preservative paste according to claim 4, characterized in that, In the polyisobutylene catalytic oxidation step, the reaction time is 2-3 hours, the stirring speed is 60-80 rpm, and the oxygen pressure is 1.3-1.5 MPa.

7. The method for preparing the preservative paste according to claim 4, characterized in that, In the catalytic hydrogenation step of polyisobutylene aldehyde, the second catalyst is Os / ZnO, and the addition amount of Os and ZnO accounts for 1-3% of the mass ratio of the reactants; the stirring speed is 40-60 rpm, and the hydrogen pressure is 3.0-4.0 MPa.

8. The method for preparing the preservative paste according to claim 4, characterized in that, In the polyisobutylene cerium synthesis step, ammonia gas is introduced to adjust the pH of the reaction system to 8-10.

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