阅读说明：本技术 一种长寿命极压抗磨液压油及其制备方法 (Long-life extreme pressure antiwear hydraulic oil and preparation method thereof ) 是由 张炳初 于 2021-06-18 设计创作，主要内容包括：本发明公开一种长寿命极压抗磨液压油及其制备方法,包括97.56-98.46份基础油,1.54-2.44份复合添加剂；复合添加剂包括复配抗氧剂、降凝剂、破乳剂、消泡剂和含ZDDP的抗磨液压油复合剂,该复合添加剂包括如下步骤制成：按重量份计,将0.1-0.25份复配抗氧剂加入三口烧瓶中,升温至70℃,磁力搅拌30-40mi n,之后依次加入0.1-0.5份降凝剂、0.8-1份含ZDDP的抗磨液压油复合剂、0.01-0.1份破乳剂和0.01份消泡剂,混合均匀,制得复合添加剂；通过有机钼、胺类抗氧剂与复合剂里含有的ZDDP形成三元复合抗氧剂,不仅具有优异的抗氧化性能,还可获得优秀的极压、抗磨和减摩性能。(The invention discloses long-life extreme pressure anti-wear hydraulic oil and a preparation method thereof, wherein the long-life extreme pressure anti-wear hydraulic oil comprises 97.56-98.46 parts of base oil and 1.54-2.44 parts of compound additive; the composite additive comprises a compound antioxidant, a pour point depressant, a demulsifier, a defoaming agent and an anti-wear hydraulic oil complexing agent containing ZDDP, and is prepared by the following steps: adding 0.1-0.25 part of compound antioxidant into a three-neck flask, heating to 70 ℃, magnetically stirring for 30-40min, sequentially adding 0.1-0.5 part of pour point depressant, 0.8-1 part of wear-resistant hydraulic oil complexing agent containing ZDDP, 0.01-0.1 part of demulsifier and 0.01 part of defoamer, and uniformly mixing to obtain a composite additive; the ternary composite antioxidant is formed by organic molybdenum, amine antioxidant and ZDDP contained in the complexing agent, and has excellent antioxidant performance and excellent extreme pressure, wear resistance and antifriction performance.)

1. The long-life extreme pressure antiwear hydraulic oil comprises the following raw materials in parts by weight: 97.56-98.46 parts of base oil and 1.54-2.44 parts of compound additive; the composite additive comprises a compound antioxidant, a pour point depressant, a demulsifier, a defoaming agent and an anti-wear hydraulic oil complexing agent containing ZDDP, and is characterized by comprising the following steps:

adding 0.1-0.25 part of compound antioxidant into a three-neck flask, heating to 70 ℃, magnetically stirring for 30-40min, then sequentially adding 0.1-0.5 part of pour point depressant, 0.8-1 part of antiwear hydraulic oil complexing agent containing ZDDP, 0.01-0.1 part of demulsifier and 0.01 part of defoamer, and uniformly mixing to obtain the composite additive.

2. The long-life extreme pressure anti-wear hydraulic oil according to claim 1, wherein the base oil is a second-class hydrogenated base oil, the compound antioxidant is a compound of organic molybdenum or alkyl thiocarbamic acid and an amine antioxidant in a weight ratio of 1: 20, the pour point depressant is a polymethacrylate pour point depressant, and the demulsifier is a condensate of amine and an epoxy compound or an oil ether high molecular compound synthesized by multiple monomers.

3. The long-life extreme pressure anti-wear hydraulic oil as claimed in claim 1, wherein the defoaming agent is prepared by the following steps:

step S1, sequentially adding polyethylene glycol, tetra-n-butylammonium bromide and sodium hydroxide into a three-neck flask, heating in a water bath at 35-40 ℃, dropwise adding epichlorohydrin, heating to 55 ℃ after completely adding the epichlorohydrin, then adding a sodium hydroxide aqueous solution with the mass fraction of 10%, stirring at a constant speed, reacting for 2 hours, cooling, performing suction filtration, adjusting the pH value to be neutral, performing reduced pressure distillation to obtain an intermediate 1, controlling the molar ratio of the total amount of the polyethylene glycol, the tetra-n-butylammonium bromide, the sodium hydroxide and the epichlorohydrin to be 1: 0.02: 3: 2.5, and controlling the molar ratio of the sodium hydroxide adding amount in two times to be 1: 1;

step S2, adding the prepared intermediate 1 into deionized water, dropwise adding sulfuric acid with the mass fraction of 75%, uniformly stirring and hydrolyzing for 3h, then adding sodium carbonate to adjust the pH of the system to be neutral, carrying out reduced pressure distillation at the temperature of 90 ℃ and the vacuum degree of 0.080MPa, and carrying out suction filtration to obtain an intermediate 2, wherein the use amount of the sulfuric acid is controlled to be 1-5% of the weight of the intermediate 1;

step S3, adding the prepared intermediate 2 and a catalyst into a reaction kettle, performing vacuum dehydration and replacement with nitrogen for three times, stirring at a constant speed, heating to 120 ℃, adding allyl glycidyl ether, stirring at a constant speed after completely adding, and reacting for 4 hours to prepare an intermediate 3, wherein the weight ratio of the intermediate 2 to the allyl glycidyl ether is controlled to be 0.8: 0.2, and the amount of the catalyst is 1% of the weight of the intermediate 2;

step S4, adding the prepared intermediate 3 into a three-neck flask, sequentially adding hydroquinone and p-toluenesulfonic acid, heating to 80 ℃ while stirring, adding tetradecanoic acid, continuously heating to 110 ℃, stirring at a constant speed, reacting for 2 hours, heating to 130 ℃, stirring at a constant speed until the reaction is finished, cooling to 90 ℃, distilling under reduced pressure, purifying to obtain an intermediate 4, and controlling the weight ratio of the intermediate 3 to the hydroquinone to the p-toluenesulfonic acid to the tetradecanoic acid to be 10: 0.1: 0.2: 2.80-2.85;

step S5, adding low-hydrogen silicone oil into a three-neck flask, adding the prepared intermediate 4 and isopropanol, stirring at a constant speed, heating to 70 ℃, adding chloroplatinic acid, continuing heating to 85 ℃, stirring at a constant speed, reacting for 6 hours, preparing a crude product after the reaction is finished, and distilling under reduced pressure to prepare the defoaming agent, wherein the weight ratio of the low-hydrogen silicone oil to the intermediate 4 is controlled to be 0.5: 1, the dosage of the isopropanol is 30% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4, and the dosage of the chloroplatinic acid is 0.1% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4.

4. The long-life extreme pressure antiwear hydraulic oil of claim 3, wherein the catalyst in step S3 is a double metal cyanide complex.

5. The preparation method of the long-life extreme pressure anti-wear hydraulic oil as claimed in claim 1, characterized by comprising the following steps:

heating the base oil to 70 ℃, adding the composite additive, magnetically stirring for 60min, and filtering to obtain the long-life extreme pressure antiwear hydraulic oil.

Technical Field

The invention belongs to the technical field of industrial lubricating oil, and particularly relates to long-life extreme pressure antiwear hydraulic oil and a preparation method thereof.

Background

Along with the rapid development of infrastructure, particularly the acceleration of urbanization process and railway construction pace, mechanical equipment, particularly excavators and other equipment are applied more and more, the structure and working conditions of a hydraulic system of the mechanical equipment are greatly different from those of a common industrial hydraulic system, and the common industrial wear-resistant hydraulic oil is frequently subjected to various faults, such as frequent hydraulic pump damage, weak arm hooking action, lag, overhigh oil temperature, blackening and bluing of a piston rod and the like, because field construction machinery such as engineering machinery belongs to heavy equipment, the working load is large, the working pressure is high, generally 21-35 MPa and up to 42MPa, the industrial hydraulic system is generally 15-25 MPa, the pressure is high, the hydraulic pump is easy to wear quickly, the service life is short, and therefore higher wear resistance of oil is required; in addition, the equipment has compact structure, small oil tank and no special cooling system, so that the oil temperature is high, usually 80-100 ℃, and 50-70 ℃ in an industrial hydraulic system, so that the oil oxidation is accelerated and the service life is shortened, and the oil is required to have better anti-oxidation stability.

Disclosure of Invention

In order to overcome the technical problems, the invention provides long-life extreme pressure antiwear hydraulic oil and a preparation method thereof.

The purpose of the invention can be realized by the following technical scheme:

the long-life extreme pressure antiwear hydraulic oil comprises the following raw materials in parts by weight: 97.56-98.46 parts of base oil and 1.54-2.44 parts of compound additive; the composite additive comprises a compound antioxidant, a pour point depressant, a demulsifier, a defoaming agent and an anti-wear hydraulic oil complexing agent containing ZDDP, and is prepared by the following steps:

adding 0.1-0.25 part of compound antioxidant into a three-neck flask, heating to 70 ℃, magnetically stirring for 30-40min, then sequentially adding 0.1-0.5 part of pour point depressant, 0.8-1 part of antiwear hydraulic oil complexing agent containing ZDDP, 0.01-0.1 part of demulsifier and 0.01 part of defoamer, and uniformly mixing to obtain the composite additive.

Further, the base oil is second-class hydrogenated base oil, the compound antioxidant is compounded by organic molybdenum or alkyl thiocarbamic acid compounds and amine antioxidants according to the weight ratio of 1: 20, the pour point depressant is a polymethacrylate pour point depressant, and the demulsifier amine and epoxy compound condensation compound or an oil ether high molecular compound synthesized by multiple monomers.

Further, the organic molybdenum or alkyl thiocarbamic acid compound is one or more of diisooctyl molybdenum dithiophosphate, molybdenum dialkyl dithiocarbamate and dialkyl dithiocarbamate which are mixed according to any proportion.

Further, the amine antioxidant is one or more of dioctyl diphenylamine, butyl octyl diphenylamine, dinonyl diphenylamine and N-phenyl-a naphthylamine which are mixed according to any proportion.

Further, the defoaming agent is prepared by the following steps:

step S1, sequentially adding polyethylene glycol, tetra-n-butylammonium bromide and sodium hydroxide into a three-neck flask, heating in a water bath at 35-40 ℃, dropwise adding epichlorohydrin, heating to 55 ℃ after completely adding the epichlorohydrin, then adding a sodium hydroxide aqueous solution with the mass fraction of 10%, stirring at a constant speed, reacting for 2 hours, cooling, performing suction filtration, adjusting the pH value to be neutral, performing reduced pressure distillation to obtain an intermediate 1, controlling the molar ratio of the total amount of the polyethylene glycol, the tetra-n-butylammonium bromide, the sodium hydroxide and the epichlorohydrin to be 1: 0.02: 3: 2.5, and controlling the molar ratio of the sodium hydroxide adding amount in two times to be 1: 1;

in step S1, the intermediate 1 is prepared by reacting polyethylene glycol with epichlorohydrin, and the reaction process is as follows:

step S2, adding the prepared intermediate 1 into deionized water, dropwise adding sulfuric acid with the mass fraction of 75%, uniformly stirring and hydrolyzing for 3h, then adding sodium carbonate to adjust the pH of the system to be neutral, carrying out reduced pressure distillation at the temperature of 90 ℃ and the vacuum degree of 0.080MPa, and carrying out suction filtration to obtain an intermediate 2, wherein the use amount of the sulfuric acid is controlled to be 1-5% of the weight of the intermediate 1;

in the step S2, the intermediate 1 undergoes a ring-opening reaction under the catalytic action of an acid to generate an intermediate 2, and the reaction process is as follows:

step S3, adding the prepared intermediate 2 and a catalyst into a reaction kettle, performing vacuum dehydration and replacement with nitrogen for three times, stirring at a constant speed, heating to 120 ℃, adding allyl glycidyl ether, stirring at a constant speed after completely adding, and reacting for 4 hours to prepare an intermediate 3, wherein the weight ratio of the intermediate 2 to the allyl glycidyl ether is controlled to be 0.8: 0.2, and the amount of the catalyst is 1% of the weight of the intermediate 2;

in step S3, the intermediate 2 is mixed with allyl glycidyl ether under the action of a catalyst, and the intermediate 2 reacts with allyl glycidyl ether to generate an intermediate 3, wherein the reaction process is as follows:

step S4, adding the prepared intermediate 3 into a three-neck flask, sequentially adding hydroquinone and p-toluenesulfonic acid, heating to 80 ℃ while stirring, adding tetradecanoic acid, continuously heating to 110 ℃, stirring at a constant speed, reacting for 2 hours, heating to 130 ℃, stirring at a constant speed until the reaction is finished, cooling to 90 ℃, distilling under reduced pressure, purifying to obtain an intermediate 4, and controlling the weight ratio of the intermediate 3 to the hydroquinone to the p-toluenesulfonic acid to the tetradecanoic acid to be 10: 0.1: 0.2: 2.80-2.85;

in step S4, the intermediate 3 is mixed with myristic acid to perform an esterification reaction to generate an intermediate 4, hydroquinone is added as a polymerization inhibitor, p-toluenesulfonic acid is used as a catalyst, and the reaction process is as follows:

step S5, adding low-hydrogen silicone oil into a three-neck flask, adding the prepared intermediate 4 and isopropanol, stirring at a constant speed, heating to 70 ℃, adding chloroplatinic acid, continuing heating to 85 ℃, stirring at a constant speed, reacting for 6 hours, preparing a crude product after the reaction is finished, and distilling under reduced pressure to prepare the defoaming agent, wherein the weight ratio of the low-hydrogen silicone oil to the intermediate 4 is controlled to be 0.5: 1, the dosage of the isopropanol is 30% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4, and the dosage of the chloroplatinic acid is 0.1% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4.

In step S5, low hydrogen silicone oil and intermediate 4 are mixed in isopropanol, chloroplatinic acid is added as a catalyst, and then the mixture is distilled under reduced pressure to obtain a defoaming agent, wherein the reaction process is as follows:

the intermediate 4 is introduced with long-chain alkyl to prepare the defoaming agent, so that the defoaming agent can be endowed with better lubricity, defoaming property and anti-adhesion property.

Further, the catalyst in step S3 is a double metal cyanide complex.

A preparation method of long-life extreme pressure antiwear hydraulic oil comprises the following steps:

heating the base oil to 70 ℃, adding the composite additive, magnetically stirring for 60min, and filtering to obtain the long-life extreme pressure antiwear hydraulic oil.

The invention has the beneficial effects that:

the invention relates to long-life extreme pressure anti-wear hydraulic oil, which forms a ternary composite antioxidant by organic molybdenum, amine antioxidant and ZDDP contained in a complexing agent, has excellent antioxidant performance, and can obtain excellent extreme pressure, anti-wear and antifriction performance, and has extreme pressure anti-wear effect and cost advantage compared with the prior patents under the condition of the same service life, moreover, the preparation method uses a prepared defoaming agent in the preparation of the hydraulic oil, in the preparation process, the intermediate 1 is prepared by the reaction of polyethylene glycol and epoxy chloropropane in the step S1, in the step S2, the intermediate 1 generates an intermediate 2 by the ring-opening reaction under the catalysis of acid, in the step S3, the intermediate 2 is mixed with allyl glycidyl ether under the action of a catalyst, the intermediate 2 reacts with allyl glycidyl ether to generate an intermediate 3, in the step S4, the intermediate 3 is mixed with tetradecanoic acid, and (2) performing esterification reaction to generate an intermediate 4, mixing low-hydrogen silicone oil and the intermediate 4 in isopropanol in step S5, adding chloroplatinic acid as a catalyst, then performing reduced pressure distillation to prepare a defoaming agent, and introducing long-chain alkyl to the intermediate 4 to prepare the defoaming agent, so that the defoaming agent can be endowed with better lubricity, defoaming property and anti-stickiness.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The long-life extreme pressure antiwear hydraulic oil comprises the following raw materials in parts by weight: 97.56 parts of second-class hydrogenated base oil and 1.54 parts of a composite additive;

the preparation method of the long-life extreme pressure anti-wear hydraulic oil comprises the following steps:

heating the second-class hydrogenated base oil to 70 ℃, adding the composite additive, magnetically stirring for 60min, and filtering to obtain the long-life extreme pressure antiwear hydraulic oil.

The composite additive comprises a compound antioxidant, a polymethacrylate pour point depressant, a demulsifier 1001, a defoaming agent prepared by the invention and an anti-wear hydraulic oil complex agent containing ZDDP, and is prepared by the following steps:

adding 0.1 part of compound antioxidant into a three-neck flask, heating to 70 ℃, magnetically stirring for 30min, then sequentially adding 0.1 part of polymethacrylate pour point depressant, 0.8 part of anti-wear hydraulic oil complexing agent containing ZDDP, 0.01 part of condensate of T1001 amine and epoxy compound and 0.01 part of defoaming agent prepared by the method, and uniformly mixing to obtain the composite additive.

The compound antioxidant is prepared by compounding diisooctyl molybdenum dithiophosphate and dioctyldiphenylamine according to the weight ratio of 1: 20.

Example 2

The long-life extreme pressure antiwear hydraulic oil comprises the following raw materials in parts by weight: 98.00 parts of base oil and 2.04 parts of composite additive;

the preparation method of the long-life extreme pressure anti-wear hydraulic oil comprises the following steps:

heating the second-class hydrogenated base oil to 70 ℃, adding the composite additive, magnetically stirring for 60min, and filtering to obtain the long-life extreme pressure antiwear hydraulic oil.

The composite additive comprises a compound antioxidant, a polymethacrylate pour point depressant, a demulsifier 1001, a defoaming agent and an anti-wear hydraulic oil complex agent containing ZDDP, and is prepared by the following steps:

adding 0.15 part of compound antioxidant into a three-neck flask, heating to 70 ℃, magnetically stirring for 35min, then sequentially adding 0.3 part of polymethacrylate pour point depressant, 0.9 part of anti-wear hydraulic oil complexing agent containing ZDDP, 0.05 part of condensate of T1001 amine and epoxy compound and 0.01 part of defoaming agent, and uniformly mixing to obtain the composite additive.

The compound antioxidant is prepared by compounding diisooctyl molybdenum dithiophosphate and dioctyldiphenylamine according to the weight ratio of 1: 20.

Example 3

The long-life extreme pressure antiwear hydraulic oil comprises the following raw materials in parts by weight: 98.46 parts of base oil and 2.44 parts of a composite additive;

the preparation method of the long-life extreme pressure anti-wear hydraulic oil comprises the following steps:

heating the second-class hydrogenated base oil to 70 ℃, adding the composite additive, magnetically stirring for 60min, and filtering to obtain the long-life extreme pressure antiwear hydraulic oil.

The composite additive comprises a compound antioxidant, a polymethacrylate pour point depressant, a demulsifier 1001, a defoaming agent and an anti-wear hydraulic oil complex agent containing ZDDP, and is prepared by the following steps:

adding 0.25 part of compound antioxidant into a three-neck flask, heating to 70 ℃, magnetically stirring for 40min, then sequentially adding 0.5 part of polymethacrylate pour point depressant, 1 part of anti-wear hydraulic oil complexing agent containing ZDDP, 0.1 part of condensate of T1001 amine and epoxy compound and 0.01 part of defoaming agent, and uniformly mixing to obtain the composite additive.

The compound antioxidant is prepared by compounding diisooctyl molybdenum dithiophosphate and dioctyldiphenylamine according to the weight ratio of 1: 20.

Table 1 shows the comparison of the oil products of examples 1 to 3 of the present invention with 46-specification antiwear hydraulic oil of GB 11118.1-94.

TABLE 1

Example 4

The defoaming agent comprises the following steps:

step S1, sequentially adding polyethylene glycol, tetra-n-butyl ammonium bromide and sodium hydroxide into a three-neck flask, heating in a water bath at 35 ℃, dropwise adding epoxy chloropropane, heating to 55 ℃ after completely adding the epoxy chloropropane, then adding a sodium hydroxide aqueous solution with the mass fraction of 10%, stirring at a constant speed and reacting for 2 hours, cooling, performing suction filtration, adjusting the pH value to be neutral, performing reduced pressure distillation to prepare an intermediate 1, controlling the molar ratio of the total amount of the polyethylene glycol, the tetra-n-butyl ammonium bromide and the sodium hydroxide to the epoxy chloropropane to be 1: 0.02: 3: 2.5, and controlling the molar ratio of the sodium hydroxide adding amount of two times to be 1: 1;

step S2, adding the prepared intermediate 1 into deionized water, dropwise adding sulfuric acid with the mass fraction of 75%, uniformly stirring and hydrolyzing for 3h, then adding sodium carbonate to adjust the pH of the system to be neutral, carrying out reduced pressure distillation at the temperature of 90 ℃ and the vacuum degree of 0.080MPa, and carrying out suction filtration to obtain an intermediate 2, wherein the use amount of the sulfuric acid is controlled to be 1% of the weight of the intermediate 1;

step S3, adding the prepared intermediate 2 and cobalt-zinc double metal cyanide complex into a reaction kettle, performing vacuum dehydration, replacing with nitrogen for three times, stirring at a constant speed, heating to 120 ℃, adding allyl glycidyl ether, stirring at a constant speed after completely adding, and reacting for 4 hours to prepare an intermediate 3, wherein the weight ratio of the intermediate 2 to the allyl glycidyl ether is controlled to be 0.8: 0.2, and the dosage of the cobalt-zinc double metal cyanide complex is 1% of the weight of the intermediate 2;

step S4, adding the prepared intermediate 3 into a three-neck flask, sequentially adding hydroquinone and p-toluenesulfonic acid, heating to 80 ℃ while stirring, adding tetradecanoic acid, continuously heating to 110 ℃, stirring at a constant speed, reacting for 2 hours, heating to 130 ℃, stirring at a constant speed until the reaction is finished, cooling to 90 ℃, distilling under reduced pressure, purifying to obtain an intermediate 4, and controlling the weight ratio of the intermediate 3 to the hydroquinone to the p-toluenesulfonic acid to the tetradecanoic acid to be 10: 0.1: 0.2: 2.80;

step S5, adding low-hydrogen silicone oil into a three-neck flask, adding the prepared intermediate 4 and isopropanol, stirring at a constant speed, heating to 70 ℃, adding chloroplatinic acid, continuing heating to 85 ℃, stirring at a constant speed, reacting for 6 hours, preparing a crude product after the reaction is finished, and distilling under reduced pressure to prepare the defoaming agent, wherein the weight ratio of the low-hydrogen silicone oil to the intermediate 4 is controlled to be 0.5: 1, the dosage of the isopropanol is 30% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4, and the dosage of the chloroplatinic acid is 0.1% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4.

Example 5

The defoaming agent comprises the following steps:

step S1, sequentially adding polyethylene glycol, tetra-n-butyl ammonium bromide and sodium hydroxide into a three-neck flask, heating in a water bath at 35 ℃, dropwise adding epoxy chloropropane, heating to 55 ℃ after completely adding the epoxy chloropropane, then adding a sodium hydroxide aqueous solution with the mass fraction of 10%, stirring at a constant speed and reacting for 2 hours, cooling, performing suction filtration, adjusting the pH value to be neutral, performing reduced pressure distillation to prepare an intermediate 1, controlling the molar ratio of the total amount of the polyethylene glycol, the tetra-n-butyl ammonium bromide and the sodium hydroxide to the epoxy chloropropane to be 1: 0.02: 3: 2.5, and controlling the molar ratio of the sodium hydroxide adding amount of two times to be 1: 1;

step S2, adding the prepared intermediate 1 into deionized water, dropwise adding sulfuric acid with the mass fraction of 75%, uniformly stirring and hydrolyzing for 3h, then adding sodium carbonate to adjust the pH of the system to be neutral, carrying out reduced pressure distillation at the temperature of 90 ℃ and the vacuum degree of 0.080MPa, and carrying out suction filtration to obtain an intermediate 2, wherein the use amount of the sulfuric acid is controlled to be 3% of the weight of the intermediate 1;

step S3, adding the prepared intermediate 2 and cobalt-zinc double metal cyanide complex into a reaction kettle, performing vacuum dehydration, replacing with nitrogen for three times, stirring at a constant speed, heating to 120 ℃, adding allyl glycidyl ether, stirring at a constant speed after completely adding, and reacting for 4 hours to prepare an intermediate 3, wherein the weight ratio of the intermediate 2 to the allyl glycidyl ether is controlled to be 0.8: 0.2, and the dosage of the cobalt-zinc double metal cyanide complex is 1% of the weight of the intermediate 2;

step S4, adding the prepared intermediate 3 into a three-neck flask, sequentially adding hydroquinone and p-toluenesulfonic acid, heating to 80 ℃ while stirring, adding tetradecanoic acid, continuously heating to 110 ℃, stirring at a constant speed, reacting for 2 hours, heating to 130 ℃, stirring at a constant speed until the reaction is finished, cooling to 90 ℃, distilling under reduced pressure, purifying to obtain an intermediate 4, and controlling the weight ratio of the intermediate 3 to the hydroquinone to the p-toluenesulfonic acid to the tetradecanoic acid to be 10: 0.1: 0.2: 2.83;

step S5, adding low-hydrogen silicone oil into a three-neck flask, adding the prepared intermediate 4 and isopropanol, stirring at a constant speed, heating to 70 ℃, adding chloroplatinic acid, continuing heating to 85 ℃, stirring at a constant speed, reacting for 6 hours, preparing a crude product after the reaction is finished, and distilling under reduced pressure to prepare the defoaming agent, wherein the weight ratio of the low-hydrogen silicone oil to the intermediate 4 is controlled to be 0.5: 1, the dosage of the isopropanol is 30% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4, and the dosage of the chloroplatinic acid is 0.1% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4.

Example 6

The defoaming agent comprises the following steps:

step S1, sequentially adding polyethylene glycol, tetra-n-butyl ammonium bromide and sodium hydroxide into a three-neck flask, heating in a water bath at 40 ℃, dropwise adding epoxy chloropropane, heating to 55 ℃ after completely adding the epoxy chloropropane, then adding a sodium hydroxide aqueous solution with the mass fraction of 10%, stirring at a constant speed and reacting for 2 hours, cooling, performing suction filtration, adjusting the pH value to be neutral, performing reduced pressure distillation to prepare an intermediate 1, controlling the molar ratio of the total amount of the polyethylene glycol, the tetra-n-butyl ammonium bromide and the sodium hydroxide to the epoxy chloropropane to be 1: 0.02: 3: 2.5, and controlling the molar ratio of the sodium hydroxide adding amount of two times to be 1: 1;

step S2, adding the prepared intermediate 1 into deionized water, dropwise adding sulfuric acid with the mass fraction of 75%, uniformly stirring and hydrolyzing for 3h, then adding sodium carbonate to adjust the pH of the system to be neutral, carrying out reduced pressure distillation at the temperature of 90 ℃ and the vacuum degree of 0.080MPa, and carrying out suction filtration to obtain an intermediate 2, wherein the use amount of the sulfuric acid is controlled to be 1-5% of the weight of the intermediate 1;

step S3, adding the prepared intermediate 2 and cobalt-zinc double metal cyanide complex into a reaction kettle, performing vacuum dehydration, replacing with nitrogen for three times, stirring at a constant speed, heating to 120 ℃, adding allyl glycidyl ether, stirring at a constant speed after completely adding, and reacting for 4 hours to prepare an intermediate 3, wherein the weight ratio of the intermediate 2 to the allyl glycidyl ether is controlled to be 0.8: 0.2, and the dosage of the cobalt-zinc double metal cyanide complex is 1% of the weight of the intermediate 2;

step S4, adding the prepared intermediate 3 into a three-neck flask, sequentially adding hydroquinone and p-toluenesulfonic acid, heating to 80 ℃ while stirring, adding tetradecanoic acid, continuously heating to 110 ℃, stirring at a constant speed, reacting for 2 hours, heating to 130 ℃, stirring at a constant speed until the reaction is finished, cooling to 90 ℃, distilling under reduced pressure, purifying to obtain an intermediate 4, and controlling the weight ratio of the intermediate 3 to the hydroquinone to the p-toluenesulfonic acid to the tetradecanoic acid to be 10: 0.1: 0.2: 2.85;

step S5, adding low-hydrogen silicone oil into a three-neck flask, adding the prepared intermediate 4 and isopropanol, stirring at a constant speed, heating to 70 ℃, adding chloroplatinic acid, continuing heating to 85 ℃, stirring at a constant speed, reacting for 6 hours, preparing a crude product after the reaction is finished, and distilling under reduced pressure to prepare the defoaming agent, wherein the weight ratio of the low-hydrogen silicone oil to the intermediate 4 is controlled to be 0.5: 1, the dosage of the isopropanol is 30% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4, and the dosage of the chloroplatinic acid is 0.1% of the sum of the weight of the low-hydrogen silicone oil and the intermediate 4.

A comparative experiment was conducted on the defoaming agents prepared in examples 4 to 6 and a commercially available silicone defoaming agent, 50mL of a foaming solution (0.5% foaming solution prepared from sodium dodecylbenzenesulfonate and TX10 in a ratio of 1: 1) was added to a 100mL measuring cylinder, 0.2g of the defoaming agent was added dropwise, the mixture was shaken under 30 ℃ and the foam decay time was observed while standing, and a test was conducted on a comparative sample and the time was recorded.

Therefore, the defoaming agent prepared by the method has more excellent defoaming performance for the commercial silicone defoaming agent.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.