CN103484205B - Thermoplastic-elastomer-containing complex aluminum-based lubricating grease composition and preparation method thereof - Google Patents

Abstract

The invention provides a thermoplastic-elastomer-containing complex aluminum-based lubricating grease composition and a preparation method thereof. The lubricating grease composition is prepared from the following components in parts by mass: 1-5 parts of thermoplastic elastomer, 5-15 parts of complex aluminum thickener and 80-94 parts of base oil. The preparation method comprises the following steps: adding benzoic acid and stearic acid into 80% of base oil, and uniformly stirring; when the oil temperature is 90-100 DEG C, adding aluminum isopropoxide tripolymer to carry out saponification until isopropanol in the material is completely released; adding a thermoplastic elastomer, and heating to 110-120 DEG C while stirring until the thermoplastic elastomer is completely dissolved; continuing heating the product to 190-220 DEG C, and adding the rest of base oil. The thermoplastic-elastomer-containing complex aluminum-based lubricating grease enhances the adhesiveness to metals, enhances the high-temperature colloid stability and reduces the high-temperature loss under the condition of no additive, and is suitable for use under high-temperature severe conditions.

Description

A kind of composite aluminum base grease composition and preparation method containing thermoplastic elastomer

Technical field

The present invention relates to a kind of lubricant, is specifically a kind of composite aluminum base grease composition and preparation method of containing thermoplastic elastomer.

Background technology

Along with the fast development of the industries such as metallurgy, mine, cement, the high temperature service of maximization also gets more and more, and therefore requires more and more higher to the hot properties of lubricating grease.The lubricating grease kind that can be used for worst hot case is a lot, comprise polyurea grease, grease of calcium sulfonic acid, complex lithium grease, composite aluminum base grease etc., but general employing of high temperature service lubrication is concentrated for fat system, therefore requires very high to the pumping of lubricating grease.In pumping, composite aluminum base grease has absolute leading superiority than other several lubricating grease.Composite aluminum base grease is as the high temperature grease of generally acknowledging, there is higher dropping point and high-temperature and reversible, there is outstanding pumping and water resisting property simultaneously, very strong thickening ability can be shown to different types of base oil, use under being very suitable for high temperature and wet condition, be therefore subject to the favor of steel industry.Especially the appearance of Extreme pressure Al Matrix Grease, shows high application prospect at the high temperature heavy load such as iron and steel, cement industry field, makes composite aluminum base grease obtain vigorous growth.

Compound aluminium soap is reacted also multiviscosisty base oil formed by aluminum isopropylate (or tripolymer), phenylformic acid, stearic acid, and production technique is simple, constant product quality.Reaction mechanism is: the aluminum isopropylate of a part contains the Virahol of three molecules, two molecule Virahols are wherein replaced generation bisgallic acid aluminium soap by the lipid acid of the phenylformic acid of a part and a part, remaining a part Virahol generates hydroxyl with the water reaction of a part again, finally generate alkali formula bisgallic acid aluminium soap, altogether discharge the Virahol of three molecules.Due to a large amount of Virahol gas will be discharged in reaction process, larger harm can be brought to environment, therefore generally all adopt aluminum isopropylate tripolymer to replace aluminum isopropylate as raw material abroad.Adopt the Virahol much less that aluminum isopropylate tripolymer discharges, and oil soluble is better than aluminum isopropylate, production process does not need aquation, and production technique controllability is strong, and quality product is better.But the trimerical price of aluminum isopropylate is higher, preparation technology's relative complex, does not therefore substitute aluminum isopropylate at home completely.

Composite aluminum base grease has less soap fibrous texture, relies on hydrogen bond, coordinate bond, Van der Waals force equimolecular intermolecular forces to make soap fiber form stable pearl string model.Compound aluminium soap has very strong adsorptive power to base oil, and thickening ability is very strong.The thinning deliquescing of meeting under high temperature and External Force Acting, but lower the temperature and grease structure can be recovered rapidly after removing external force, and therefore thixotropy is excellent, and high-temperature and reversible is given prominence to.

But, composite aluminum base grease also has some not too gratifying places.It is general to the adhesivity of metal, has certain leakage problem in actual use.Simultaneously at high temperature compound aluminium soap can thinning deliquescing, colloidal structure stability declines, and can greatly reduce the adsorptive power of base oil, high temperature at this moment can be caused under external force to run off very serious, which also limits composite aluminum base grease to use under the operating mode of some harshnesses, need to improve.

Thermoplastic elastomer, also known as synthetic chloroprene rubber, both the snappiness of traditional cross-linking vulcanized rubber, ageing-resistant, the every excellent properties of oil-proofness had been possessed, possesses again common plastics feature easy to process, repeatedly used, that there is hommization and high-grade novel synthetic material, also be globalization standard environment-friendly materials, be described as " third generation synthetic rubber ".Thermoplastic elastomer is made up of the molecular chain of the identical different chain length of structural unit, be divided into line style, star-like and build three types, formation polymer gel can be dissolved in all kinds of base oil, to various metal, all there is very strong adhesive capacity, and this gel and base oil have very strong Intermolecular Forces, even if at high temperature also stably base oil can be adsorbed, play and suppress a point effect for oil.Simultaneously thermoplastic elastomer can not decomposes at high temperature, has fine stability, can be widely used as high-temperature oil separating inhibitor and deflocculant.

Summary of the invention

The object of this invention is to provide a kind of the composite aluminum base grease composition and the preparation method that contain thermoplastic elastomer; Composite aluminum base grease containing thermoplastic elastomer, except the good pumping that this lubricating grease has except common composite aluminum base grease and water resisting property, improve the adhesivity stronger to metal, and at high temperature also good stability, not easily run off.

Technical scheme of the present invention is as follows:

Containing the composite aluminum base grease composition of thermoplastic elastomer, its component and ratio of quality and the number of copies as follows:

Thermoplastic elastomer: 1 ~ 5 part;

Clad aluminum viscosifying agent: 5 ~ 15 parts;

Base oil: 80 ~ 94 parts.

Described thermoplastic elastomer is styrene block copolymer.

Described thermoplastic elastomer is lubrizol7306.

Described clad aluminum viscosifying agent reacts preparation by stearic acid, phenylformic acid and aluminum isopropylate tripolymer.

The mol ratio of the reactant of described clad aluminum viscosifying agent is 1:1:2.

Described stearic acid is the organic acid that oil soluble is slightly good.

Described phenylformic acid is the slightly poor organic acid of oil soluble.

The trimerical purity of described aluminum isopropylate is 70%.

Described base oil, refers to mineral oil and PAO synthetic oil, and the kinematic viscosity of 100 DEG C is 6-45mm ²/ s.

The kinematic viscosity of described 100 DEG C is 18-25mm ²/ s.

The preparation method of grease composition of the present invention, comprises the following steps:

1) saponification: add phenylformic acid, stearic acid in base oil, uniform stirring, the consumption of base oil is 80%, adds aluminum isopropylate tripolymer carry out saponification reaction when oil liquid temperature is 90-100 DEG C, until the Virahol in material is released completely;

2) dissolve: in step 1) product in add thermoplastic elastomer, heated and stirred, when 110-120 DEG C till thermoplastic elastomer dissolves completely;

3) become fat: by step 2) product continue to be warmed up to 190-220 DEG C, add remaining base oil.

Described preparation process does not add additive.

The composite aluminum base grease containing thermoplastic elastomer that the present invention prepares, when not containing additive, improves the adhesivity to metal, improves high temperature colloidal stability, decreases high temperature and runs off, use under being adapted at high temperature exacting terms.

Embodiment

Embodiment 1:

Add 150BS(ν in the reactor ₁₀₀=34.17) 500g and 500SN(ν ₁₀₀=12.18) 520g, add phenylformic acid 15g, stearic acid 35g mixing and stirring, temperature of reaction adds aluminum isopropylate tripolymer 18g(purity 70% when being 90-92 DEG C) react 60 minutes afterwards, add thermoplastic elastomer lubrizol 7306 14g, when being warmed up to 110-112 DEG C, constant temperature stirs 60 minutes, continue to be warmed up to 218-220 DEG C, constant temperature 10 minutes, adds 500SN(ν ₁₀₀=12.18) be down to room temperature after 255g, finally grind to form fat with three-roller.Performance is in table 1

Embodiment 2:

Add 500SN(ν in the reactor ₁₀₀=11.18) 650g and 150BS(ν ₁₀₀=33.92) 415g, add phenylformic acid 16g, stearic acid 37g mixing and stirring, temperature of reaction adds aluminum isopropylate tripolymer 19g(purity 70% when being 94-96 DEG C) react 60 minutes afterwards, add thermoplastic elastomer lubrizol 7306 43g, when being warmed up to 118-120 DEG C, constant temperature stirs 60 minutes, continue to be warmed up to 200-202 DEG C, constant temperature 10 minutes, adds 150BS(ν ₁₀₀=33.92) be down to room temperature after 266g, finally grind to form fat with three-roller.Performance is in table 1

Embodiment 3:

Add 150BS(ν in the reactor ₁₀₀=35.21) 450g and 500SN(ν ₁₀₀=10.88) 462g, add phenylformic acid 14g, stearic acid 33g mixing and stirring, temperature of reaction adds aluminum isopropylate tripolymer 17g(purity 70% when being 98-100 DEG C) react 60 minutes afterwards, add thermoplastic elastomer lubrizol 7306 63g, when being warmed up to 114-116 DEG C, constant temperature stirs 60 minutes, continue to be warmed up to 190-192 DEG C, constant temperature 10 minutes, adds 500SN(ν ₁₀₀=10.88) be down to room temperature after 228g, finally grind to form fat with three-roller.Performance is in table 1

Embodiment 4:

Add 150BS(ν in the reactor ₁₀₀=33.95) 350g and 500SN(ν ₁₀₀=11.34) 422g, add phenylformic acid 40g, stearic acid 93g mixing and stirring, temperature of reaction adds aluminum isopropylate tripolymer 48g(purity 70% when being 97-99 DEG C) react 60 minutes afterwards, add thermoplastic elastomer lubrizol 7306 60g, when being warmed up to 116-118 DEG C, constant temperature stirs 60 minutes, continue to be warmed up to 193-195 DEG C, constant temperature 10 minutes, adds 500SN(ν ₁₀₀=11.34) be down to room temperature after 193g, finally grind to form fat with three-roller.Performance is in table 1

Embodiment 5:

Add PAO40(ν in the reactor ₁₀₀=39.65) 500g and PAO10(ν ₁₀₀=9.54) 450g, add phenylformic acid 22g, stearic acid 51g mixing and stirring, when temperature of reaction is 93-95 DEG C, add aluminum isopropylate tripolymer 26g(purity 70%) react 70 minutes afterwards, add thermoplastic elastomer lubrizol 7306 40g, be warmed up to 115-117 DEG C of constant temperature and stir 60 minutes, continue to be warmed up to 205-207 DEG C, constant temperature 10 minutes, adds PAO10(ν ₁₀₀=9.54) be down to room temperature after 237g, finally grind to form fat with three-roller.Performance is in table 1

Embodiment 6:

Add 150BS(ν in the reactor ₁₀₀=37.78) 513g and 500SN(ν ₁₀₀=10.34) 700g, add phenylformic acid 32g, stearic acid 75g mixing and stirring, when temperature of reaction is 91-93 DEG C, add aluminum isopropylate tripolymer 38g(purity 70%) react 60 minutes afterwards, add thermoplastic elastomer lubrizol 7306 19g, be warmed up to 110-120 DEG C of constant temperature and stir 60 minutes, continue to be warmed up to 207-209 DEG C, constant temperature 10 minutes, adds 150BS(ν ₁₀₀=37.78) be down to room temperature after 170g, finally grind to form fat with three-roller.Performance is in table 1

Comparative example 1:

Add 150BS(ν in the reactor ₁₀₀=34.35) 450g and 500SN(ν ₁₀₀=12.07) 442g, add phenylformic acid 20g, stearic acid 47g mixing and stirring, when temperature of reaction is 93-95 DEG C, add aluminum isopropylate tripolymer 24g(purity 70%) react 60 minutes afterwards, be warmed up to 114-116 DEG C of constant temperature afterwards and stir 60 minutes, continue to be warmed up to 203-205 DEG C, constant temperature 10 minutes, adds 150BS(ν ₁₀₀=34.35) be down to room temperature after 223g, finally grind to form fat with three-roller.Performance is in table 1

Comparative example 2:

Add PAO40(ν in the reactor ₁₀₀=40.21) 750g and PAO10(ν ₁₀₀=10.11) 454g, add phenylformic acid 27g, stearic acid 63g mixing and stirring, when temperature of reaction is 98-100 DEG C, add aluminum isopropylate tripolymer 32g(purity 70%) react 60 minutes afterwards, be warmed up to 110-120 DEG C of constant temperature afterwards and stir 60 minutes, continue to be warmed up to 202-204 DEG C, constant temperature 10 minutes, adds PAO10(ν ₁₀₀=10.11) be down to room temperature after 301g, finally grind to form fat with three-roller.Performance is in table 1

The performance comparison of table 1 lubricating grease

As shown in table 1, comparison example 7 and contrast 1, example 6 and contrast 2, base oil and soap divide all identical, and the thermoplastic elastomer adding 1% just can obviously increase lubricating grease viscosity, reduce high temperature Stencil oil-dividing; Comparison example 1, example 2 and example 3, soap divides identical, increases the content of thermoplastic elastomer gradually, and high temperature Stencil oil-dividing reduces gradually, and viscosity increases gradually; Comparison example 1, example 4 and example 7, thermoplastic elastomer content is identical, but soap divides difference, and high temperature Stencil oil-dividing difference is little, and viscosity differences is also little, illustrates to be thermoplastic elastomer to high temperature Stencil oil-dividing and viscosity plays Main Function.

Sum up above learning, the composite aluminum base grease composition containing thermoplastic elastomer provided by the invention can improve the high-temperature oil separating of clad aluminum really, reduces and runs off, and increases system viscosity simultaneously thus strengthens the adhesivity to metal.

Claims (5)

1. containing the composite aluminum base grease composition of thermoplastic elastomer, its component and ratio of quality and the number of copies as follows:

Thermoplastic elastomer: 1 ~ 5 part;

Clad aluminum viscosifying agent: 5 ~ 15 parts;

Base oil: 80 ~ 94 parts;

Described thermoplastic elastomer is styrene block copolymer; Described clad aluminum viscosifying agent reacts preparation by phenylformic acid, stearic acid and aluminum isopropylate tripolymer; The trimerical mol ratio of phenylformic acid, stearic acid and aluminum isopropylate is 1:1:2; Described base oil, refers to mineral oil and PAO synthetic oil, and the kinematic viscosity of 100 DEG C is 6-45mm ²/ s.

2. grease composition as claimed in claim 1, is characterized in that the trimerical purity of described aluminum isopropylate is 70%.

3. grease composition as claimed in claim 1, is characterized in that the kinematic viscosity of described 100 DEG C is 18-25mm ²/ s.

4. the preparation method of grease composition as claimed in claim 1, is characterized in that comprising the following steps:

1) saponification: add phenylformic acid, stearic acid in base oil, uniform stirring, the consumption of base oil is 80%, adds aluminum isopropylate tripolymer carry out saponification reaction when oil liquid temperature is 90-100 DEG C, until the Virahol in material is released completely;

2) dissolve: in step 1) product in add thermoplastic elastomer, heated and stirred, when 110-120 DEG C till thermoplastic elastomer dissolves completely;

3) become fat: by step 2) product continue to be warmed up to 190-220 DEG C, add remaining base oil.

5. as described in claim 4 preparation method, is characterized in that described by step 2) product continue to be warmed up to 195-210 DEG C, add remaining base oil.