CN114561237B - Preparation method of shear-responsive water-based gel lubricant - Google Patents

Preparation method of shear-responsive water-based gel lubricant Download PDF

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CN114561237B
CN114561237B CN202210407670.XA CN202210407670A CN114561237B CN 114561237 B CN114561237 B CN 114561237B CN 202210407670 A CN202210407670 A CN 202210407670A CN 114561237 B CN114561237 B CN 114561237B
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water
shear
friction
based gel
gel lubricant
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CN114561237A (en
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胡丽天
曹文辉
丁奇
秦宝锋
张松伟
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M149/00—Lubricating compositions characterised by the additive being a macromolecular compound containing nitrogen
    • C10M149/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M149/06—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amido or imido group
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52—Amides or imides
    • C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/56—Acrylamide; Methacrylamide
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
    • C10M2209/084—Acrylate; Methacrylate
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/024—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amido or imido group
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/56—Boundary lubrication or thin film lubrication
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/68—Shear stability
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Lubricants (AREA)

Abstract

本发明公开了一种剪切响应性水基凝胶润滑剂的制备方法，是将丙烯酰胺、丙烯酸溶解于水中，加热搅拌至溶液澄清透明；向体系中通入高纯氮气并升温至70℃~75℃，加入交联剂MBA搅拌反应一段时间后，再加入引发剂APS聚合6~8h，得到该剪切响应性水基凝胶润滑剂溶液。该水基凝胶润滑剂初始为液态，容易注入摩擦界面；具有快速剪切响应特性，在摩擦过程中迅速增稠，在摩擦界面上形成润滑膜，具有优异的粘附能力。用于摩擦配副时，不但能降低摩擦系数，而且能极大缓解摩擦界面的粘着磨损。另外，该剪切响应水基凝胶润滑剂对于不同摩擦速度具有响应性，表现为在不同剪切速度下有着不同的摩擦系数，因此具有一定工况自适应特性。The invention discloses a preparation method of a shear-responsive water-based gel lubricant. The acrylamide and acrylic acid are dissolved in water, heated and stirred until the solution is clear and transparent; high-purity nitrogen gas is introduced into the system and the temperature is raised to 70° C. At ~75°C, after adding the cross-linking agent MBA and stirring for a period of time, then adding the initiator APS to polymerize for 6-8 h to obtain the shear-responsive water-based gel lubricant solution. The water-based gel lubricant is initially liquid and can be easily injected into the friction interface; it has fast shear response characteristics, rapidly thickens during friction, forms a lubricating film on the friction interface, and has excellent adhesion ability. When used in friction matching pairs, it can not only reduce the friction coefficient, but also greatly alleviate the adhesive wear of the friction interface. In addition, the shear-responsive water-based gel lubricant is responsive to different friction speeds, showing that it has different friction coefficients under different shear speeds, so it has certain working condition adaptive characteristics.

Description

Preparation method of shear-responsive water-based gel lubricant
Technical Field
The invention relates to a preparation method of a water-based gel lubricant, in particular to a preparation method of a shear-responsive water-based gel lubricant, which is mainly used for lubricating a steel and silicon nitride friction pair and belongs to the fields of high polymer materials and lubricating technology.
Technical Field
The water lubrication has the characteristics of no pollution, good cooling performance, high safety and the like, and is widely applied to the fields of mechanical lubrication, cutting and the like. But the application range is limited due to the defects of low viscosity of water, easy loss in the lubricating process, poor actual lubricating effect compared with oil lubricating and the like. In order to improve the water lubrication performance, a plurality of water-soluble nano particles are introduced into the water lubrication to reduce the friction and the abrasion of a friction pair. In recent years, soft substances (polymer brushes and hydrogels) are widely researched, particularly, a hydrophilic three-dimensional network structure material such as a hydrogel has good biocompatibility, and a chemical network structure of the hydrogel has high designability, so that various responsive molecules can be introduced into a hydrogel network, and the hydrogel can respond to different environmental stimuli by changing the external environment to achieve the conversion of molecular conformation in a gel system. At present, the research is widely carried out on temperature, pH, light, electricity and other responsive hydrogels, and the hydrogel is widely applied to the fields of drug release, artificial muscle and the like.
With the proposal of the concept of lubrication adaptation in the field of tribology, researches on the application of responsive gel in the field of tribology are gradually paid attention, but the mechanical strength of hydrogel is generally weak, and the hydrogel is difficult to adapt to continuous shearing in the friction process. Chinese patent CN109825269A discloses application of a shear-responsive gel plugging agent in the field of drilling fluid plugging, but the shear-responsive gel with shear thinning and standing thickening characteristics is finally obtained by the scheme; chinese patent CN114058029A discloses a vibration gelling technology, the prepared hydrogel stock solution can be gelled after slight vibration, which is not suitable for the self-adaptive scene of the working condition that the required friction initial lubricant is easy to inject and the shearing gelling is existed in the friction process. Therefore, at present, no water lubrication technical scheme with shear-forming glue and shear-thickening regulation and control performance exists for the water lubrication friction pair.
Disclosure of Invention
The invention aims to provide a preparation method of a high-molecular water-based gel lubricant with shear response, aiming at the problems that the water lubricating film forming capability of a friction interface is insufficient and adhesive wear is easy to occur in the existing water lubricating technology.
The invention discloses a preparation method of a shear-responsive water-based gel lubricant, which comprises the steps of dissolving Acrylamide (AM) and Acrylic Acid (AA) in water, heating to 50 to 55 ℃, and stirring until a solution is clear and transparent; introducing high-purity nitrogen into the system to remove oxygen dissolved in water, heating the reaction system to 70-75 ℃, adding a crosslinking agent N, N-Methylenebisacrylamide (MBA) into the reaction system, stirring for 8-15min, adding an initiator Ammonium Persulfate (APS) into the reaction system, stirring and polymerizing for 6-8h, and cooling to room temperature to obtain the shear-responsive water-based gel lubricant solution.
The molar ratio of Acrylamide (AM) to Acrylic Acid (AA) is 3.5 to 1 to 4.5; acrylamide (AM) and Acrylic Acid (AA) are dissolved in water according to the mass percent of 1 to 1.5 percent.
The molar ratio of Acrylamide (AM) to N, N-Methylenebisacrylamide (MBA) is 40.
2. Structure and performance of water-based lubricants
1. Morphology of Water-based Lubricants
Fig. 1 is a picture of the appearance of a water-based gel lubricant prepared according to the present invention. Therefore, the water-based lubricant prepared by the invention is colorless liquid, and is dispersed uniformly and stably for a long time. The initial liquid state enables the lubricant to be more easily injected into the friction interface.
FIG. 2 is a scanning electron micrograph of a water-based gel lubricant prepared according to the present invention after lyophilization. It can be seen that the freeze-dried sample appears fibrous, and this structure enables the molecular chains to be oriented in the shear direction during shearing, giving them shear-responsiveness.
FIG. 3 is an infrared spectrum of a water-based gel lubricant prepared in accordance with the present invention. It can be seen that AA and AM participate in the polymerization reaction to give a copolymer.
2. Shear response characteristic
The shear response of the water-based gel lubricant was studied using an antopa MCR 302 rheometer with the test conditions: PP25 plate measurement system, slit width 1mm, rotation mode, fixed shear frequency, measurement temperature 25 ℃.
FIG. 4 shows that the water-based gel lubricant prepared by the present invention is at 0.5s -1 Response characteristics at low shear rate. As can be seen from FIG. 4, the water-based gel lubricant was used at 0.5s -1 At a constant shear rate, the viscosity increased with increasing shear time and became gel-like after shearing for 60 s. The macroscopic state of the water-based gel lubricant after shearing is shown in fig. 5 and is gel-like.
FIG. 6 shows the water-based gel lubricant at 100s -1 Response at shear rate. The viscosity graph 6 shows that the water-based gel lubricant prepared by the invention still has the special property of shear thickening and gelling under high-speed shearing.
3. Tribological properties
The HT-1000 high-temperature reciprocating friction and wear testing machine is adopted, and the specific experimental conditions are as follows: load 10N, different frequency, upper sample is 304 stainless steel ball or Si with diameter 6mm 3 N 4 And (3) ceramic balls. The lower samples were 304 stainless steel blocks and Si, respectively 3 N 4 A ceramic block. The duration of the test was 30min.
FIG. 7 is a graph of the coefficient of friction under water lubrication conditions, and FIG. 7 (a) shows a stainless steel-stainless steel friction pair with an average coefficient of friction of about 0.32; wherein FIG. 7 (b) is represented by Si 3 N 4 -Si 3 N 4 The average coefficient of friction is about 0.45 for a friction pair.
FIG. 8 is a plot of coefficient of friction curves under lubricated conditions for a sample of water-based lubricant prepared in accordance with the present invention (example 1), expressed as Si 3 N 4 -Si 3 N 4 Is a friction pair, has an average friction coefficient of about 0.188 at a frequency of 4Hz, and is lubricated with pure water 3 N 4 The friction coefficient is reduced by about 60% compared to the friction pair. And the rubbed sample is adsorbed on the surface of the friction pair in a gel state, and the reciprocating shearing can also thicken and gel the material.
FIG. 9 is a plot of coefficient of friction at different frequencies for water-based lubricant lubricated samples prepared according to the present invention (example 2). 304-304 stainless steel is used as a friction pair. Has a fast frequency response characteristic. Fig. 9 shows that stainless steel-stainless steel is used as the friction pair, the average friction coefficient at 4Hz frequency is as low as 0.262, and the friction coefficient is reduced by about 20% compared with the friction pair of 304 stainless steel lubricated by pure water. The rubbed sample also exhibited gel-like adsorption on the surface of the rubbing pair.
The results of fig. 8 and 9 show that the water-based gel lubricant has response characteristics to different friction pairs, and the friction coefficient gradually decreases with increasing reciprocating frequency, indicating that the higher the shear frequency, the faster the molecules of the water-based gel lubricant cross-link and the easier the water-based gel lubricant becomes to gel.
In conclusion, the shear response water-based gel lubricant disclosed by the invention is constructed based on self-assembly of a polymer chain, and effectively solves the problems of insufficient film forming capability and easiness in adhesive wear in the water lubricating process; the water-based gel lubricant has low initial viscosity and is easy to inject into a friction interface; the high-viscosity polyurethane rubber has a quick shear response characteristic, can be thickened quickly in a friction process, forms a lubricating film on a friction interface, and has excellent adhesion capability. When the gel material is used for a friction matching pair, the friction coefficient can be reduced, the adhesive wear of a friction interface can be greatly relieved, the film formation of the shear response gel material on the friction interface is mainly benefited, the direct contact of a friction couple is avoided, and the better tribological performance is realized. In addition, the shear response water-based gel lubricant has different friction coefficients under different frequencies, so that the shear response water-based gel lubricant has certain working condition adaptability. And is responsive to different frictional speeds.
Drawings
Fig. 1 is a macroscopic picture of a water-based gel lubricant prepared according to the present invention.
FIG. 2 is a scanning electron micrograph of a water-based gel lubricant prepared according to the present invention after freeze-drying.
FIG. 3 is an infrared spectrum of a water-based gel lubricant gel prepared according to the present invention.
FIG. 4 shows that the water-based gel lubricant prepared by the present invention is at 0.5s -1 Response characteristics at shear rate.
Fig. 5 is a macroscopic view of a water-based gel lubricant prepared according to the present invention after shearing.
FIG. 6 shows the water-based gel lubricant prepared by the present invention in 100s -1 Response characteristics at shear rate.
FIG. 7 is a plot of coefficient of friction for a friction pair under water lubrication conditions.
FIG. 8 is a plot of coefficient of friction (Si) for water-based lubricant lubricants prepared in accordance with the present invention at various frequencies 3 N 4 -Si 3 N 4 As a friction pair).
FIG. 9 is a graph of coefficient of friction curves for water-based lubricants prepared in accordance with the present invention lubricated at different frequencies (304-304 stainless steel is the friction pair).
Detailed Description
The preparation and application properties of the shear-responsive water-based gel lubricant of the present invention are further illustrated by the following specific examples.
Example 1
Putting 23.10mmol AM and 5.83mmol AA into a three-neck flask, adding 130mL distilled water, and magnetically stirring at 50 ℃ until the solution is clear and transparent; introducing high-purity nitrogen into the system for 20min to remove oxygen dissolved in water, then heating the reaction system to 70 ℃, adding 0.52mmol of MBA into the system, heating and stirring for 10min, adding 0.26mmol of APS, continuing stirring for 6h, and cooling to room temperature to obtain the shear-responsive water-based gel lubricant.
With Si 3 N 4 -Si 3 N 4 As a friction pair, the average friction coefficients of the water-based gel lubricant measured at frequencies of 2Hz,4Hz and 8Hz were 0.271, 0.188 and 0.146, respectively.
Example 2
Placing 21.83mmol AM and 5.28mmol AA into a three-neck flask, adding 110ml distilled water, and magnetically stirring at 50 deg.C until the solution is clear and transparent; and introducing high-purity nitrogen into the system for 20min to remove oxygen dissolved in water, heating the reaction system to 75 ℃, adding 0.38mmol of MBA into the system, heating and stirring for 10min, adding 0.17mmol of APS, heating and stirring for 7h, and cooling to room temperature to obtain the shear-responsive water-based gel lubricant.
The average friction coefficients of the water-based gel lubricant measured by using 304-304 stainless steel as a friction pair at frequencies of 2Hz,48Hz and 8Hz are 0.287,0.262 and 0.231 respectively.

Claims (3)

1.一种剪切响应性水基凝胶润滑剂在润滑钢和氮化硅摩擦副中的应用，其特征在于：剪切响应水基凝胶润滑剂的制备方法为：将丙烯酰胺、丙烯酸溶解于水中，加热至50~55℃，搅拌至溶液澄清透明；向体系中通入高纯氮气以除去溶解在水中的氧气，然后将反应体系升温至70℃~75℃，再向反应体系中加入交联剂N,N-亚甲基双丙烯酰胺，搅拌8~15min，然后向反应体系中加入引发剂过硫酸铵，搅拌聚合6~8h后冷却至室温，得到该剪切响应性水基凝胶润滑剂溶液；丙烯酰胺和丙烯酸的摩尔比为3.5:1~4.5:1，丙烯酰胺和丙烯酸按1~1.5%的质量百分数溶于水中。1. The application of a shear-responsive water-based gel lubricant in lubricating steel and silicon nitride friction pairs, characterized in that: the preparation method of the shear-responsive water-based gel lubricant is: acrylamide, acrylic acid Dissolve in water, heat to 50~55°C, stir until the solution is clear and transparent; pass high-purity nitrogen into the system to remove oxygen dissolved in water, then raise the temperature of the reaction system to 70°C~75°C, and then pour into the reaction system Add the cross-linking agent N,N-methylenebisacrylamide, stir for 8~15min, then add the initiator ammonium persulfate into the reaction system, stir and polymerize for 6~8h and then cool to room temperature to obtain the shear-responsive water-based Gel lubricant solution; the molar ratio of acrylamide and acrylic acid is 3.5:1~4.5:1, and the acrylamide and acrylic acid are dissolved in water at a mass percentage of 1~1.5%. 2.如权利要求1所述剪切响应性水基凝胶润滑剂在润滑钢和氮化硅摩擦副中的应用，其特征在于：丙烯酰胺和N,N-亚甲基双丙烯酰胺的摩尔比为40:1~65:1。2. The application of shear responsive water-based gel lubricant in lubricating steel and silicon nitride friction pair as claimed in claim 1, is characterized in that: the mole of acrylamide and N,N-methylenebisacrylamide The ratio is 40:1~65:1. 3.如权利要求1所述剪切响应性水基凝胶润滑剂在润滑钢和氮化硅摩擦副中的应用，其特征在于：N,N-亚甲基双丙烯酰胺和过硫酸铵的摩尔比为1.5:1~1.8:1。3. the application of shear responsive water-based gel lubricant in lubricating steel and silicon nitride friction pair as claimed in claim 1, is characterized in that: N, N-methylenebisacrylamide and ammonium persulfate The molar ratio is 1.5:1~1.8:1.
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纳米复合水凝胶在人工软骨中的研究进展;萧彤等;《中国科学》;20211202;第52卷(第2期);第162-180页 *
聚N-异丙基丙烯酰胺/甲基丙烯酸聚乙二醇酯温敏性水凝胶的制备及性能研究;张晓丽等;《现代化工》;20080731;第28卷(第7期);第54-56页 *

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