CN112522004B - High-temperature-resistant shield tail sealing grease and preparation method thereof - Google Patents

High-temperature-resistant shield tail sealing grease and preparation method thereof Download PDF

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CN112522004B
CN112522004B CN202011388810.0A CN202011388810A CN112522004B CN 112522004 B CN112522004 B CN 112522004B CN 202011388810 A CN202011388810 A CN 202011388810A CN 112522004 B CN112522004 B CN 112522004B
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fiber
temperature
shield tail
tail sealing
sealing grease
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CN112522004A (en
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谢宇飞
王德乾
沈亮
何盛坤
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CRCC South China Construction Guangzhou High Tech Industry Co Ltd
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CRCC South China Construction Guangzhou High Tech Industry Co Ltd
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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
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10—Compounds containing silicon
    • C10M2201/102—Silicates
    • C10M2201/103—Clays; Mica; Zeolites
    • 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
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/022—Ethene
    • 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
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/024—Propene
    • 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
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/026—Butene
    • 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
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
    • 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
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/045—Polyureas; Polyurethanes

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention relates to high-temperature-resistant shield tail sealing grease and a preparation method thereof. The high-temperature-resistant shield tail sealing grease is prepared from the following raw materials in percentage by mass: 10 to 20 percent of base oil, 1 to 5 percent of sepiolite fiber, 2 to 20 percent of base oil absorption fiber and 60 to 87 percent of auxiliary agent; the oil absorption rate of the basic oil absorption fiber to the basic oil is 30-90%. The high-temperature-resistant shield tail sealing grease is very environment-friendly and excellent in high temperature resistance, and meanwhile, the core performance of the high-temperature-resistant shield tail sealing grease is not influenced in water pressure sealing performance, pumping performance and water flushing loss resistance, so that the high-temperature use efficiency of the grease can be effectively improved, the use temperature range of a product is enlarged, and shield construction can be smoothly carried out in a high-temperature environment.

Description

High-temperature-resistant shield tail sealing grease and preparation method thereof
Technical Field
The invention relates to the field of chemical industry, in particular to high-temperature-resistant shield tail sealing grease and a preparation method thereof.
Background
The shield tail seal is a very important safety barrier for ensuring the shield machine to be isolated from underground water, and shield tail seal grease is one of main materials in a shield tail seal link, has the functions of sealing and lubricating, can effectively protect the shield tail, and can isolate soil sand of surrounding strata, underground water, filling slurry behind the shield tail and the like to ensure the shield to be smoothly pushed; and also has the functions of corrosion prevention and friction reduction.
The shield tail sealing grease is a core material for shield tail sealing, the performance index of the shield tail sealing grease can directly influence the efficacy of shield tail sealing, especially in the environment with complex construction processes such as part of high temperature, high water pressure, high permeability and the like and high safety coefficient, the shield tail sealing grease has extremely high requirements on the performance of the shield tail sealing grease, generally speaking, the performance index of the shield tail sealing grease is easy to change suddenly, for example, the shield tail sealing grease can become thin at high temperature, the index fluctuation of the shield tail sealing grease such as pumpability, water pressure resistance sealing performance, water flushing resistance performance and the like is large, water leakage and slurry leakage are easily caused in shield construction of a high water pressure and high permeability stratum, construction is influenced, and normal tunneling cannot be realized.
In most areas of China, the temperature is about 35 ℃ on average in summer, the highest temperature can reach 45 ℃ in some areas, and the high-temperature environment has great test on each link of construction. Therefore, the shield tail sealing grease which can resist high temperature and has good comprehensive performance has important significance.
Disclosure of Invention
Based on the above, the invention aims to provide the high-temperature-resistant shield tail sealing grease which has excellent high-temperature resistance, good comprehensive performance at high temperature (30-45 ℃), good temperature stability and unaffected core performances such as water pressure sealing performance, pumping performance and water-washing loss resistance.
The technical scheme is as follows:
the high-temperature-resistant shield tail sealing grease is prepared from the following raw materials in percentage by mass:
Figure BDA0002811724020000021
the oil absorption rate of the basic oil absorption fiber to the basic oil is 60-90%.
In one embodiment, the length of the sepiolite fiber is 2mm to 4 mm.
In one embodiment, the basic oil-absorbing fiber comprises a natural oil-absorbing fiber and a synthetic oil-absorbing fiber, and the mass ratio of the natural oil-absorbing fiber to the synthetic oil-absorbing fiber is 1: 1-1: 2.
In one embodiment, the length of the natural oil absorption fiber is 1 mm-2 mm; the length of the synthetic oil absorption fiber is 4 mm-8 mm.
In one embodiment, the natural oil absorbing fiber is selected from at least one of wood fiber, bamboo fiber, flax fiber, cotton fiber, kapok fiber, and pulp fiber.
In one embodiment, the synthetic oil absorbing fibers are selected from at least one of polypropylene fibers and polyurethane fibers.
In one embodiment, the additive is selected from at least one of a viscosity index improver, a filler, and a lubricant.
In one embodiment, the high-temperature-resistant shield tail sealing grease is prepared from the following raw materials in percentage by mass:
Figure BDA0002811724020000022
Figure BDA0002811724020000031
in one embodiment, the high-temperature-resistant shield tail sealing grease is prepared from the following raw materials in percentage by mass:
Figure BDA0002811724020000032
in one embodiment, the kinematic viscosity of the viscosity index improver at 100 ℃ is 2000mm2/s～8000mm2/s。
In one embodiment, the viscosity index improver consists of a polymer A and a polymer B according to the mass ratio of 1: 1-1: 1.5;
the polymer A is selected from at least one of polyisobutylene, coumarone resin and terpene resin;
the polymer B is at least one selected from ethylene propylene rubber and polyacrylic acid.
In one embodiment, the base oil has a saturates content of greater than 90% and a viscosity index of greater than 80.
In one embodiment, the base oil is selected from at least one of 150N, 150SN, and 250N.
In one embodiment, the filler is selected from at least one of light calcium, talc, mica powder, silica, and barium carbonate.
In one embodiment, the filler has a particle size of 2000-6000 mesh.
In one embodiment, the lubricant is selected from at least one of 2# extreme pressure lithium base grease and 3# extreme pressure lithium base grease.
The invention also provides a preparation method of the high-temperature-resistant shield tail sealing grease, which comprises the following steps:
and mixing the base oil, the sepiolite fibers, the base oil absorption fibers and the auxiliary agent.
Compared with the prior art, the invention has the following beneficial effects:
the formula of the high-temperature-resistant shield tail sealing grease provided by the invention comprises base oil, sepiolite fibers, specific base oil absorption fibers and an auxiliary agent in a specific mass percentage. The sepiolite fiber is a natural mineral fiber, the specific surface area is large, a layer of magnesium-oxygen octahedron is sandwiched between two silicon-oxygen tetrahedrons in the structure to form a 2: 1 type layered structure unit, the magnesium-oxygen octahedron layer forms channels which are arranged alternately at the upper layer and the lower layer, the orientation of the channels is consistent with the sepiolite fiber axis, and the base oil can enter the channels, so that the sepiolite fiber is very stable and not easy to separate, and the density and the compactness of the shield tail sealing grease can be improved; meanwhile, the sepiolite fibers have excellent characteristics of good heat resistance, insulation, heat insulation and the like, and the integral high-temperature resistance of the shield tail sealing grease is improved. The basic oil absorption fibers are used in a matched mode, the basic oil absorption fibers are mutually interpenetrated, the sepiolite fibers and the basic oil absorption fibers are mutually interpenetrated and criss-cross staggered to form a network, the basic oil and the auxiliary agent are filled in the network, the structure is very stable, and the high-temperature resistance performance is excellent. In addition, the base oil absorption rate of the base oil absorption fiber to the base oil is high, the base oil is not easy to separate, and the high-temperature stability of the shield tail sealing grease is further improved. And the fiber material has excellent ductility and toughness, and the compounding of various fiber materials can endow the shield tail sealing grease of the invention with excellent compression resistance and tear resistance, and can solve the problems of water leakage and slurry leakage of the shield machine in the construction environment with high temperature, high water pressure and high permeability.
In addition, the shield tail sealing grease is non-toxic, odorless, biodegradable, green and environment-friendly, has no pollution to soil and underground water, has no corrosivity to related parts of a shield machine, and has wide application prospect.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the present invention, the oil absorption is calculated according to formula (1):
Figure BDA0002811724020000051
in the formula:
Rxy-is the oil absorption,%;
mohthe mass g of the sample after the oil absorption material is saturated in oil absorption and stands;
moq-sample mass of oil absorbing material before oil absorption, g.
The shield tail sealing grease is a core material for shield tail sealing, main raw materials of the shield tail sealing grease are greatly influenced by temperature fluctuation, the shield tail sealing grease becomes thin at high temperature, and the water resistance and pressure maintaining performance is poor, so that normal construction tunneling is influenced.
Aiming at the problems, the inventor provides the high-temperature-resistant shield tail sealing grease which has excellent high-temperature resistance, still has better comprehensive performance at high temperature (30-45 ℃), has good temperature stability, and has the core performance of water pressure sealing resistance, pumping performance and water washing loss resistance which are not influenced, so that shield construction can still be carried out smoothly in a high-temperature environment.
The technical scheme is as follows:
the high-temperature-resistant shield tail sealing grease is prepared from the following raw materials in percentage by mass:
Figure BDA0002811724020000061
the oil absorption rate of the basic oil absorption fiber to the basic oil is 60-90%.
The sepiolite fiber is a natural mineral fiber, has large specific surface area, a layer of magnesium-oxygen octahedron is sandwiched between two silicon-oxygen tetrahedrons in the structure to form a 2: 1 type layered structure unit, the magnesium-oxygen octahedron forms channels which are arranged alternately at the upper layer and the lower layer, the orientation of the channels is consistent with the sepiolite fiber axis, and the base oil can enter the channels, is very stable and is not easy to separate; meanwhile, the sepiolite fibers have excellent characteristics of good heat resistance, insulation, heat insulation and the like, and the integral high-temperature resistance of the shield tail sealing grease is improved. The basic oil absorption fibers are used in a matched mode, the basic oil absorption fibers are mutually interpenetrated, the sepiolite fibers and the basic oil absorption fibers are mutually interpenetrated and criss-cross staggered to form a network, the basic oil and the auxiliary agent are filled in the network, the structure is very stable, and the high-temperature resistance performance is excellent. In addition, the base oil absorption rate of the base oil absorption fiber to the base oil is high, the base oil is not easy to separate, and the high-temperature stability of the shield tail sealing grease is further improved. And the fiber material has excellent ductility and toughness, and the compounding of various fiber materials endows the shield tail sealing grease of the invention with excellent compression resistance and tear resistance, so that the problems of water leakage and slurry leakage of the shield machine in a high-temperature, high-water pressure and high-permeability construction environment can be solved.
Tests prove that the high-temperature-resistant shield tail sealing grease provided by the invention can keep the pressure for 30min and does not leak water at the temperature of 30-45 ℃ and under the pressure of 8MPa, the maximum water pressure of 8bar in field construction application does not leak water or slurry, and the pumpability and the water-impact resistance are basically unchanged. In addition, the shield tail sealing grease is non-toxic, odorless, biodegradable, green and environment-friendly, has no pollution to soil and underground water, has no corrosivity to related parts of the shield tunneling machine, and has wide application prospect.
In one embodiment, the basic oil-absorbing fiber comprises a natural oil-absorbing fiber and a synthetic oil-absorbing fiber, wherein the mass ratio of the natural oil-absorbing fiber to the synthetic oil-absorbing fiber is 1: 1-1: 2; the natural oil absorption fiber is selected from at least one of wood fiber, bamboo fiber, flax fiber, cotton fiber, kapok fiber and pulp fiber; the synthetic oil absorbing fiber is at least one selected from polypropylene fiber, polyurethane fiber and alkyl ethylene polymer.
The oil absorption principle of the natural oil absorption fiber depends on the pores of the material and utilizes the capillary principle to absorb oil; the synthetic oil absorption fiber is used for hiding and absorbing oil by utilizing the hydrophobic and oleophylic characteristics of the synthetic oil absorption fiber and gaps among polymer molecules, and has the advantages of high oil absorption speed, high oil absorption rate, good overall performance and convenience in use and recovery. The two oil absorption fibers are compounded for use, so that the absorption capacity of the base oil can be further improved, and the compactness of the shield tail sealing grease is improved.
In one embodiment, the length of the natural oil absorption fiber is 1 mm-2 mm; the length of the synthetic oil absorption fiber is 4 mm-8 mm. The basic oil absorption fibers with different lengths are compounded, so that a stable network structure is formed among the basic oil absorption fibers.
If the length of the sepiolite fiber is controlled at the same time, the sepiolite fiber is in the length range of the basic oil absorption fiber, and a compact network structure is formed between the basic oil absorption fiber and the sepiolite fiber. Preferably, the length of the sepiolite fiber is 2 mm-4 mm.
In one embodiment, the additive is selected from at least one of a viscosity index improver, a filler, and a lubricant.
The viscosity index improver can improve the viscosity-temperature characteristic of shield tail sealing grease so as to meet the requirement of a wide temperature range on grease viscosity; and the viscosity index improver has a strong tackifying effect, increases the integral viscosity of the shield tail sealing grease, can be stably adhered to the shield tail, is not easy to fall off, further enhances the sealing effect of the shield tail sealing grease, and is beneficial to construction. The filler is filled in the fiber network, so that the function of a reinforcing agent and an excipient can be exerted, the shield tail sealing grease is pasty, and the sealing function, the water resistance and the corrosion resistance are realized; and the base oil, the viscosity index improver and the lubricant can be adsorbed, so that the base oil, the viscosity index improver and the lubricant are stably contained in the shield tail sealing grease together, and the sealing effect, the water pressure resistance and the high temperature stability of the shield tail sealing grease are enhanced. And the lubricant is added into the formula, so that the shield tail sealing grease has better lubricating effect and pumping property on the shield machine, and the shield construction is ensured to be carried out smoothly. Therefore, through the synergy of all components, the high-temperature-resistant shield tail sealing grease disclosed by the invention has excellent temperature stability (especially high-temperature stability), water pressure sealing resistance, pumping property, adhesion, tear tensile resistance and lubricity, and can completely fill a shield tail grease cavity, a shield tail gap and a shield tail steel wire brush, and the high-temperature-resistant shield tail sealing grease provided by the invention is applied to shield tail sealing in shield construction, so that the problem of performance index mutation of the shield tail sealing grease in a high-temperature environment of 30-45 ℃ can be solved; the problem of water leakage and slurry leakage caused by failure of shield tail sealing grease during construction of the shield tunneling machine under complex geological conditions of high water pressure, high permeability and the like can also be solved.
In one embodiment, the high-temperature-resistant shield tail sealing grease is prepared from the following raw materials in percentage by mass:
Figure BDA0002811724020000081
in one preferable embodiment, the high-temperature-resistant shield tail sealing grease is prepared from the following raw materials in percentage by mass:
Figure BDA0002811724020000082
Figure BDA0002811724020000091
in one embodiment, the kinematic viscosity of the viscosity index improver at 100 ℃ is 2000mm2/s～8000mm2And/s is more favorable for ensuring the viscosity and the high-temperature resistance of the shield tail sealing grease.
In one embodiment, the viscosity index improver consists of a polymer A and a polymer B according to the mass ratio of 1: 1-1: 1.5; the polymer A is selected from at least one of polyisobutylene, coumarone resin and terpene resin; the polymer B is at least one selected from ethylene propylene rubber and polyacrylic acid. The viscosity index improver is favorable for improving the temperature stability, water pressure resistance, adhesion and tear and tensile properties of the shield tail sealing grease.
In one embodiment, the base oil has a saturates content of greater than 90% and a viscosity index of greater than 80. Preferably, the base oil is selected from at least one of 150N, 150SN and 250N.
In one embodiment, the filler is selected from at least one of light calcium, talc, mica powder, silica, and barium carbonate. The filler is beneficial to improving the temperature stability and the water pressure resistance of the shield tail sealing grease. Preferably, the filler is light calcium.
In one preferable embodiment, the particle size of the filler is 2000-6000 meshes.
In one embodiment, the lubricant is selected from at least one of 2# extreme pressure lithium base grease and 3# extreme pressure lithium base grease. Such lubricants are beneficial for improving the pumpability and lubricity impact of the tail seal grease.
The invention also provides a preparation method of the high-temperature-resistant shield tail sealing grease, which comprises the following steps:
and mixing the base oil, the sepiolite fibers, the base oil absorption fibers and the auxiliary agent.
The preparation method of the high-temperature-resistant shield tail sealing grease which contains base oil, sepiolite fibers, base oil absorption fibers, fillers, viscosity index improver and lubricant in the formula comprises the following steps;
dissolving and stirring the base oil and the viscosity index improver in a dissolving tank, and uniformly mixing to obtain a mixture A;
and sequentially adding the mixture A, the basic oil absorption fiber, the sepiolite fiber, the filler and the lubricant into a kneader and uniformly mixing.
Preferably, the preparation method of the high-temperature-resistant shield tail sealing grease containing the base oil, the sepiolite fibers, the base oil absorption fibers, the filler, the viscosity index improver and the lubricant in the formula comprises the following steps;
first, equipment parameter
Setting a mold temperature machine: the temperature is 140-150 ℃, and can be properly adjusted according to the situation
Oil material feeding setting: preparing base oil in advance;
the kneader is arranged:
(1) host stirring frequency: 30Hz
(2) Screw stirring frequency: 40Hz, and can be adjusted according to the actual situation during discharging;
(3) oil temperature: the temperature is 80-90 ℃, and can be adjusted according to the actual production condition;
(4) material temperature: the temperature is 70-80 ℃, and can be adjusted according to the actual production condition;
secondly, controlling the charging process
1. Feeding an oil material stirring barrel:
(1) opening a set parameter of a mold temperature controller, and starting an oil barrel heating system;
(2) opening a charging operation interface, setting basic oil charging parameters, starting charging, and charging the basic oil;
(3) after the first two steps are finished, adding a viscosity index improver into the stirring barrel;
(4) after the raw materials are added, the oil material barrel is heated to 90 ℃ and is continuously stirred for 20-30 min, and the mixture is fed into a kneader.
2. Feeding of kneading machine
(1) Starting a kneader for preheating (the kneader can be started for preheating 15min before oil is injected), starting the kneader for stirring after preheating is finished, and carrying out the next step;
(2) injecting the oil into a kneader;
(3) adding natural oil absorption fiber, stirring for 1-15 min after completion, adding sepiolite fiber and synthetic oil absorption fiber, and continuously stirring for 1-15 min after completion;
(4) adding the filler, and suspending the stirring of the kneading machine after the completion;
(5) and (3) putting the lubricant into a kneader, starting stirring, continuously stirring for 1-5 h, and taking the product out of the pot.
The following are specific examples.
All starting materials are, unless otherwise specified, derived from commercially available products.
Example 1
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof.
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 1 are as follows by mass percent:
150N 14% of base oil, and polyisobutene (kinematic viscosity at 100 ℃ of 5200 mm)210% of/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 mm)27% of/s), 8% of cotton fiber (with the length of 1-2 mm), 4% of sepiolite fiber (with the length of 2-4 mm), 3% of polypropylene fiber (with the length of 4-8 mm), 44% of light calcium (2000 mesh), 10% of 2# extreme pressure lithium base grease, 80% of oil absorption rate of the cotton fiber on base oil and 75% of oil absorption rate of the polypropylene fiber on the base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 1:
first, equipment parameter
(1) Setting a mold temperature machine: the temperature is 140-150 ℃, and can be properly adjusted according to the situation
(2) Oil material feeding setting: preparing base oil in advance;
(3) the kneader is arranged:
host stirring frequency: 30 Hz;
screw stirring frequency: 40 Hz;
oil temperature: 80-90 ℃;
material temperature: 70-80 ℃;
secondly, controlling the charging process
1. Feeding an oil material stirring barrel:
(1) opening a set parameter of a mold temperature controller, and starting an oil barrel heating system;
(2) opening a charging operation interface, setting basic oil charging parameters, starting charging, and charging the basic oil;
(3) adding a viscosity index improver into the stirring barrel;
(4) and continuing stirring for 20-30 min after the temperature of the oil barrel is raised to 90 ℃.
2. Feeding by a kneader:
(1) opening a kneading machine for preheating 15min before oil injection, and starting the kneading machine for stirring after preheating is finished;
(2) injecting the oil into a kneader;
(3) adding natural oil-absorbing fiber, stirring for 3min, adding sepiolite fiber and synthetic oil-absorbing fiber, and stirring for 5 min;
(4) adding the filler, and suspending the stirring of the kneading machine after the completion;
(5) and (3) adding the lubricant into a kneader, starting stirring, and continuously stirring for 2 hours to obtain the high-temperature-resistant shield tail sealing grease 1, wherein the physical and chemical indexes are shown in table 1.
TABLE 1 high-temp. resistant shield tail sealing grease 1 Performance parameter table
Figure BDA0002811724020000121
Figure BDA0002811724020000131
Example 2
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof.
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 2 are as follows by mass percent:
150N 16% of base oil, and polyisobutylene (kinematic viscosity at 100 ℃ C. of 2400 m)28% of ethylene propylene rubber (the kinematic viscosity at 100 ℃ is 8000 mm)25% of/s), 7% of cotton fiber (length 1 mm-2 mm), sea2% of sepiolite fiber (with the length of 2-4 mm), 3% of polypropylene fiber (with the length of 4-8 mm), 47% of light calcium (2000 meshes), 12% of 2# extreme pressure lithium-based grease, 85% of oil absorption rate of cotton fiber on base oil and 70% of oil absorption rate of polypropylene fiber on base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 2:
the preparation method is the same as that of the example 1, and the high-temperature-resistant shield tail sealing grease 2 is obtained, and the physical and chemical indexes of the high-temperature-resistant shield tail sealing grease are shown in the table 2.
TABLE 2 high temperature resistant shield tail sealing grease 2 Performance parameter Table
Figure BDA0002811724020000132
Figure BDA0002811724020000141
Example 3
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof.
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 3 are as follows by mass percent:
150N 15% of base oil and polyisobutene (kinematic viscosity at 100 ℃ of 6000 m)26% of ethylene propylene rubber (kinematic viscosity at 100 ℃) of 3200m29 percent/s), 4 percent of cotton fiber (with the length of 1 mm-2 mm), 1 percent of sepiolite fiber (with the length of 2 mm-4 mm), 2 percent of polypropylene fiber (with the length of 4 mm-8 mm), 51 percent of light calcium (2000 mesh), 12 percent of 2# extreme pressure lithium base grease, 80 percent of oil absorption rate of the cotton fiber to the base oil and 75 percent of oil absorption rate of the polypropylene fiber to the base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 3:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 3 is obtained, and the physical and chemical indexes of the grease are shown in table 3.
TABLE 3 high-temp. resistant shield tail sealing grease 3 performance parameter table
Figure BDA0002811724020000151
Example 4
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof. Compared with example 1, the difference is that the kinematic viscosity of the polyisobutene is 3200m2The kinematic viscosity of the ethylene propylene rubber is 5200m2/s。
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 4 are as follows by mass percent:
150N 14% of base oil, and polyisobutene (kinematic viscosity at 100 ℃ of 3200 m)210% of ethylene propylene rubber (with the kinematic viscosity of 5200m at 100℃)27% of/s), 8% of cotton fiber (with the length of 1-2 mm), 4% of sepiolite fiber (with the length of 2-4 mm), 3% of polypropylene fiber (with the length of 4-8 mm), 44% of light calcium (2000 mesh), 10% of 2# extreme pressure lithium base grease, 80% of oil absorption rate of the cotton fiber on base oil and 75% of oil absorption rate of the polypropylene fiber on the base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 4:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 4 is obtained, and the physical and chemical indexes of the grease are shown in table 4.
TABLE 4 high-temp. resistant shield tail sealing grease 4 performance parameter table
Figure BDA0002811724020000161
Figure BDA0002811724020000171
Example 5
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof. Compared with the example 1, the difference is that the length of the sepiolite fiber is 6mm to 8 mm.
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 5 are as follows by mass percent:
150N 14% of base oil, polyisobutylene (at 100 ℃ C. for sports)Viscosity of 5200m210% of (a)/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 m)2S)7 percent, 8 percent of cotton fiber (with the length of 1 mm-2 mm), 4 percent of sepiolite fiber (with the length of 6 mm-8 mm), 3 percent of polypropylene fiber (with the length of 4 mm-8 mm), 44 percent of light calcium (2000 mesh), 10 percent of 2# extreme pressure lithium base grease, 80 percent of oil absorption rate of the cotton fiber to the base oil and 75 percent of oil absorption rate of the polypropylene fiber to the base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 5:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 5 is obtained, and the physical and chemical indexes of the grease are shown in table 5.
TABLE 5 high-temp. resistant shield tail sealing grease 5 Performance parameter table
Figure BDA0002811724020000172
Figure BDA0002811724020000181
Example 6
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof. Compared with the example 1, the difference is that the length of the sepiolite fiber, the cotton fiber and the polypropylene fiber is 2mm to 4 mm.
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 6 are as follows by mass percent:
150N 14% of base oil, and polyisobutene (with a kinematic viscosity of 5200m at 100 ℃)210% of (a)/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 m)27% of/s), 8% of cotton fiber (with the length of 2-4 mm), 4% of sepiolite fiber (with the length of 2-4 mm), 3% of polypropylene fiber (with the length of 2-4 mm), 44% of light calcium (2000 meshes) and 10% of 2# extreme pressure lithium-based grease.
(2) Preparing high-temperature-resistant shield tail sealing grease 6:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 6 is obtained, and the physical and chemical indexes of the grease are shown in table 6.
TABLE 6 high-temp. resistant shield tail sealing grease 6 performance parameter table
Figure BDA0002811724020000182
Figure BDA0002811724020000191
Example 7
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof. Compared with the example 1, the difference is that the adopted natural oil absorption fiber is bamboo fiber.
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 7 are as follows by mass percent:
150N 14% of base oil, and polyisobutene (with a kinematic viscosity of 5200m at 100 ℃)210% of (a)/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 m)27% of/s), 8% of bamboo fiber (with the length of 1-2 mm), 4% of sepiolite fiber (with the length of 2-4 mm), 3% of polypropylene fiber (with the length of 4-8 mm), 44% of light calcium (2000 mesh), 10% of 2# extreme pressure lithium base grease, 60% of oil absorption rate of the bamboo fiber on base oil and 75% of oil absorption rate of the polypropylene fiber on the base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 7:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 7 is obtained, and the physical and chemical indexes of the grease are shown in table 7.
TABLE 7 high-temp. resistant shield tail sealing grease 7 performance parameter table
Figure BDA0002811724020000201
Example 8
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof. Compared with example 1, the difference is that the synthetic oil absorbing fiber is polyurethane fiber.
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 7 are as follows by mass percent:
150N 14% of base oil, and polyisobutene (with a kinematic viscosity of 5200m at 100 ℃)210% of (a)/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 m)27% of/s), 8% of cotton fiber (with the length of 1-2 mm), 4% of sepiolite fiber (with the length of 2-4 mm), 3% of polyurethane fiber (with the length of 4-8 mm), 44% of light calcium (2000 mesh), 10% of 2# extreme pressure lithium base grease, 80% of oil absorption rate of the cotton fiber on base oil and 60% of oil absorption rate of the polyurethane fiber on the base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 8:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 8 is obtained, and the physical and chemical indexes of the grease are shown in table 5.
TABLE 8 high-temp. resistant shield tail sealing grease 8 performance parameter table
Figure BDA0002811724020000211
Figure BDA0002811724020000221
Example 9
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof. Compared to example 1, the difference is that only one base oil absorbing fiber is used.
(1) The high-temperature-resistant shield tail sealing grease 9 is prepared from the following raw materials in percentage by mass:
150N 14% of base oil, and polyisobutene (with a kinematic viscosity of 5200m at 100 ℃)210% of (a)/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 m)27% of/s), 11% of cotton fiber (with the length of 1-2 mm), 4% of sepiolite fiber (with the length of 2-4 mm), 44% of light calcium (2000 meshes), 10% of 2# extreme pressure lithium base grease, and 80% of oil absorption rate of the cotton fiber to base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 9:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 9 is obtained, and the physical and chemical indexes of the grease are shown in table 9.
TABLE 9 PERFORMANCE PARAMETERS OF HIGH-temp. RESISTANT SEALING OIL 9
Figure BDA0002811724020000222
Figure BDA0002811724020000231
Example 10
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof. Compared to example 1, the difference is that only one base oil absorbing fiber is used.
(1) The high-temperature-resistant shield tail sealing grease 10 is prepared from the following raw materials in percentage by mass:
150N 14% of base oil, and polyisobutene (with a kinematic viscosity of 5200m at 100 ℃)210% of (a)/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 m)27% of/s), 4% of sepiolite fiber (with the length of 2 mm-4 mm), 11% of polypropylene fiber (with the length of 4 mm-8 mm), 44% of light calcium (2000 meshes), 10% of 2# extreme pressure lithium base grease, and 75% of oil absorption rate of the polypropylene fiber to base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 10:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 10 is obtained, and the physical and chemical indexes of the grease are shown in table 10.
TABLE 10 high-temp. resistant shield tail sealing grease 10 performance parameter table
Figure BDA0002811724020000232
Figure BDA0002811724020000241
Example 11
The embodiment provides high-temperature-resistant shield tail sealing grease and a preparation method thereof.
(1) The preparation raw materials of the high-temperature-resistant shield tail sealing grease 11 are as follows by mass percent:
250N 10% of base oil and 4600m of coumarone resin (kinematic viscosity at 100℃)25% of acrylic acid (with a kinematic viscosity of 3000m at 100 ℃ C.)25% of/s), 5% of flax fiber (with the length of 1-2 mm), 2% of sepiolite fiber (with the length of 2-4 mm), 3% of polyurethane fiber (with the length of 4-8 mm), 60% of light calcium (2000 mesh), 10% of 3# extreme pressure lithium base grease, 75% of oil absorption rate of the flax fiber on base oil and 60% of oil absorption rate of the polyurethane fiber on the base oil.
(2) Preparing high-temperature-resistant shield tail sealing grease 11:
the preparation method is the same as that of example 1, and the high-temperature-resistant shield tail sealing grease 11 is obtained, and the physical and chemical indexes of the grease are shown in table 11.
Table 11 high temperature resistant shield tail sealing grease 11 performance parameter table
Figure BDA0002811724020000251
Comparative example 1
The comparative example provides shield tail sealing grease and a preparation method thereof. The difference compared to example 1 is that the addition of sepiolite fibers was omitted.
(1) The shield tail sealing grease 12 is prepared from the following raw materials in percentage by mass:
150N 14% of base oil, and polyisobutene (with a kinematic viscosity of 5200m at 100 ℃)210% of (a)/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 m)2S)7 percent, 8 percent of cotton fiber (with the length of 1 mm-2 mm), 7 percent of polypropylene fiber (with the length of 4 mm-8 mm), 44 percent of light calcium (2000 meshes), 10 percent of 2# extreme pressure lithium base grease, 80 percent of oil absorption rate of the cotton fiber to the base oil and 75 percent of oil absorption rate of the polypropylene fiber to the base oil.
(2) Preparing shield tail sealing grease 12:
sepiolite fibers were removed, and the preparation method was substantially the same as in example 1, to obtain shield tail seal grease 12, the physical and chemical indexes of which are shown in table 12.
Table 12 shield tail sealing grease 12 performance parameter table
Figure BDA0002811724020000261
Comparative example 2
The comparative example provides shield tail sealing grease and a preparation method thereof. Compared with example 1, the sepiolite fibers were replaced with polyester fibers.
(1) The shield tail sealing grease 13 is prepared from the following raw materials in percentage by mass:
150N 14% of base oil, and polyisobutene (with a kinematic viscosity of 5200m at 100 ℃)210% of (a)/s) and ethylene propylene rubber (kinematic viscosity at 100 ℃ of 4600 m)2S)7 percent, 8 percent of cotton fiber (with the length of 1 mm-2 mm), 4 percent of polyester fiber (with the length of 2 mm-4 mm), 3 percent of polypropylene fiber (with the length of 4 mm-8 mm), 44 percent of light calcium (2000 mesh), 10 percent of 2# extreme pressure lithium base grease, 80 percent of oil absorption rate of the cotton fiber to the base oil, and 75 percent of oil absorption rate of the polypropylene fiber to the base oil.
(2) Preparing shield tail sealing grease 13:
the sepiolite fiber was replaced with a polyester fiber, and the preparation method was substantially the same as in example 1, to obtain shield tail sealing grease 13, whose physical and chemical indexes are shown in table 13.
Table 13 shield tail sealing grease 13 performance parameter table
Figure BDA0002811724020000271
Figure BDA0002811724020000281
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The high-temperature-resistant shield tail sealing grease is characterized by being prepared from the following raw materials in percentage by mass:
Figure FDA0003119665250000011
the oil absorption rate of the base oil absorption fiber to the base oil is 60-90%;
the kinematic viscosity of the viscosity index improver at 100 ℃ is 2000mm2/s～8000mm2/s；
The basic oil absorption fiber comprises a natural oil absorption fiber and a synthetic oil absorption fiber, wherein the natural oil absorption fiber is a cotton fiber, and the synthetic oil absorption fiber is a polypropylene fiber;
the length of the natural oil absorption fiber is 1 mm-2 mm; the length of the synthetic oil absorption fiber is 4-8 mm; the length of the sepiolite fiber is 2 mm-4 mm.
2. The high-temperature-resistant shield tail sealing grease as claimed in claim 1, wherein the saturated hydrocarbon content of the base oil is greater than 90%, and the viscosity index is greater than 80.
3. The high-temperature-resistant shield tail sealing grease of claim 2, wherein the base oil is at least one selected from 150N, 150SN and 250N.
4. The high-temperature-resistant shield tail sealing grease as claimed in claim 1, wherein the mass ratio of the natural oil-absorbing fiber to the synthetic oil-absorbing fiber is 1: 1-1: 2.
5. The high-temperature-resistant shield tail sealing grease as claimed in claim 1, wherein the viscosity index improver consists of a polymer A and a polymer B in a mass ratio of 1: 1-1: 1.5;
the polymer A is selected from at least one of polyisobutylene, coumarone resin and terpene resin;
the polymer B is at least one selected from ethylene propylene rubber and polyacrylic acid.
6. The high-temperature-resistant shield tail sealing grease as claimed in claim 1, wherein the filler is at least one selected from light calcium, talcum powder, mica powder, silica and barium carbonate;
the lubricant is selected from at least one of 2# extreme pressure lithium base grease and 3# extreme pressure lithium base grease.
7. The high-temperature-resistant shield tail sealing grease as claimed in claim 1, wherein the filler has a particle size of 2000-6000 meshes.
8. The high-temperature-resistant shield tail sealing grease as claimed in claim 1, which is prepared from the following raw materials in percentage by mass:
150N 14% of base oil, 10% of polyisobutylene, 7% of ethylene propylene rubber, 8% of cotton fiber, 4% of sepiolite fiber, 3% of polypropylene fiber, 44% of light calcium and 10% of 2# extreme pressure lithium base grease;
the kinematic viscosity of the polyisobutene at 100 ℃ is 5200mm2/s；
The kinematic viscosity of the ethylene propylene rubber at 100 ℃ is 4600mm2/s；
The length of the cotton fiber is 1 mm-2 mm, the length of the sepiolite fiber is 2 mm-4 mm, and the length of the polypropylene fiber is 4 mm-8 mm;
the particle size of the light calcium carbonate is 2000 meshes, the oil absorption rate of the cotton fiber to the base oil 150N is 80%, and the oil absorption rate of the polypropylene fiber to the base oil 150N is 75%.
9. The high-temperature-resistant shield tail sealing grease as claimed in claim 1, which is prepared from the following raw materials in percentage by mass:
150N 16% of base oil, 8% of polyisobutylene, 5% of ethylene propylene rubber, 7% of cotton fiber, 2% of sepiolite fiber, 3% of polypropylene fiber, 47% of light calcium and 12% of 2# extreme pressure lithium base grease;
the kinematic viscosity of the polyisobutene at 100 ℃ is 2400mm2/s；
The kinematic viscosity of the ethylene propylene rubber at 100 ℃ is 8000mm2/s；
The length of the cotton fiber is 1 mm-2 mm, the length of the sepiolite fiber is 2 mm-4 mm, and the length of the polypropylene fiber is 4 mm-8 mm;
the particle size of the light calcium carbonate is 2000 meshes, the oil absorption rate of the cotton fiber to the base oil 150N is 85%, and the oil absorption rate of the polypropylene fiber to the base oil 150N is 70%.
10. The preparation method of the high-temperature-resistant shield tail sealing grease as claimed in any one of claims 1 to 9, which is characterized by comprising the following steps:
and mixing the base oil, the sepiolite fibers, the base oil absorption fibers and the auxiliary agent.
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