CN108659297A - A kind of novel fire resistant silicone grease composition and preparation method thereof - Google Patents
A kind of novel fire resistant silicone grease composition and preparation method thereof Download PDFInfo
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- CN108659297A CN108659297A CN201810387410.4A CN201810387410A CN108659297A CN 108659297 A CN108659297 A CN 108659297A CN 201810387410 A CN201810387410 A CN 201810387410A CN 108659297 A CN108659297 A CN 108659297A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
A kind of novel fire resistant silicone grease composition of present invention offer and preparation method thereof.The novel fire resistant silicone grease composition, in terms of mass fraction, including following components：70~90 parts of base oil, 1~10 part of organic thickening agent, 0~10 part of inorganic thickening agent, 0.1~2 part of structural stabilizing agent, 1~5 part of 1~10 part of lubricant, 0.1~2 part of antioxidant and dispersant, the base oil, which is selected from, adds one or more of hydrogen paraffine base crude oil, naphthene base crude oil, polyalphaolefin and silicone oil.High temperature resistant silicon oil/fat composition disclosed by the invention solves the problems, such as the poor compatibility of common insulation lubrication silicone grease and cable accessory, contacts non-swelling or slight swelling for a long time with silicon rubber and ethylene propylene diene rubber, can ensure cable accessory use steady in a long-term.
Description
Technical field：
The invention belongs to technical field of polymer materials, and in particular to a kind of novel fire resistant silicone grease composition and its preparation
Method.
Background technology：
Cable accessory is connecting cable and electric line and the product of related power distribution equipment, and electric power is constituted together with cable
Transport net；Cable accessory requires the characteristic for having the construction of cable, can restore the performance of cable and the extension of cable length
And the connection of terminal.The reliability of cable accessory can be from electric property, moisture resistant seal, mechanical performance and processing performance etc.
Aspect is judged.The main material of end attachment is silicon rubber, and the connection type generally used is prefabricated, in connection
It needs to coat electric insulation special-purpose grease.
Electric insulation special-purpose grease will have good stability, with cable accessory because being in direct contact with cable accessory
It contacts for a long time non-swelling.The general material of cable accessory is silicon rubber or ethylene propylene diene rubber, therefore it is required that electric insulation is special
There is good compatibility with fat and silicon rubber and ethylene propylene diene rubber.The electric insulation special-purpose grease used on the market at present is main
It is divided into three categories：Insulation lubrication silicone grease, extraordinary insulation fat and ether fat.The ether fat largely used at China's cable connector at present is easy
Desiccation, stability is very poor, and being easy, which makes cable accessory that breakdown occur, causes cable integrally to scrap.And commonly insulate lubrication silicone grease and silicon
The poor compatibility of rubber has cable connector special requirement, can not be widely used.Therefore it develops and a is exclusively used in cable accessory
And contacted with its long-time non-swelling electric insulation special-purpose grease be very it is necessary to.
Invention content：
It is disclosed by the invention resistance to the object of the present invention is to provide a kind of novel fire resistant silicone grease composition and preparation method thereof
High temperature silicone grease composition solves the problems, such as the poor compatibility of common insulation lubrication silicone grease and cable accessory, with silicon rubber and three
First EP rubbers contacts non-swelling or slight swelling for a long time, can ensure cable accessory use steady in a long-term.
The object of the present invention is to provide a kind of novel fire resistant silicone grease compositions, in terms of mass fraction, including with the following group
Point：70~90 parts of base oil, 1~10 part of organic thickening agent, 0~10 part of inorganic thickening agent, 0.1~2 part of structural stabilizing agent, lubrication
1~5 part of 1~10 part of agent, 0.1~2 part of antioxidant and dispersant, the base oil is selected from plus hydrogen paraffine base crude oil, naphthene base crude oil,
One or more of polyalphaolefin and silicone oil.
It is preferred that the base oil is polyalphaolefin or dimethicone.
It is preferred that the organic thickening agent is selected from styrene-butadiene (SB), styrene-butadiene/propylene (SEP), benzene
Ethylene-butylene/ethylene (SEB), styrene-butadiene-styrene (SBS), styrene-ethylene/butylene-styrene
(SEBS), one or more of styrene-ethylene/propylene-styrene (SEPS) and ethylene propylene diene rubber.
It is preferred that the inorganic thickening agent be aerosil, the structural stabilizing agent be ethylene glycol, propylene glycol or
Glycerine, the lubricant are ptfe micropowder.It is white puff sprills under aerosil room temperature, has very
Good thickening effect.
It is preferred that the antioxidant is be obstructed kind antioxidant or phosphoric acid ester antioxidant, the dispersant is that silane is even
Join agent, silane coupling agent is selected from one or more of KH-550, KH-560 and KH-570.
It is preferred that above-mentioned high temperature resistant silicon oil/fat composition, in terms of mass fraction, including following components：75~88 parts of base oil,
6.5~10 parts of organic thickening agent, 0~6.5 part of inorganic thickening agent, 0.25~0.5 part of structural stabilizing agent, 2~5 parts of lubricant resist
1.5~3 parts of 0.25~0.5 part of oxygen agent and dispersant.Further preferably, above-mentioned high temperature resistant silicon oil/fat composition, with mass fraction
Meter, including following components：80 parts of base oil, 6.5 parts of organic thickening agent, 4.5 parts of inorganic thickening agent, 0.5 part of structural stabilizing agent, profit
3 parts of 5 parts of lubrication prescription, 0.5 part of antioxidant and dispersant.
Another object of the present invention is to provide a kind of preparation method of above-mentioned high temperature resistant silicon oil/fat composition, including it is as follows
Step：
(1) base oil for taking 70~90 mass parts is warming up to 125 DEG C~135 DEG C, keeps the temperature 1~3h；
(2) organic thickening agent of 1~10 mass parts of addition in the base oil after being kept the temperature to step (1), 100 DEG C~120 DEG C
1~2h is stirred, the mixture of base oil and thickener is obtained；
(3) sequentially added into the mixture of step (2) base oil and thickener 0.1~2 mass parts antioxidant, 0.1
The dispersant of the structural stabilizing agent of~2 mass parts, the lubricant of 1~10 mass parts and 1~5 mass parts, 80 DEG C~100 DEG C stirrings
1~2h obtains high temperature resistant silicon oil/fat composition semi-finished product；
(4) the high temperature resistant silicon oil/fat composition semi-finished product that step (3) obtains are cooled to 50 DEG C~70 DEG C, 0~10 matter is added
The inorganic thickening agent for measuring part, vacuumizes after being stirred for 0.5~1h, obtains high temperature resistant silicon oil/fat composition.
Unless otherwise indicated, nominal definition of the present invention has is generally understood identical contain with those skilled in the art
Justice.
Compared with prior art, the present invention has the following advantages：
(1) high temperature resistant silicon oil/fat composition proposed by the present invention contacts non-swelling for a long time with silicon rubber and ethylene propylene diene rubber
Or slight swelling, it can ensure cable accessory use steady in a long-term.
(2) mode of the use of the invention based on organic thickening agent, supplemented by inorganic thickening agent is prepared into a kind of novel resistance to
The silicone grease composition of high temperature, the high temperature resistant silicon oil/fat composition have good high temperature resistance, can high temperature resistant reach 150 DEG C,
There is excellent sealing, waterproof, lubrication, chemical stability and electrical insulation capability simultaneously；
(3) high temperature resistant silicon oil/fat composition coating processes proposed by the present invention are simple so that cable accessory replaces succinct, cleaning
It is convenient.
Specific implementation mode：
The following examples are further illustrations of the invention, rather than limiting the invention.
Embodiment 1：
A kind of preparation method of high temperature resistant silicon oil/fat composition, includes the following steps：
(1) polyalphaolefin for taking 75g is warming up to 125 DEG C, keeps the temperature 1h；
(2) mixture of the SB and SEP of 10g are added in the polyalphaolefin after being kept the temperature to step (1), 110 DEG C of stirring 1h are obtained
The mass ratio of the mixture of polyalphaolefin, SB and SEP, wherein SB and SEP is 1:1；
(3) sequentially added into the mixture of step (2) antioxidant 1010 of 0.25g, the ethylene glycol of 0.25g, 5g it is poly-
The KH-550 of tetrafluoroethene micro mist and 3g, 80 DEG C of stirring 1h, obtains high temperature resistant silicon oil/fat composition semi-finished product；
(4) the high temperature resistant silicon oil/fat composition semi-finished product that step (3) obtains are cooled to 50 DEG C, 6.5g gas phase titanium dioxides is added
Silicon stirs 1h, vacuumizes, and obtains high temperature resistant silicon oil/fat composition.
Embodiment 2：
A kind of preparation method of high temperature resistant silicon oil/fat composition, includes the following steps：
(1) dimethicone for taking 88g is warming up to 135 DEG C, keeps the temperature 3h；
(2) mixture of the SEB and SBS of 8g are added in the dimethicone after being kept the temperature to step (1), 120 DEG C are stirred 2h,
The mass ratio of wherein SEB and SBS is 1:1, obtain the mixture of dimethicone and thickener；
(3) sequentially added into the mixture of step (2) antioxidant 1010 of 0.25g, the propylene glycol of 0.25g, 2g it is poly-
The KH-560 of tetrafluoroethene micro mist and 1.5g, 100 DEG C of stirring 2h, obtains high temperature resistant silicon oil/fat composition semi-finished product；
(4) the high temperature resistant silicon oil/fat composition semi-finished product that step (3) obtains are cooled to 70 DEG C, the gas phase dioxy of 6.5g is added
SiClx vacuumizes after being stirred for 1h, obtains high temperature resistant silicon oil/fat composition.
Embodiment 3：
A kind of preparation method of above-mentioned high temperature resistant silicon oil/fat composition, includes the following steps：
(1) polyalphaolefin for taking 80g is warming up to 130 DEG C, keeps the temperature 2h；
(2) to step (1) keep the temperature after polyalphaolefin in be added 6.5g SEPS, 110 DEG C stirring 1.5h, obtain polyalphaolefin and
The mixture of SEPS；
(3) sequentially added into the mixture of step (2) polyalphaolefin and SEPS the antioxidant 1010 of 0.5g, 0.5g third
The KH-570 of triol, the ptfe micropowder of 5g and 3g, 90 DEG C of stirring 1.5h, obtains high temperature resistant silicon oil/fat composition semi-finished product；
(4) the high temperature resistant silicon oil/fat composition semi-finished product that step (3) obtains are cooled to 60 DEG C, the gas phase dioxy of 4.5g is added
SiClx vacuumizes after being stirred for 1h, obtains high temperature resistant silicon oil/fat composition.
Comparative example 1：
A kind of preparation method of high temperature resistant silicon oil/fat composition, includes the following steps：
(1) polyalphaolefin for taking 80g is warming up to 130 DEG C, keeps the temperature 2h；
(2) antioxidant 1010 of 0.5g, the glycerine of 0.5g, 5g are sequentially added in the polyalphaolefin after being kept the temperature to step (1)
Ptfe micropowder and 3g KH-570,90 DEG C stirring 1.5h, obtain silicone grease composition intermediate products；
(3) the silicone grease composition intermediate products that step (2) obtains are cooled to 60 DEG C, the aerosil of 11g are added,
It is vacuumized after being stirred for 1h, obtains silicone grease composition.
Comparative example 2：
A kind of preparation method of above-mentioned high temperature resistant silicon oil/fat composition, includes the following steps：
(1) polyalphaolefin for taking 80g is warming up to 130 DEG C, keeps the temperature 2h；
(2) to step (1) keep the temperature after polyalphaolefin in be added 11g SEPS, 110 DEG C stirring 1.5h, obtain polyalphaolefin and
The mixture of SEPS；
(3) sequentially added into the mixture of step (2) polyalphaolefin and SEPS the antioxidant 1010 of 0.5g, 0.5g third
The KH-570 of triol, the ptfe micropowder of 5g and 3g, 90 DEG C of stirring 1.5h, obtains high temperature resistant silicon oil/fat composition semi-finished product；
(4) the high temperature resistant silicon oil/fat composition semi-finished product that step (3) obtains are cooled to 60 DEG C, vacuumized, obtain high temperature resistant
Silicone grease composition.
High temperature resistant is tested：The silicone grease composition that embodiment 3, comparative example 1 and comparative example 2 are prepared is respectively coated on electricity
On cable end attachment, it is put into baking oven and carries out high temperature resistant test.The heat safe maximum temperature for the silicone grease composition that embodiment 3 obtains is
150 DEG C, the heat safe maximum temperature for the silicone grease composition that comparative example 1 obtains is 120 DEG C, the silicone grease combination that comparative example 2 obtains
The heat safe maximum temperature of object is 110 DEG C.
Embodiment 4：
A kind of preparation method of above-mentioned high temperature resistant silicon oil/fat composition, includes the following steps：
(1) polyalphaolefin for taking 70g is warming up to 125 DEG C, keeps the temperature 1h；
(2) mixture of the SB and SEP of 1g are added in the polyalphaolefin after being kept the temperature to step (1), 100 DEG C of stirring 1h are obtained poly-
The mass ratio of the mixture of alhpa olefin and thickener, wherein SB and SEP is 1:1；
(3) sequentially added into the mixture of step (2) antioxidant 1010 of 0.1g, the ethylene glycol of 0.1g, 1g poly- four
The KH-550 of vinyl fluoride micro mist and 1g, 80 DEG C of stirring 1h, obtains high temperature resistant silicon oil/fat composition semi-finished product；
(4) the high temperature resistant silicon oil/fat composition semi-finished product that step (3) obtains are cooled to 50 DEG C, vacuumized, obtain high temperature resistant
Silicone grease composition.
Embodiment 5：
A kind of preparation method of above-mentioned high temperature resistant silicon oil/fat composition, includes the following steps：
(1) dimethicone for taking 90g is warming up to 135 DEG C, keeps the temperature 3h；
(2) mixture of the SEB and SBS of 10g, 120 DEG C of stirrings are added in the dimethicone after being kept the temperature to step (1)
The mass ratio of 2h, wherein SEB and SBS are 1:1, obtain the mixture of dimethicone and thickener；
(3) polytetrafluoroethyl-ne of the antioxidant 1010 of 2g, the propylene glycol of 2g, 10g are sequentially added into the mixture of step (2)
The KH-560 of alkene micro mist and 5g, 100 DEG C of stirring 2h, obtains high temperature resistant silicon oil/fat composition semi-finished product；
(4) the high temperature resistant silicon oil/fat composition semi-finished product that step (3) obtains are cooled to 70 DEG C, the gas phase dioxy of 10g is added
SiClx vacuumizes after being stirred for 1h, obtains high temperature resistant silicon oil/fat composition.
The silicone grease composition technology that the silicone grease composition that Examples 1 to 3 is prepared is prepared with comparative example 1~2 refers to
Mark comparison is as shown in table 1：
Table 1
Silicone grease composition made from Examples 1 to 3 and comparative example 1~2 is carried out and silicone rubber plate and ethylene propylene diene rubber
Piece does the experiment of the compatibility at 150 DEG C, and steps are as follows with silicone rubber plate and ethylene-propylene-diene monomer film compatibility test：
1) silicone rubber plate vulcanizated and ethylene-propylene-diene monomer film are cut into the identical square of size (5cm × 4cm)；
2) silicone rubber plate cut and ethylene-propylene-diene monomer film are weighed respectively, and has recorded data；
3) silicone grease composition made from Examples 1 to 3 and comparative example 1~2 is uniformly coated in silicone rubber plate and ternary
EP rubbers on piece, coating thickness 1mm, 90% or more coated area, then the silicone rubber plate and ethylene-propylene-diene monomer after coating
Film is put into 150 DEG C of baking ovens and places 7 days (168h), and the silicone rubber plate and ethylene propylene diene rubber after coating are taken out from baking oven after 168h
Piece is cooled to room temperature；
4) the silicone grease wiped clean of the silicone rubber plate and ethylene propylene diene rubber on piece coating after application, observation and silicon rubber
Whether film and ethylene-propylene-diene monomer film appearance and shape deform, then weigh silicone rubber plate and ethylene-propylene-diene monomer after coating respectively
The weight of film.
Test result is as shown in table 2：
Table 2
| Project name | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| With silicon rubber swellability | 0.34 | 0.37 | 0.4 | 2.5 | 2.0 |
| With ethylene-propylene-diene monomer peptization | 2.5 | 1.8 | 4.0 | 18 | 15 |
It is obtained by table 2：Be coated with silicone grease composition made from Examples 1 to 3 with silicone rubber plate and ethylene propylene diene rubber
Piece weightening after 150 DEG C of baking ovens place 168h is less than 5%, and appearance is unchanged, shape invariance shape.Test result shows that this is resistance to
The physical and chemical properties of the various substances of high temperature silicone grease will not change, with silicone rubber plate and ethylene-propylene-diene monomer film compatibility
It is good, it can be used for and end attachment made from silicone rubber plate and ethylene-propylene-diene monomer film.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications etc.
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of novel fire resistant silicone grease composition, which is characterized in that in terms of mass fraction, including following components：Base oil 70
~90 parts, 1~10 part of organic thickening agent, 0~10 part of inorganic thickening agent, 0.1~2 part of structural stabilizing agent, 1~10 part of lubricant,
1~5 part of 0.1~2 part of antioxidant and dispersant, the base oil is selected from plus hydrogen paraffine base crude oil, naphthene base crude oil, polyalphaolefin and
One or more of silicone oil.
2. novel fire resistant silicone grease composition according to claim 1, which is characterized in that the base oil is poly- α alkene
Hydrocarbon or dimethicone.
3. novel fire resistant silicone grease composition according to claim 1 or 2, which is characterized in that the organic thickening agent
Selected from styrene-butadiene, styrene-butadiene/propylene, styrene-butadiene/ethylene, styrene-butadiene-benzene second
Alkene, styrene-ethylene/butylene-styrene, styrene-ethylene/one or more of propylene-styrene and ethylene propylene diene rubber.
4. novel fire resistant silicone grease composition according to claim 1 or 2, which is characterized in that the inorganic thickening agent
For aerosil.
5. novel fire resistant silicone grease composition according to claim 1 or 2, which is characterized in that the structural stabilizing agent
For ethylene glycol, propylene glycol or glycerine.
6. novel fire resistant silicone grease composition according to claim 1 or 2, which is characterized in that the lubricant is poly-
Tetrafluoroethene micro mist.
7. novel fire resistant silicone grease composition according to claim 1 or 2, which is characterized in that the antioxidant be by
Hinder kind antioxidant or phosphoric acid ester antioxidant.
8. novel fire resistant silicone grease composition according to claim 1 or 2, which is characterized in that the dispersant is silicon
Alkane coupling agent.
9. novel fire resistant silicone grease composition according to claim 1 or 2, which is characterized in that in terms of mass fraction, including
Following components：75~88 parts of base oil, 6.5~10 parts of organic thickening agent, 0~6.5 part of inorganic thickening agent, structural stabilizing agent 0.25
~0.5 part, 2~5 parts of lubricant, 1.5~3 parts of 0.25~0.5 part of antioxidant and dispersant.
10. a kind of preparation method of novel fire resistant silicone grease composition as claimed in claim 1 or 2, which is characterized in that including such as
Lower step：
(1) base oil for taking 70~90 mass parts is warming up to 125 DEG C~135 DEG C, heat preservation；
(2) organic thickening agent of 1~10 mass parts is added in the base oil after being kept the temperature to step (1), 100 DEG C~120 DEG C are stirred,
Obtain the mixture of base oil and thickener；
(3) antioxidant, 0.1~2 matter of 0.1~2 mass parts are sequentially added into the mixture of step (2) base oil and thickener
The dispersant of the structural stabilizing agent of part, the lubricant and 1~5 mass parts of 1~10 mass parts is measured, 80 DEG C~100 DEG C stirrings obtain resistance to
High temperature silicone grease composition semi-finished product；
(4) the high temperature resistant silicon oil/fat composition semi-finished product that step (3) obtains are cooled to 50 DEG C~70 DEG C, 0~10 mass parts is added
Inorganic thickening agent, be stirred for uniformly after vacuumize, obtain high temperature resistant silicon oil/fat composition.
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| CN109797027A (en) * | 2019-01-22 | 2019-05-24 | 东莞市港田高分子材料有限公司 | A kind of High Performance Insulation lubricating grease and preparation method thereof |
| CN110499030A (en) * | 2019-09-17 | 2019-11-26 | 昆山纳诺新材料科技有限公司 | A kind of silicone grease high temperature resistant additive and preparation method |
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| US6160939A (en) * | 1999-03-31 | 2000-12-12 | Lucent Technologies Inc. | Optical cable having a filling material with stable viscosity and yield stress |
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| CN110499030A (en) * | 2019-09-17 | 2019-11-26 | 昆山纳诺新材料科技有限公司 | A kind of silicone grease high temperature resistant additive and preparation method |
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| CN108659297B (en) | 2020-08-18 |
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