CN101804991B - Shell porous silicate, preparation method thereof and friction material containing same - Google Patents
Shell porous silicate, preparation method thereof and friction material containing same Download PDFInfo
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- CN101804991B CN101804991B CN2009100103609A CN200910010360A CN101804991B CN 101804991 B CN101804991 B CN 101804991B CN 2009100103609 A CN2009100103609 A CN 2009100103609A CN 200910010360 A CN200910010360 A CN 200910010360A CN 101804991 B CN101804991 B CN 101804991B
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Abstract
The invention discloses silicate of special crystal morphology, in particular a porous spherical material enclosed by closed shells woven by needle-like crystal chopped fibers. The bulk density of the material is 20 to 200g/L, the average size of the material is 1 to 1,000 micrometers, the main ingredient of the material is Ca6Si6O17(OH)2, and the material also contains 1 to 20 weight percent of CaSiO3.H2O. The material of the invention is manufactured by using a calcium compound and a silicon compound as raw materials, wherein the raw materials are uniformly mixed in a mol ratio of Ca<2+> to Si<4+> of 0.8 to 1.2; metal powder and water, which serve as reaction promoters are added into the raw materials; and the hydro-thermal synthesis is performed for 30 to 24 hours in a high-pressure reaction kettle under the conditions of stirring, a temperature rise speed of 0.2 to 3 DEG C/min, a constant temperature of 160 to 280 DEG C and a constant pressure of 6 to 68 Kg/cm<2>, and the product of the reaction is washed, filtered out and dried to give the finished product. The shell porous silicate of the invention has high heat resistance, high wear resistance, little wear and no noises, can be used as the friction material of the braking devices of automobiles, trains and air planes and is the optimal product for substituting asbestos. The material and the preparation process of the invention cause little environmental pollution and are suitable for industrial production.
Description
Technical field
The present invention relates to a kind of silicate of special crystallization shape, the silicate of the porous spherical that the sealing shell that is particularly woven by the needle-like crystal staple fibre surrounds, and the preparation method of the silicate of this special crystallization shape also relate to a kind of friction materials that contains it.
Background technology
Mostly friction materials as brake component was to be dispersed in the asbestos in organic binder bond or the inorganic adhesive in the past.Yet these materials do not possess sufficient thermotolerance and abrasion resistance properties.Unstable like frictional coefficient, wear resistance is relatively poor, and these performances can obviously descend in the high-temperature zone especially, can cause its damage that declines more greatly.When implementing braking, friction materials can cause bigger " brake noise " with contacting of high speed brake(-holder) block.Simultaneously, asbestos are a kind of known carcinogenic substances, and its dust can make operator suck onset.In view of such environmental health problem, the use of asbestos is restricted day by day, presses for the surrogate of development asbestos.
The potassium titanate crystal whisker friction materials that has proposed to use non-carcinogenic is as the friction control agent, and has been used for the brake pad of automobile.Have good sliding capability and braking effect although contain the friction materials of potassium titanate crystal whisker; To the little advantage of friction pair brake(-holder) block damage, but the wear resistance of this material is not enough, especially in the high-temperature zone; The rate of wear is very fast, and can not effectively solve " brake noise ".
In order to address the above problem; The inventor is according to formula material commonly used in the present friction materials; Seek similar basically but the novel isomer that structure is different of composition; Particularly want to produce the light material of hollow structure, and require this material can be high temperature resistant, can keep stable friction factor, abrasion little in friction materials use temperature scope.Because hollow structure comprises many holes, good result must be arranged to the noise abatement noise reduction.Through investigation and experimental study, find can prepare the housing porous spherical silicate of this special crystallization shape with controllable crystallization method, this material light weight, heat-resisting, wear-resisting, frictional behaviour can reach requirement.
About making light body formed material, more existing at present patents are delivered.Introduced the product that under HTHP, obtains through spraying with silicic acid and lime white hydro-thermal reaction like U.S. Pat 3915725 and added caking agent, extrusion forming, drying are prepared the light system article of the sphere aggregates moulding of being twined by the strip crystal; The clear 56-78465 of jp patent publication has introduced the method for manufacture of Calucium Silicate powder formed body, and lime, silicic acid and fibrous material are mixed mutually, and it is dry at high pressure, high temperature vapor condition compacted under to add water, makes goods; Chinese patent ZL200410009902.8 has introduced the super preparation methods in a kind of Calucium Silicate powder composite Nano hole; The hollow secondary particle that has adopted the xonotlite fiber of ultra-fine diameter to form is compound as rigid support skeleton and aerosil; Made bulk, tubulose and watt shape super insulating material product, the strength of materials is increased substantially.But also do not appear in the newspapers about silicate of housing vesicular structure characteristic of the present invention and preparation method thereof.
Summary of the invention
The housing porous silicate that the purpose of this invention is to provide a kind of novelty; This material non-toxic property; Be the material of the feature of environmental protection, when using this material, can improve thermotolerance and abrasion resistance properties, to eliminating " brake noise " positive effect is arranged especially as friction material formulation.The present invention also provides the method for making this material and uses this material to make the friction materials of formula material.
For achieving the above object; After the inventor has carried out going deep into persistent research; The silicate of the housing vesicular structure of the novelty through adopting controllable special crystallization method successfully to obtain to meet above-mentioned requirements, and make prescription with the material of this novel structure and produced and can guarantee thermotolerance and wearability and friction materials that can obvious noise abatement noise reduction.
The constitutional features of this novel materials is the porous globe that has by the sealing shell encirclement of needle-like crystal staple fibre braiding, and tap density is 20～200g/L, and mean sizes is 1～1000 μ m, and its staple is chemical formula Ca
6Si
6O
17(OH)
2, and contain the CaSiO of 1～20wt.%
3.H
2The silicate that O representes.
The invention provides the method for making above-mentioned shell porous silicate, is raw material with calcium containing compound, silicon-containing compound, and adds the reaction promotor metallic silicon power, is obtained by hydro-thermal reaction, it is characterized in that:
---with calcium containing compound and silicon-containing compound is main raw material, Ca
2+: Si
4+Be 0.8～1.2: 1 mol ratio, and the metallic silicon power that adds raw material total amount 0.1～5wt.% therein makes reaction promotor, add an amount of water again, Gu its liquid/than being that 10～100 (weight ratios) are mixed mutually;
---hydro-thermal reaction is at 0.2～3 ℃/min of heat-up rate, 160 ℃～280 ℃ of holding temperatures, pressure 6～68Kg/cm
2Under carry out, be incubated 30 minutes～24 hours, stirring velocity is 20～500rpm.
---the silicate that aforesaid method obtains is after washing, filtering, in oven dry in 120 ℃～280 ℃, 3～20 hours.
The present invention makes in the method for shell porous silicate, and institute's calcium containing compound is one or more of quicklime, calcium hydroxide, lime carbonate, calcium chloride, calcium sulfate.
The present invention makes in the method for shell porous silicate, one or more of institute's silicon-containing compound such as silicon-dioxide, white carbon black, silica sand, silicon ash, silica gel.
The technical characterictic of this method is to have added nucleation reaction promotor metallic silicon power, has adopted suitable heat-up rate, holding temperature, pressure and stirring velocity technology, with controllable special crystallization method, success prepare shell porous silicate.
The present invention also provides a kind of friction materials, is characterized in containing 1～80wt.% shell porous silicate of the present invention.
The friction materials that the silicate that uses the present invention to have the vesicular structure that the special sealing shell by the braiding of needle-like crystal staple fibre surrounds is made; Have good thermotolerance and abrasion resistance properties; Even at life-time service more than tens hours; From the room temperature to high temperature, also can keep stable frictional coefficient, the noise abatement noise reduction has good result during especially to braking.Simultaneously, material of the present invention also has following technological advantage: as in producing the friction materials process, help mixing, moulding process.In whipping process, because shear action, part particle shell will be broken and get in the batching, form the crystal staple fibre and play enhancement; And ground grains does not interact with other food ingredient because porosity is big and infiltration, can improve dispersiveness, eliminates static charge, obviously shortens mixing time, makes mixing reach even rapidly; The premolding effect be can also improve, green strength and good edge forming stability guaranteed.Improved perviousness owing to added the silicate of hollow housing vesicular structure in the prescription; Gas can well be discharged; Thereby reduce surface and matrix internal fissure; Guarantee quality product, and the physical and mechanical properties and the frictional behaviour of friction materials had desirable influence: can under the prerequisite that guarantees mechanical property, make friction materials density lower; Simultaneously; Because the increase of connective pore has improved perviousness; Make gas on frictional contact surface, more be prone to dissipate and obviously increase frictional coefficient, the stability of the frictional behaviour under the assurance temperature variations makes friction materials can not cause that braking effect weakens because of receiving heat fading.More significant advantage is that noise abatement, erasure effect are arranged, and can guarantee the brake comfortableness.Material of the present invention does not contain deleterious chemical ingredients, and is nontoxic, is environmentally friendly machine.
Therefore, use material of the present invention to be specially adapted to make brake component: as be installed in clutch facing, braking liner and the dish pad in the drift stop of automobile, aircraft, train and shop equipment.Be suitable for industrial mass production.
Description of drawings
Fig. 1. the shell porous silicate stereoscan photograph.
Fig. 2. the X-ray diffraction spectrogram of shell porous silicate reaches with standard diagram and compares.
Fig. 3. with the friction materials frictional coefficient and the temperature relation curve of shell porous silicate.
Fig. 4. with the friction materials wear rate of shell porous silicate and the relation curve of temperature.
Embodiment
Through embodiment the present invention is detailed below.
Embodiment 1:
In the autoclave of 5L, put into 3620g water earlier, add silica powder more respectively and (contain SiO
2Account for 98%) 147.8g, unslaked lime (contain CaO and account for 96%) 138g and metallic silicon power (containing more than the Si99%) 2.8g, stirring and evenly mixing, good seal reaction kettle cover is warming up to 200 ℃, pressure 16Kg/cm with 2 ℃/minute rate of heating with still
2Down, be incubated 6 hours, heat up with insulating process in, for preventing the reaction product deposition, blade otherwise stop stirring, stirring velocity is 220rpm, the insulation end stops to heat furnace cooling.Cool off the back and take out product, through washing, filtration, in electric dry oven, dried 8 hours for 120 ℃, obtain white powder 180g, the mensuration bulk density is 86g/L.Through the X-ray diffraction analysis, its staple is chemical formula Ca
6Si
6O
17(OH)
2, and contain 6wt.%CaSiO
3.H
2The silicate compound that O representes, (like Fig. 2).With this product of scanning electron microscopic observation, shape characteristic is that mean sizes is 82 μ m, (like Fig. 1) by the porous spherical thing of the sealing shell encirclement of needle-like crystal staple fibre braiding.
Embodiment 2:
In the autoclave of 5L, put into 3697g water earlier, add silica powder (SiO more respectively
2Account for more than 98%) 53.1g, unslaked lime (CaO purity 96%) 49.6g and metallic silicon power (containing more than the Si99%) 1.0g, stirring and evenly mixing, good seal reaction kettle cover is warming up to 210 ℃ with 1.8 ℃/minute rate of heating with still, pressure 20Kg/cm
2Down, be incubated 6 hours, in intensification and insulating process, blade does not stop to stir, and stirring velocity is 230rpm, and insulation finishes to stop heating, furnace cooling.Product is taken out in cooling back, and through washing, filter, 130 ℃ of dryings are 6 hours in electric oven, obtain white meal 102g, and the mensuration tap density is 110g/L.Through the X-ray diffraction analysis, its staple is chemical formula Ca
6Si
6O
17(OH)
2, and contain 5wt.%CaSiO
3.H
2The silicate that O representes.With this product of scanning electron microscopic observation, shape characteristic is that mean sizes is 65 μ m by the porous spherical thing of the sealing shell encirclement of needle-like crystal staple fibre braiding.
Embodiment 3:
In the autoclave of 5L, put into 3619g water earlier, add SiO more respectively
2(analytical pure) 81g, Ca (OH)
2(analytical pure) 100g and metallic silicon power (containing more than the Si99%) 1.8g, stirring and evenly mixing, good seal reaction kettle cover is warming up to 200 ℃ with 2 ℃/minute rate of heating with still, pressure 16Kg/cm
2Under be incubated 6 hours, heat up with insulating process in, blade does not stop to stir, stirring velocity is 230rpm, insulation finishes to stop to heat furnace cooling.Product is taken out in cooling back, and through washing, filter, 120 ℃ of dryings are 8 hours in electric oven, obtain white meal 157g, and the mensuration tap density is 95g/L.Through the X-ray diffraction analysis, its staple is chemical formula Ca
6Si
6O
17(OH)
2, and contain 6wt.%CaSiO
3.H
2The silicate that O representes.With this product of scanning electron microscopic observation, shape characteristic is that mean sizes is 78 μ m by the porous spherical thing of the sealing shell encirclement of needle-like crystal staple fibre braiding.
Embodiment 4:
In the autoclave of 5L, put into 3697g water earlier, add SiO more respectively
2(analytical pure) 46g, Ca (OH)
2(analytical pure) 56.7g adds metallic silicon power (containing Si more than 99%) 1.0g, stirring and evenly mixing, and good seal reaction kettle cover is warming up to 200 ℃ with 2 ℃/minute rate of heating with still, pressure 16Kg/cm
2Down, be incubated 6 hours, in intensification and insulating process, blade does not stop to stir, and stirring velocity is 230rpm, and insulation finishes to stop heating, furnace cooling.Product is taken out in cooling back, and through washing, filter, 120 ℃ of dryings are 8 hours in electric oven, obtain white meal 88g, and the mensuration tap density is 115g/L.Through the X-ray diffraction analysis, its staple is chemical formula Ca
6Si
6O
17(OH)
2, and contain 5.5wt.%CaSiO
3.H
2The silicate that O representes.With this product of scanning electron microscopic observation, shape characteristic is that mean sizes is 60 μ m by the porous spherical thing of the sealing shell encirclement of needle-like crystal staple fibre braiding.
Embodiment 5:
With embodiment 1 prescription and operation, but, only be incubated 3 hours, then furnace cooling at 200 ℃; All the other operations obtain white meal 175g with embodiment 1, and tap density is 130g/L.Through the X-ray diffraction analysis, its staple is chemical formula Ca
6Si
6O
17(OH)
2, and contain 10wt.%CaSiO
3.H
2The silicate compound that O representes.With this product of scanning electron microscopic observation, shape characteristic is that mean sizes is 36 μ m by the porous spherical thing of the sealing shell encirclement of needle-like crystal staple fibre braiding.
Embodiment 6:
With embodiment 1 prescription and operation, but stirring velocity is 260rpm, obtains white meal 176g, and the mensuration tap density is 102g/L.Through the X-ray diffraction analysis, its staple is chemical formula Ca
6Si
6O
17(OH)
2, and contain 5wt.%CaSiO
3.H
2The silicate compound that O representes.With this product of scanning electron microscopic observation, shape characteristic is that mean sizes is 70 μ m by the porous spherical thing of the sealing shell encirclement of needle-like crystal staple fibre braiding.
Embodiment 7:
With embodiment 3 prescriptions and operation, at 230 ℃, pressure 28Kg/cm
2Down, be incubated 4 hours, furnace cooling then, all the other are operated with embodiment 3, obtain white meal 156g, and the mensuration tap density is 68g/L.Through the X-ray diffraction analysis, its staple is chemical formula Ca
6Si
6O
17(OH)
2, and contain 5wt.%CaSiO
3.H
2The silicate that O representes.With this product of scanning electron microscopic observation, shape characteristic is that mean sizes is 102 μ m by the hole globe of the sealing shell encirclement of needle-like crystal staple fibre braiding.
Embodiment 8 (comparative example)
In the autoclave of 5L, put into 3620g water earlier, add silica powder more respectively and (contain SiO
2Account for 98%) 147.8g, unslaked lime (contain CaO and account for 96%) 138g, but do not add the promoter metals silica flour fully, and stirring and evenly mixing, good seal reaction kettle cover is warming up to 200 ℃, pressure 16Kg/cm with 2 ℃/minute rate of heating with still
2Down, be incubated 6 hours, in intensification and insulating process, blade does not stop to stir, and stirring velocity is 220rpm, and insulation finishes to stop heating, furnace cooling.Cool off the back and take out product, through washing, filtration, in electric dry oven, dried 8 hours for 120 ℃, obtain white powder 192g, the mensuration bulk density is 560g/L.Through the X-ray diffraction analysis, its staple is chemical formula CaSiO
3.H
2O only contains a small amount of Ca
6Si
6O
17(OH)
2With this product of scanning electron microscopic observation, be all the needle-like crystal and the strip crystal of accumulation, do not see housing porous product.It is 3～8 μ m that needle-like crystal is about, wide about 0.5～2 μ m of strip crystal, and length is 5～12 μ m.
Embodiment 9
By weight, the housing porous spherical silicate that obtains among 20 parts of embodiment 1,10 parts of PA tynexs (3 millimeters of average fiber length), 20 parts of resol and 50 parts of permanent white are mixed.This mixture with 28MPa pressure preliminary shaping 1 minute, applies 14MPa pressure in 170 ℃ again and made its combination in 5 minutes under room temperature in mould, 180 ℃ of thermal treatment is 3 hours again.From mould, take out the product that is shaped, process dish pad (JISD 4411 test films).
In making this friction materials process, find to use material of the present invention to help mixing, moulding process.Get in the batching because the shear action of whipping process, part particle shell will be broken, form the crystal staple fibre and play enhancement; Ground grains does not interact with other food ingredient because porosity is big and infiltration, has improved dispersiveness, has eliminated static charge, has obviously shortened mixing time, makes mixing reach even rapidly; Because the silicate that has added the hollow vesicular structure in the prescription has improved ventilation property, gas can well be discharged, reduce surface and matrix internal fissure, assurance test piece quality.
Wearing test
According to " test of automotive friction liner " standard JISD 4411, the dish pad that embodiment 9 is made carries out constant speed wearing test (friction disc Facing material: graphitic cast iron, surface pressure: 1MPa, friction speed: 7 meter per seconds), measure frictional coefficient (μ) and wear rate (10
-7Cm
3/ Kgm).The result is shown in Fig. 3 and Fig. 4.
Visible by figure, this friction materials has high friction coefficient, and receives Influence of Temperature very little, has shown the excellent friction stability; Abrasion loss is little, and also not obvious with temperature rising increase, has good wear resistance.Entire test do not have noise to take place basically, shown the good result of friction materials noise abatement, noise reduction.
Can obviously find out by the foregoing description: with the prepared shell porous silicate of the inventive method heat-resisting good, frictional behaviour is excellent; Stable from low temperature to the high temperature friction coefficient; Little, the noiselessness that weares and teares can be used as drift stop, clutch facing and the brake facing etc. of automobile, train, aircraft, and material of the present invention does not contain deleterious chemical ingredients; Nontoxic, be the environmentally friendly machine that replaces asbestos.By preparation technology provided by the invention, method is easy, with low cost, and non-environmental-pollution is applicable to industrial-scale production.
Industrial application
The invention provides the shell porous silicate that is suitable as friction material formulation.
Friction materials of the present invention contains above-mentioned shell porous silicate, is suitable for doing brake component, as is installed in clutch facing in the drift stop of automobile, aircraft, train and shop equipment, brake facing, braking liner etc.
Claims (4)
1. shell porous silicate, staple is expression formula Ca
6Si
6O
17(OH)
2, and contain the CaSiO of 1～20wt.%
3H
2O;
Its outward appearance is a white powder, and microstructure is that tap density is 20～200g/L by the porous spherical thing of the sealing shell encirclement of needle-like crystal staple fibre braiding, and mean sizes is 1 to 1000 μ m.
2. the preparation method of the said shell porous silicate of claim 1 is a raw material with calcium containing compound, silicon-containing compound, and adds the reaction promotor metallic silicon power, is obtained by hydro-thermal reaction, it is characterized in that:
---with calcium containing compound and silicon-containing compound is main raw material, Ca
2+: Si
4+Be 0.8～1.2: 1 mol ratio, and the metallic silicon power that adds calcium containing compound and two kinds of raw material total amounts of silicon-containing compound, 0.1～5wt.% therein making reaction promotor, add an amount of water again, is 10～100 to mix mutually Gu make its liquid/weight ratio;
---hydro-thermal reaction is at 0.2～3 ℃/min of heat-up rate, 160 ℃～280 ℃ of holding temperatures, pressure 6～68Kg/cm
2Under carry out, be incubated 30 minutes～24 hours, stirring velocity is 20～500rpm;
---the silicate that aforesaid method obtains is after washing, filtering, in oven dry in 120～280 ℃, 3～20 hours;
Said silicon-containing compound is one or more in silicon-dioxide, white carbon black, silica sand, silicon ash, the silica gel.
3. according to the preparation method of the said shell porous silicate of claim 2, it is characterized in that: said calcium containing compound is one or more in quicklime, calcium hydroxide, lime carbonate, calcium chloride, the calcium sulfate.
4. a friction materials is characterized in that: the described shell porous silicate of claim 1 that comprises 1～80wt.% in the friction materials.
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Families Citing this family (8)
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|---|---|---|---|---|
| CN102969489B (en) * | 2012-12-05 | 2016-08-17 | 奇瑞汽车股份有限公司 | A kind of Si-C composite material and preparation method thereof, lithium ion battery containing this material |
| CN104310415B (en) * | 2014-10-13 | 2016-06-22 | 杭州桑拉科技有限公司 | A kind of preparation method of the porous calcium silicate granule of friction resistance material |
| CN104449566B (en) * | 2014-10-31 | 2016-10-05 | 杭州优纳摩擦材料有限公司 | A kind of modified friction particles for friction material and preparation method thereof |
| CN105202084A (en) * | 2015-09-28 | 2015-12-30 | 东营博瑞制动***有限公司 | Little-metal brake pad prepared from calcium hydrate silicate powder |
| PL3538786T3 (en) * | 2016-11-11 | 2023-07-10 | Promat Research And Technology Centre N.V. | Friction material |
| JP2019023255A (en) * | 2017-07-24 | 2019-02-14 | 株式会社アドヴィックス | Dry brake friction material |
| CN115259170B (en) * | 2022-07-15 | 2023-04-25 | 南京工业大学 | Preparation method of porous xonotlite |
| CN115430202B (en) * | 2022-09-06 | 2023-10-27 | 苏州贝林微纤科技有限公司 | Large bulk density paper fiber filter aid and preparation method and application thereof |
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| CN1146441A (en) * | 1996-06-28 | 1997-04-02 | 中国建筑材料科学研究院 | In-situ preparation of microporous hard rankinite thermal-insulation material |
| CN1307083A (en) * | 2000-01-24 | 2001-08-08 | 莱州明发隔热材料有限公司 | Method for mfg. thermal insulation and fireproof calcium silicate material |
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2009
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146441A (en) * | 1996-06-28 | 1997-04-02 | 中国建筑材料科学研究院 | In-situ preparation of microporous hard rankinite thermal-insulation material |
| CN1307083A (en) * | 2000-01-24 | 2001-08-08 | 莱州明发隔热材料有限公司 | Method for mfg. thermal insulation and fireproof calcium silicate material |
Non-Patent Citations (2)
| Title |
|---|
| 李懋强等.超轻微孔硅酸钙绝热材料的显微结构和工艺控制".《硅酸盐学报》.2000,第28卷(第5期),文章1、2、3部分内容，图4、7. |
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