CN101085854A - Preparation method for inorganic nano material modified phenolic resins - Google Patents

Preparation method for inorganic nano material modified phenolic resins Download PDF

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CN101085854A
CN101085854A CN 200710052004 CN200710052004A CN101085854A CN 101085854 A CN101085854 A CN 101085854A CN 200710052004 CN200710052004 CN 200710052004 CN 200710052004 A CN200710052004 A CN 200710052004A CN 101085854 A CN101085854 A CN 101085854A
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resol
resin
qualified
preparation
coupling agent
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CN100513480C (en
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史宝平
孙振亚
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WUHAN HIGH BALANCE COMPOSITE MATERIAL CO Ltd
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WUHAN HIGH BALANCE COMPOSITE MATERIAL CO Ltd
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Abstract

The invention relates to a method for preparing inorganic nanometer modified formaldehyde-phenol resin. It comprises following steps: (1) mixing inorganic nanometer material into organic surface activator; (2) adding treated inorganic nanometer material in step (1) during formaldehyde-phenol resin synthesizing process or after organic synthesizing, stirring to mix inorganic material and formaldehyde-phenol resin thoroughly; (3)dewatering mixed formaldehyde-phenol resin and drying and getting solid lump resin, grinding said lump resin with ball grinder into particles with size being 400- 600 order, adding resin micro- particle demolding agent and hexamethylenetetramine solidifying agent during grinding process. The product is characterized by improved high- temperature resistant property, reduced heat expansion rate, increased size stabilizing property and mechanical strength for products when said product is used as binding agent.

Description

The preparation method of inorganic nano material modified phenolic resins
Technical field
The present invention is mainly used in brake friction material, and industry such as resin wheel grinding tool, engineering plastics, electric light source, fire-resistant and casting is specifically related to a kind of preparation method of inorganic nano material modified phenolic resins.
Background technology
It is serious etc. that common resol self exists the inherent shortcoming such as property is crisp, hardness is big, poor toughness, not alkaline-resisting, non-stop run temperature surpass 350 degree thermolysiss.As use common resol or organically-modified resol to make products such as type high performance disc brake material or heavy loading resin wheel, and the decline of friction materials high temperature friction coefficient is big or the emery wheel revolving strength is low, and work-ing life is short.In recent years for adapting to the requirement of premium quality product and leading-edge field, in the production development and application of resol and plastics, common resol the organic of multiple technologies and inorganic chemistry modification have been carried out, at aspects such as turnout, quality and new variety development is faster arranged all, multiple high performance modified phenolic resin fat prod is come out one after another.As modified rubbers such as boron modification, organic-silicon-modified, Ding Qing etc., inorganic and organically-modified resol etc., they differ from one another.As one of three big thermosetting resins traditional material--modified phenolic resins is being opened up new application more widely, shows bright development prospect.But general inorganic modified resol such as boron, silicon modification price are too high, are difficult to be applied to industries such as general friction materials, grinding tool, though and organically-modified phenolic aldehyde fragility improves to some extent, resistance to elevated temperatures and thermal expansion do not improve yet.Use is restricted in the premium quality product field.
Summary of the invention
Purpose of the present invention is in order to overcome the low and big shortcoming of coefficient of thermal expansion of common and organically-modified resol thermotolerance, and provide a kind of preparation method of inorganic nano material modified phenolic resins, the present invention mainly is at high-quality friction material and resin wheel and the preparation method of the ultra-fine powdered resin of developing of an analog thermoplastic, adopt the inorganic rigid nano material of a small amount of high chemical mobility of the surface resol to be carried out modification through dispersion and Combined Machining Technology, the two advantages of polymer and inorganic materials is got up, improve the resistance to elevated temperatures of resol emphatically, reduce abrasion and coefficient of thermal expansion.
The preparation method of inorganic nano material modified phenolic resins, carry out according to the following steps: (1) inorganic nano material is: get nano silicon oxide 2-4%, aluminum oxide 0-3%, titanium oxide 1-4%, nanoclay 1.5-3%, barium sulfate 2-4% respectively by the per-cent of resol weight, add the 0.02-0.6% organic surface active agent that accounts for the inorganic nano material gross weight and mix standby; (2) behind resol synthetic mesophase stage or end of synthesis, add the inorganic nano material of handling through organic surface active agent of the first step preparation, stir and make nano inorganic material and resol molecule fully compound; (3) abundant compound resol dewatered drying is become the solid block resin, adopting ball mill to be crushed to granularity the solid block resin again is the 400-600 order, adds the resin micro mist particle separant and the hexamethyl tetramine solidifying agent that accounts for the 6-9% of resol weight of the 0.5-2% that accounts for resol weight when pulverizing with ball mill.
Described machine tensio-active agent is silane coupling agent, chelating titanate coupling agent or zirconium class coupling agent, silane coupling agent is that alkyl phenoxy polyoxyethylene methyldiethoxysilane is that hydramine lipid acid titanic acid ester replaces with the JN-54 title with the replacement of JS-D758 title, chelating titanate coupling agent, and zirconium class coupling agent is the methacryloxy zirconium coupling agent.Described resin micro mist particle separant is calcium carbonate superfine powder and/or barium sulfate, and the particle size range of calcium carbonate superfine powder or barium sulfate is the 2-5 micron.
One, improvement in performance
(1) inorganic nano material modified phenolic resins fineness 400-600 order percent of pass is greater than 95%, the fineness height, and specific surface area is big, good fluidity.In wide temperature range, during this resin solidification bonding compound, show good dispersiveness, wettability and rapid reaction.Especially high-temperature stability significantly improves, and obtains favorable mechanical performance and snappiness.The energy stably stored is 10-12 month under the normal temperature.
(2) inorganic nano material modified phenolic resins is as a kind of STUDY ON THE MODIFICATION OF PENOLIC RESIN thing of uniqueness, than organically-modified resol, has good heat-resisting, water-fast, oil resistant and chemical resistance; Having in solidifying the machine-shaping process is difficult for expanding bubbles, and production technique is easy to control, product qualified rate height, the characteristic of finish size good stability.
(3) because the compound synergistic effect of nano redigity particle in the modified resin, when being used as the binding agent of friction materials and products such as resin wheel and large power, electrically light source, have unique hot operation stability, the thermal stability under 400 ℃ significantly improves, and thermal weight loss is 5-7% only generally.Be added on nano material in the resin and form stable friction transfer layer (film) on the brake facing surface when helping to brake, thereby stablize high temperature friction coefficient.As heavy duty and during the express locomotive brake material high temperature friction coefficient more stable, low fading rate is hanged down rate of wear.This specific character is particularly evident under harsh Working environment.
Two, resistance toheat
The resistance toheat analytical results of typical inorganic nanometer modified resol is as follows.Common resol
Figure A20071005200400041
The commercially available trade mark is 2123, and manufacturer is holy well sea, a Shandong Butterworth company.Common 2123 resol through the DTA of nano material composite modified front and back analytic curve comparison diagram as illustrated in fig. 1 and 2.
The TG of comparative analysis 2123 and nano modification resin and DSC curve are adding same amount (7%) hexamethylenetetramine, and the curing reaction temperature of two resins is basic identical, 160-162 ℃ of scope.Among the contrast experiment, about 187 ℃ of the weightless initial temperature of 2123 resins, the starting temperature of the quick catabolic phase of molecular resin is 362.6 ℃;
The weightless initial temperature of resol after the modification is then significantly brought up to about 243 ℃; The starting temperature of the quick catabolic phase of molecular resin is then corresponding to be increased to 394.3 ℃.The peak temperature of the pyrolysis of DSC is brought up to 652 ℃ of resol after the modification by 587 ℃ of 2123 resins.
The hot analytical parameters representative value of inorganic nanometer modified rosin products sees Table 1.
The inorganic nanometer modified phenolic resin heat analytical parameters of table 1 representative value
Product specification Weightless 10% temperature of TG Weightless 25% temperature The DSC exothermic peak temperature
The nano modification resin 400-470℃ 535-580℃ 660-700℃
The present invention adopts the preparation method of nano inorganic material-modified resol, has obviously improved the resistance to elevated temperatures of resin and has reduced coefficient of thermal expansion, has improved the dimensional stability and the physical strength of goods when using as binding agent.
Description of drawings
Fig. 1 is the thermal weight loss of 2123 resol and heat differential calorimetric (TG-DSC) graphic representation of becoming estranged.
Fig. 2 is the thermal weight loss of inorganic nano material modified phenolic resins (62206) and heat differential calorimetric (TG-DSC) graphic representation of becoming estranged.
Embodiment
Table 2. is embodiment 1～4 raw materials used and amounts among the inorganic nano material modified phenolic resins preparation method of the present invention, and used common 2123 resol are that holy well sea, Shandong Butterworth company produces.
Raw materials used and amount unit: the g of embodiment 1-4 among the table 2 inorganic nano material modified phenolic resins preparation method
Inorganic nano material Organic surface active agent Resol Separant The hexamethyl tetramine
Silicon oxide Aluminum oxide Titanium oxide Clay Barium sulfate JS-D7 58 JN-54 The methacryloxy zirconium coupling agent Common 2123 resol Lime carbonate Barium sulfate
Embodiment 1 2.35 0 1.18 1.77 1.18 0.035 100.0 0.5 9.0
Embodiment 2 3.07 1.23 2.45 3.00 2.45 0.018 100.0 1.2 8.6
Embodiment 3 2.49 2.49 3.11 2.49 4.00 0.025 100.0 1.9 8.0
Embodiment 4 3.85 1.92 4.00 3.00 2.56 0.023 100.0 1.0 1.0 9.0
The preparation method of inorganic nano material modified phenolic resins, each amount of substance is got by the amount in the table 2 respectively, carries out according to the following steps: (1) adds organic surface active agent with inorganic nano material and mixes standby; (2) after also can there be end of synthesis in the resol synthetic mesophase stage, add the inorganic nano material of handling through organic surface active agent of the first step preparation, stir and make nano inorganic material and resol molecule fully compound; (3) abundant compound resol dewatered drying is become the solid block resin, adopting ball mill to be crushed to granularity the solid block resin again is the 400-600 order, adds resin micro mist particle separant and hexamethyl tetramine solidifying agent when pulverizing with ball mill.
The inorganic nano material modified phenolic resins of making of embodiment 2 is tested below.
One, is used for the 160Km/h brake block for high-speed train as the friction materials binding agent, during same recipe and the experimental result of unmodified common 2123 resins contrast, sees Table 3 and 4.Second time of the modified resin brake facing and the 3rd time wear rate are then then lower with respect to unmodified common 2123 resin synthetic brake linings.
Table 3: the synthetic brake lining of kind logical resol is used for the synthetic brake lining constant speed frictional behaviour test result of quasi high-speed passenger vehicle disc type
Warm ℃ of dish Frictional coefficient (μ) Wear rate (X10 -7cm 3/N.m)
Heat up for the first time Cooling for the first time Heat up for the second time Cooling for the second time For the first time
100 0.44 0.40 0.40 0.35 0.26
150 0.48 0.41 0.42 0.36 0.28
200 0.53 0.43 0.46 0.37 0.32
250 0.48 0.42 0.44 0.34 0.62
300 0.44 0.39 0.37 0.32 1.14
350 0.36 0.30
The inorganic nano material modified resin of table 4 synthesizes quasi high-speed passenger vehicle disc type brake lining constant speed frictional behaviour test result
Warm ℃ of dish Frictional coefficient (μ) Wear rate (X10 -7cm 3/N.m)
Heat up for the first time Cooling for the first time Heat up for the second time Cooling for the second time For the first time
100 0.42 0.40 0.43 0.41 0.18
150 0.46 0.42 0.47 0.35 0.19
200 0.48 0.41 0.46 0.37 0.13
250 0.46 0.41 0.43 0.38 0.22
300 0.41 0.40 0.41 0.37 0.37
350 0.38 0.37
Two, the platform experiment comparing result that is used for the car disc brake pad reflects that it once and aspect double-dip recession rate and secondary, three usefulness remarkable improvement being arranged, specifically sees the following form.
QC/T 582-1999 rig test result 1
Unmodified 2123 resol of same recipe and technology synthesize the disc type sheet
Sequence number Project Performance index Test-results The result judges
1#
1 Usefulness (before the break-in) for the first time V＝50km/h p＝Pmax j≥6.1m/s 2 6.35 Qualified
k≥0.75 0.77 Qualified
V＝100km/h p＝Pmax j≥5.2m/s 2 8.25 Qualified
k≥0.55 0.72 Qualified
2 Usefulness (after the break-in) for the second time V＝50km/h p＝Pmax j≥7.8m/s2 7.31 Defective
k≥0.75 0.76 Qualified
V＝100km/h p＝Pmax j≥6.8m/s 2 8.76 Qualified
k≥0.65 0.73 Qualified
V＝130km/h p＝Pmax j≥6.1m/s 2 7.58 Qualified
k≥0.60 0.72 Qualified
Obtain 7.8m/s at V=50km/h 2Respective line pressure under V＝100km/h j≥6.4m/s2 8.25 Qualified
V＝130km/h j≥5.5m/s2 7.2 39.5 Qualified
3 Heat fading for the first time and recovery test V＝100km/h，j＝4.5m/s 2, fading rate≤40% of the 4th braking moment
V=50km/h recovers test arresting retarded velocity 〉=1.5m/s for the first time 2 2.61 Qualified
V=50km/h recovers the last arresting braking moment of test and compares its rate≤23% with the braking moment of reference test 17.2 Qualified
4 Heat fading for the second time and recovery test V＝100km/h，j＝4.5m/s 2, fading rate≤40% of the 8th braking moment 38.6 Qualified
V=50km/h recovers test arresting retarded velocity 〉=1.5m/s for the first time 2 2.75 Qualified
V=50km/h recovers the last arresting braking moment of test and compares its rate≤23% with the braking moment of reference test 13.5 Qualified
5 Usefulness for the third time V＝50km/h p＝Pmax j≥7.8m/s 2 8.32 Qualified
k≥0.75 0.76 Qualified
V＝100km/h p＝Pmax j≥6.8m/s 2 8.74 Qualified
k≥0.65 0.725 Qualified
V＝130km/h p＝Pmax j≥6.1m/s 2 8.84 Qualified
k≥0.60 0.715 Qualified
Obtain 7.8m/s at V=50km/h 2Respective line pressure under V＝100km/h j≥6.4m/s2 8.24 Qualified
V＝130km/h j≥5.5m/s2 8.36 Qualified
6 Noise ≤76dB(A) ≤76dB Qualified
7 Abrasion loss (g) 9.2 Qualified
8 The retarding disc working-surface No scoring trace Do not have Qualified
Brake pad Flawless and delamination Do not have Qualified
Brake cylinder No oil leakage phenomenon Do not have Qualified
Annotate: Pmax=10MPa
QC/T 582-1999 rig test result 2
Inorganic nano material modified 2123 resol of same recipe and technology synthesize the disc type sheet
Sequence number Project Performance index Test-results The result judges
1#
1 Usefulness (before the break-in) for the first time V＝50km/h p＝Pmax j≥6.1m/s 2 6.55 Qualified
k≥0.75 0.78 Qualified
V＝100km/h p＝Pmax j≥5.2m/s 2 8.1 Qualified
k≥0.55 0.71 Qualified
2 Usefulness (after the break-in) for the second time V＝50km/h p＝Pmax j≥7.8m/s 2 8.53 Qualified
k≥0.75 0.79 Qualified
V＝100km/h p＝Pmax j≥6.8m/s 2 9.06 Qualified
k≥0.65 0.72 Qualified
V＝130km/h p＝Pmax j≥6.1m/s 2 8.63 Qualified
k≥0.60 0.705 Qualified
Obtain 7.8m/s at V=50km/h 2Respective line pressure under V＝100km/h j≥6.4m/s2 8.3 Qualified
V＝130km/h j≥5.5m/s2 7.9 Qualified
3 Heat fading for the first time and recovery test V＝100km/h，j＝4.5m/s 2, fading rate≤40% of the 4th braking moment 21.4 Qualified
V=50km/h recovers test arresting retarded velocity 〉=1.5m/s for the first time 2 2.91 Qualified
V=50km/h recovers the last arresting braking moment of test and compares its rate≤23% with the braking moment of reference test 13.6 Qualified
4 Heat fading for the second time and recovery test V＝100km/h，j＝4.5m/s 2, fading rate≤40% of the 8th braking moment 33.5 Qualified
V=50km/h recovers test arresting retarded velocity 〉=1.5m/s for the first time 2 2.94 Qualified
V=50km/h recovers the last arresting braking moment of test and compares its rate≤23% with the braking moment of reference test 9.8 Qualified
5 Usefulness for the third time V＝50km/h p＝Pmax j≥7.8m/s 2 8.48 Qualified
k≥0.75 0.77 Qualified
V＝100km/h j≥6.8m/s 2 8.95 Qualified
p＝Pmax k≥0.65 0.735 Qualified
V＝130km/h p＝Pmax j≥6.1m/s 2 8.91 Qualified
k≥0.60 0.726 Qualified
Obtain 7.8m/s at V=50km/h 2Respective line pressure under V＝100km/h j≥6.4m/s2 8.35 Qualified
V＝130km/h j≥5.5m/s2 8.31 Qualified
6 Noise ≤76dB(A) ≤76dB Qualified
7 Brake pads wear amount (g) 8.3 Qualified
8 The retarding disc working-surface No scoring trace Do not have Qualified
Brake pad Flawless and delamination Do not have Qualified
Brake cylinder No oil leakage phenomenon Do not have Qualified
Annotate: Pmax=10MPa

Claims (4)

1, the preparation method of inorganic nano material modified phenolic resins, carry out according to the following steps: (1) inorganic nano material is: get nano silicon oxide 2-4%, aluminum oxide 0-3%, titanium oxide 1-4%, nanoclay 1.5-3%, barium sulfate 2-4% respectively by the per-cent of resol weight, add the 0.02-0.6% organic surface active agent that accounts for the inorganic nano material gross weight and mix standby; (2) behind resol synthetic mesophase stage or end of synthesis, add the inorganic nano material of handling through organic surface active agent of the first step preparation, stir and make nano inorganic material and resol molecule fully compound; (3) abundant compound resol dewatered drying is become the solid block resin, adopting ball mill to be crushed to granularity the solid block resin again is the 400-600 order, adds the resin micro mist particle separant and the hexamethyl tetramine solidifying agent that accounts for the 8-9% of resol weight of the 0.5-2% that accounts for resol weight when pulverizing with ball mill.
2, preparation method according to claim 1, it is characterized in that: described machine tensio-active agent is silane coupling agent, chelating titanate coupling agent or zirconium class coupling agent.
3, preparation method according to claim 2, it is characterized in that: described silane coupling agent is an alkyl phenoxy polyoxyethylene methyldiethoxysilane, the chelating titanate coupling agent is a hydramine lipid acid titanic acid ester, and zirconium class coupling agent is the methacryloxy zirconium coupling agent.
4, preparation method according to claim 1, it is characterized in that: described resin micro mist particle separant is calcium carbonate superfine powder and/or barium sulfate, and particle diameter is the 2-5 micron.
CNB2007100520044A 2007-04-28 2007-04-28 Preparation method for inorganic nano material modified phenolic resins Expired - Fee Related CN100513480C (en)

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CN102330763A (en) * 2011-07-22 2012-01-25 江苏安捷汽车配件有限公司 Nano-material-added car brake block and method for manufacturing same
CN102875961A (en) * 2012-09-20 2013-01-16 常熟市永祥机电有限公司 Preparation method of nanomaterial-filled phenolic composite material
CN102875962A (en) * 2012-09-20 2013-01-16 常熟市永祥机电有限公司 Nanomaterial-filled phenolic composite material
CN103074015A (en) * 2013-01-06 2013-05-01 江苏省华源矿业有限公司 Preparation method of modified phenolic resin adhesive
CN103148138A (en) * 2011-11-17 2013-06-12 舍弗勒技术股份两合公司 Friction and/or sliding lining
CN103450629A (en) * 2012-05-29 2013-12-18 宝钢集团有限公司 Phenolic moulding powder based on flyash modified phenolic resin and preparation method thereof
CN104861415A (en) * 2015-05-07 2015-08-26 芜湖品度电子科技有限公司 High temperature resistant friction resistant pulley material composition for two-dimension code knitting machine and pulley production method
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CN105033166A (en) * 2015-07-06 2015-11-11 安徽三联泵业股份有限公司 Modified pump body casting foundry sand with furan resin loaded with nanosized zeolite
CN105238353A (en) * 2015-11-03 2016-01-13 傅兴琴 Preparation method for mixed abrasive for vessel cleaning and polishing
CN106517138A (en) * 2016-11-11 2017-03-22 中国科学院山西煤炭化学研究所 Preparation method for inorganic nanoparticle in-situ reinforced resin-based foam carbon
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CN102330763A (en) * 2011-07-22 2012-01-25 江苏安捷汽车配件有限公司 Nano-material-added car brake block and method for manufacturing same
CN102330763B (en) * 2011-07-22 2013-09-25 江苏安捷汽车配件有限公司 Nano-material-added car brake block and method for manufacturing same
CN103148138A (en) * 2011-11-17 2013-06-12 舍弗勒技术股份两合公司 Friction and/or sliding lining
CN103450629A (en) * 2012-05-29 2013-12-18 宝钢集团有限公司 Phenolic moulding powder based on flyash modified phenolic resin and preparation method thereof
CN102875962A (en) * 2012-09-20 2013-01-16 常熟市永祥机电有限公司 Nanomaterial-filled phenolic composite material
CN102875961B (en) * 2012-09-20 2013-10-30 常熟市永祥机电有限公司 Preparation method of nanomaterial-filled phenolic composite material
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CN102875961A (en) * 2012-09-20 2013-01-16 常熟市永祥机电有限公司 Preparation method of nanomaterial-filled phenolic composite material
CN103074015A (en) * 2013-01-06 2013-05-01 江苏省华源矿业有限公司 Preparation method of modified phenolic resin adhesive
CN103074015B (en) * 2013-01-06 2014-02-12 江苏省华源矿业有限公司 Preparation method of modified phenolic resin adhesive
CN104861415A (en) * 2015-05-07 2015-08-26 芜湖品度电子科技有限公司 High temperature resistant friction resistant pulley material composition for two-dimension code knitting machine and pulley production method
CN105033166A (en) * 2015-07-06 2015-11-11 安徽三联泵业股份有限公司 Modified pump body casting foundry sand with furan resin loaded with nanosized zeolite
CN104987657A (en) * 2015-07-31 2015-10-21 武汉理工大学 Anti-wear nano-material modified phenolic resin and preparation method therefor
CN105238353A (en) * 2015-11-03 2016-01-13 傅兴琴 Preparation method for mixed abrasive for vessel cleaning and polishing
CN106517138A (en) * 2016-11-11 2017-03-22 中国科学院山西煤炭化学研究所 Preparation method for inorganic nanoparticle in-situ reinforced resin-based foam carbon
CN114773777A (en) * 2022-05-26 2022-07-22 江西华伍制动器股份有限公司 Preparation method of resin-based composite material added with rare earth oxide and nano silicon dioxide

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