CN105252437A - Cerium and titanium precursor composite resin grinding wheel and preparation method thereof - Google Patents
Cerium and titanium precursor composite resin grinding wheel and preparation method thereof Download PDFInfo
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- CN105252437A CN105252437A CN201510651492.5A CN201510651492A CN105252437A CN 105252437 A CN105252437 A CN 105252437A CN 201510651492 A CN201510651492 A CN 201510651492A CN 105252437 A CN105252437 A CN 105252437A
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Abstract
The invention discloses a cerium and titanium precursor composite resin grinding wheel. The cerium and titanium precursor composite resin grinding wheel is composed of, by weight, 40-50 parts of cerium carbonate octahydrate, 30-40 parts of titanium sulfate, 80-100 parts of 25-28wt% ammonium hydroxide, 1-2 parts of hydrogen peroxide, 570-600 parts of cubic boron nitride (CBN) abrasives, 90-100 parts of phenol, 96-110 parts of 35-40% formaldehyde solution, 5-7 parts of boric acid, 2-6 parts of hexamethylenetetramine, 13-20 parts of phenylamine, 4-7 parts of stearic acid, 10-16 parts of graphite powder and 3-6 parts of calcium oxide. According to the cerium and titanium precursor composite resin grinding wheel, the cerium carbonate octahydrate is used as a cerium source, the titanium sulfate is used as a titanium source, and the hexamethylenetetramine is used as a precipitator, so that composite abrasives are obtained. The abrasives can improve the hardness of the finished grinding wheel and are particularly suitable for chemico-mechanical polishing of silicon wafer thermal oxide layers.
Description
Technical field
The present invention relates to emery wheel technical field, particularly relate to a kind of cerium, titanium precursor compound resin emery wheel and preparation method thereof.
Background technology
Along with automobile, the improving constantly of aircraft uniform velocity, more strict to the requirement of the friction material such as transmission, braking, and matrix is exploitation and the emphasis of research as the important component part of friction material always.Phenolic resins, epoxy resin, butadiene-styrene rubber and polytetrafluoroethylene (PTFE) all can be used as the matrix of friction material, but epoxy resin, butadiene-styrene rubber and polytetrafluoroethylene (PTFE) limit its application in friction material due to poor anti-wear performance, heat resistance and bond performance.The advantage of phenolic resins in heat resistance, bond performance, mechanical property, moulding processability and cost etc., becomes the most frequently used adhesive matrix material of composite friction material.But the defects such as when pure phenolic resin exists that fragility is large, poor toughness, hardness are high, heat resistance is not enough, intensity is low and use noise is large, extreme influence Properties of Friction Materials, therefore, carrying out modification to phenolic resins is the effective ways improving its combination property.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of cerium, titanium precursor compound resin emery wheel and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of cerium, titanium precursor compound resin emery wheel, it is made up of the raw material of following weight parts:
Eight aqueous carbonate cerium 40-50, titanium sulfate 30-40,25-28wt% ammoniacal liquor 80-100, hydrogen peroxide 1-2, CBN abrasive material 570-600, phenol 90-100,35-40% formalin 96-110, boric acid 5-7, hexamethylenetetramine 2-6, aniline 13-20, stearic acid 4-7, graphite powder 10-16, calcium oxide 3-6.
Described cerium, a preparation method for titanium precursor compound resin emery wheel, comprise the following steps:
(1) by above-mentioned, eight aqueous carbonate ceriums, titanium sulfate, 25-28wt% ammoniacal liquor are mixed, add hydrogen peroxide, stir, add agate ball according to ratio of grinding media to material 4-5:1,200-300 rev/min of ball milling 3-4 hour, ball milling product obtains cerium, titanium oxide presoma after press filtration, washing, oven dry;
(2) above-mentioned calcium oxide is joined in 16-20 times of water, be elevated to 60-70 DEG C, add graphite powder, insulated and stirred 10-20 minute, add cerium, titanium oxide presoma, at 90-100 DEG C, be heated with stirring to water do, at 860-900 DEG C, calcine 120-130 minute, naturally cool to normal temperature, with CBN abrasive material, ball milling is even, obtains abrasive compound;
(3) 70-75% of 68-75%, 35-40% formalin weight of above-mentioned phenol weight is mixed, stir, add NaOH, adjustment PH is 8-9, and raised temperature is 70-75 DEG C, insulated and stirred 1.6-2 hour, add boric acid, raised temperature is 110-120 DEG C, decompression dehydration 50-60 minute, add the absolute ethyl alcohol of mixed system weight 2-3%, stir, first at 80-90 DEG C, heat 8-10 hour, then at 110-115 DEG C, heat 8-9 hour, cooling, obtains boric acid phenolic resins;
(4) by above-mentioned hexamethylenetetramine, the mixing of boric acid phenolic resins, wear into fine powder, cross 160-200 mesh sieve, obtain boric acid phenol-formaldehyde resin powder;
(5) by remaining phenol, the mixing of 35-40% formalin, add mixed liquor weight 1-1.5 butanone doubly, stir, be heated to 80-85 DEG C, drip aniline, insulation reaction 4-6 hour at the temperature disclosed above after dropwising, heating decompression distillation to system temperature is 100-105 DEG C, cooling, obtains benzoxazine monomer;
(6) by above-mentioned boric acid phenol-formaldehyde resin powder, the mixing of benzoxazine monomer, join in compound weight 2-3 butanone doubly, stirring and dissolving, vacuum drying 2.6-3 hour at 76-80 DEG C, concentrated, be cured under following intensification system, described intensification system is: 80-90 DEG C, 50-60 minute; 100-110 DEG C, 100-120 minute; 130-140 DEG C, 40-50 minute are benzoxazine phenol-formaldehyde resin modified;
(7) above-mentioned benzoxazine phenol-formaldehyde resin modified, abrasive compound are mixed with each raw material of residue, stir, hot-forming, described hot pressing temperature is 160-170 DEG C, pressure 39O-410T, hot pressing time are 30-32 minute, and in hot pressing, every 4-5 minute steam bleeding once;
(8) by above-mentioned hot-forming after resin grinding wheels thickness closed assembly according to demand get up, separate with sheet iron plate, put into the hardening furnace preset and harden, the intensification system of sclerosis is: 100-120 DEG C, 4-5 hour; 125-140 DEG C, 7-8 hour; 150-170 DEG C, 1-2 hour; 180-185 DEG C, 8-9 hour; Naturally cool after stopping heating, obtain described resin wheel.
Advantage of the present invention is:
Emery wheel of the present invention has good heat endurance, and this is owing to introducing benzoxazine resin in phenolic cure structure, and it is a kind of containing phenyl ring and the heteroatomic dicyclic compound of N, O, so heat endurance is strong;
Wheel hardness of the present invention is high, and this is owing to adding benzoxazine monomer, and in its hot pressing at emery wheel and hardening process, volatile substances is few, reduces the porosity of emery wheel, improves compactness and hardness;
Emery wheel revolving strength of the present invention is high, and this is that emery wheel after hardening volume contraction is little owing to adding benzoxazine monomer, decreases internal stress and micro-crack;
The present invention introduces boron at emery wheel in phenolic resins, improve the combination property of finished product, this is because phenolic resins is to connect phenyl ring by C-C key, and boron bakelite resin is by B-" key connects phenyl ring; wherein the bond energy of C-C is the bond energy of 347KJ/mol, B-O is 523KJ/mol, far above the bond energy of C-C; define the three-dimensional cross-linked structure of boracic, can significantly improve the heat resistance of emery wheel, instantaneous heat-resisting quantity, ablation resistance;
The present invention adopts eight aqueous carbonate ceriums to be cerium source, and titanium sulfate is titanium source, and hexa is precipitating reagent, obtains abrasive compound, and this abrasive material can improve the hardness of finished product emery wheel, is specially adapted to the chemically mechanical polishing of silicon wafer thermal oxide layer.
Detailed description of the invention
A kind of cerium, titanium precursor compound resin emery wheel, it is made up of the raw material of following weight parts:
Eight aqueous carbonate ceriums 40, titanium sulfate 30,25wt% ammoniacal liquor 80, hydrogen peroxide 1, CBN abrasive material 570, phenol 90,35% formalin 96, boric acid 5, hexamethylenetetramine 2, aniline 13, stearic acid 4, graphite powder 10, calcium oxide 3.
Described cerium, a preparation method for titanium precursor compound resin emery wheel, comprise the following steps:
(1) by above-mentioned, eight aqueous carbonate ceriums, titanium sulfate, 25wt% ammoniacal liquor are mixed, add hydrogen peroxide, stir, add agate ball according to ratio of grinding media to material 4:1,200 revs/min of ball millings 3 hours, ball milling product obtains cerium, titanium oxide presoma after press filtration, washing, oven dry;
(2) above-mentioned calcium oxide is joined in 16 times of water, be elevated to 60 DEG C, add graphite powder, insulated and stirred 10 minutes, add cerium, titanium oxide presoma, at 90 DEG C, be heated with stirring to water do, calcine 120 minutes at 860 DEG C, naturally cool to normal temperature, with CBN abrasive material, ball milling is even, obtains abrasive compound;
(3) mix 70% of 68%, 35% formalin weight of above-mentioned phenol weight, stir, add NaOH, regulate PH to be 8, raised temperature is 70 DEG C, insulated and stirred 1.6 hours, add boric acid, raised temperature is 110 DEG C, decompression dehydration 50 minutes, add the absolute ethyl alcohol of mixed system weight 2%, stir, first heat 8 hours at 80 DEG C, then heat 8 hours at 110 DEG C, cooling, obtains boric acid phenolic resins;
(4) by above-mentioned hexamethylenetetramine, the mixing of boric acid phenolic resins, wear into fine powder, cross 160 mesh sieves, obtain boric acid phenol-formaldehyde resin powder;
(5) by remaining phenol, 35% formalin mixing, add the butanone of mixed liquor weight 1 times, stir, be heated to 80 DEG C, drip aniline, insulation reaction 4 hours at the temperature disclosed above after dropwising, heating decompression distillation to system temperature is 100 DEG C, and cooling, obtains benzoxazine monomer;
(6) by above-mentioned boric acid phenol-formaldehyde resin powder, the mixing of benzoxazine monomer, join in the butanone of compound weight 2 times, stirring and dissolving, vacuum drying 2.6 hours at 76 DEG C, concentrated, be cured under following intensification system, described intensification system is: 80 DEG C, 50 minutes; 100 DEG C, 100 minutes; 130 DEG C, 40 minutes is benzoxazine phenol-formaldehyde resin modified;
(7) above-mentioned benzoxazine phenol-formaldehyde resin modified, abrasive compound are mixed with each raw material of residue, stir, hot-forming, described hot pressing temperature is 160 DEG C, pressure 39OT, hot pressing time be 30 minutes, in hot pressing, every 4 minutes steam bleedings once;
(8) by above-mentioned hot-forming after resin grinding wheels thickness closed assembly according to demand get up, separate with sheet iron plate, put into the hardening furnace preset and harden, the intensification system of sclerosis is: 100 DEG C, 4 hours; 125 DEG C, 7 hours; 150 DEG C, 1 hour; 180 DEG C, 8 hours; Naturally cool after stopping heating, obtain described resin wheel.
Performance test:
Heat decomposition temperature: >=420 DEG C;
Revolving strength 146m/s;
Abrasion test: with commercially available phenolic resins emery wheel and the emery wheel of the present invention of identical weight, same size, weight is 1kg, cut channel-section steel continuously in the same way respectively, emery wheel weight after commercially available phenol resin sand wheel cutting is 973g, weight after emery wheel cutting of the present invention is 984g, wear away little, durability is high.
Claims (2)
1. cerium, a titanium precursor compound resin emery wheel, is characterized in that what it was made up of the raw material of following weight parts:
Eight aqueous carbonate cerium 40-50, titanium sulfate 30-40,25-28wt% ammoniacal liquor 80-100, hydrogen peroxide 1-2, CBN abrasive material 570-600, phenol 90-100,35-40% formalin 96-110, boric acid 5-7, hexamethylenetetramine 2-6, aniline 13-20, stearic acid 4-7, graphite powder 10-16, calcium oxide 3-6.
2. a preparation method for cerium as claimed in claim 1, titanium precursor compound resin emery wheel, is characterized in that comprising the following steps:
(1) by above-mentioned, eight aqueous carbonate ceriums, titanium sulfate, 25-28wt% ammoniacal liquor are mixed, add hydrogen peroxide, stir, add agate ball according to ratio of grinding media to material 4-5:1,200-300 rev/min of ball milling 3-4 hour, ball milling product obtains cerium, titanium oxide presoma after press filtration, washing, oven dry;
(2) above-mentioned calcium oxide is joined in 16-20 times of water, be elevated to 60-70 DEG C, add graphite powder, insulated and stirred 10-20 minute, add cerium, titanium oxide presoma, at 90-100 DEG C, be heated with stirring to water do, at 860-900 DEG C, calcine 120-130 minute, naturally cool to normal temperature, with CBN abrasive material, ball milling is even, obtains abrasive compound;
(3) 70-75% of 68-75%, 35-40% formalin weight of above-mentioned phenol weight is mixed, stir, add NaOH, adjustment PH is 8-9, and raised temperature is 70-75 DEG C, insulated and stirred 1.6-2 hour, add boric acid, raised temperature is 110-120 DEG C, decompression dehydration 50-60 minute, add the absolute ethyl alcohol of mixed system weight 2-3%, stir, first at 80-90 DEG C, heat 8-10 hour, then at 110-115 DEG C, heat 8-9 hour, cooling, obtains boric acid phenolic resins;
(4) by above-mentioned hexamethylenetetramine, the mixing of boric acid phenolic resins, wear into fine powder, cross 160-200 mesh sieve, obtain boric acid phenol-formaldehyde resin powder;
(5) by remaining phenol, the mixing of 35-40% formalin, add mixed liquor weight 1-1.5 butanone doubly, stir, be heated to 80-85 DEG C, drip aniline, insulation reaction 4-6 hour at the temperature disclosed above after dropwising, heating decompression distillation to system temperature is 100-105 DEG C, cooling, obtains benzoxazine monomer;
(6) by above-mentioned boric acid phenol-formaldehyde resin powder, the mixing of benzoxazine monomer, join in compound weight 2-3 butanone doubly, stirring and dissolving, vacuum drying 2.6-3 hour at 76-80 DEG C, concentrated, be cured under following intensification system, described intensification system is: 80-90 DEG C, 50-60 minute; 100-110 DEG C, 100-120 minute; 130-140 DEG C, 40-50 minute are benzoxazine phenol-formaldehyde resin modified;
(7) above-mentioned benzoxazine phenol-formaldehyde resin modified, abrasive compound are mixed with each raw material of residue, stir, hot-forming, described hot pressing temperature is 160-170 DEG C, pressure 39O-410T, hot pressing time are 30-32 minute, and in hot pressing, every 4-5 minute steam bleeding once;
(8) by above-mentioned hot-forming after resin grinding wheels thickness closed assembly according to demand get up, separate with sheet iron plate, put into the hardening furnace preset and harden, the intensification system of sclerosis is: 100-120 DEG C, 4-5 hour; 125-140 DEG C, 7-8 hour; 150-170 DEG C, 1-2 hour; 180-185 DEG C, 8-9 hour; Naturally cool after stopping heating, obtain described resin wheel.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108972386A (en) * | 2018-05-30 | 2018-12-11 | 安徽佑开科技有限公司 | A kind of modified zirconia silicon rubber phenolic resin grinding wheel and preparation method thereof |
| CN108972367A (en) * | 2018-05-30 | 2018-12-11 | 安徽佑开科技有限公司 | A kind of modified zirconia resin wheel and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108972386A (en) * | 2018-05-30 | 2018-12-11 | 安徽佑开科技有限公司 | A kind of modified zirconia silicon rubber phenolic resin grinding wheel and preparation method thereof |
| CN108972367A (en) * | 2018-05-30 | 2018-12-11 | 安徽佑开科技有限公司 | A kind of modified zirconia resin wheel and preparation method thereof |
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