CN116376216B - Preparation method of phenolic resin molding material for commutator - Google Patents
Preparation method of phenolic resin molding material for commutator Download PDFInfo
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- CN116376216B CN116376216B CN202310325594.2A CN202310325594A CN116376216B CN 116376216 B CN116376216 B CN 116376216B CN 202310325594 A CN202310325594 A CN 202310325594A CN 116376216 B CN116376216 B CN 116376216B
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- phenolic resin
- molding material
- resin molding
- aniline
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- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 192
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 189
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 239000012778 molding material Substances 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 13
- 239000011707 mineral Substances 0.000 claims abstract description 13
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 34
- 239000002245 particle Substances 0.000 claims description 29
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 22
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 11
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 11
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 11
- 229960004889 salicylic acid Drugs 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 8
- 239000003365 glass fiber Substances 0.000 claims description 8
- 238000007885 magnetic separation Methods 0.000 claims description 8
- 229920006231 aramid fiber Polymers 0.000 claims description 7
- 239000010445 mica Substances 0.000 claims description 7
- 229910052618 mica group Inorganic materials 0.000 claims description 7
- 229920002748 Basalt fiber Polymers 0.000 claims description 6
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 6
- 238000004898 kneading Methods 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 27
- 238000004132 cross linking Methods 0.000 description 14
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 12
- 239000000126 substance Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 229960004011 methenamine Drugs 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 230000002035 prolonged effect Effects 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229940039407 aniline Drugs 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000006068 polycondensation reaction Methods 0.000 description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 239000004246 zinc acetate Substances 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 210000004400 mucous membrane Anatomy 0.000 description 2
- -1 phenol aldehyde Chemical class 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- CQRYARSYNCAZFO-UHFFFAOYSA-N salicyl alcohol Chemical compound OCC1=CC=CC=C1O CQRYARSYNCAZFO-UHFFFAOYSA-N 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010456 wollastonite Substances 0.000 description 2
- 229910052882 wollastonite Inorganic materials 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 235000010585 Ammi visnaga Nutrition 0.000 description 1
- 244000153158 Ammi visnaga Species 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000629 Rh alloy Inorganic materials 0.000 description 1
- 101000809488 Starmerella bombicola UDP-glucosyltransferase B1 Proteins 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- FNYYWLDEYHKLEG-UHFFFAOYSA-N aniline;formaldehyde;phenol Chemical compound O=C.NC1=CC=CC=C1.OC1=CC=CC=C1 FNYYWLDEYHKLEG-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007336 electrophilic substitution reaction Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006148 magnetic separator Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- DQLGIONSPPKALA-UHFFFAOYSA-N phenylazanium;phenoxide Chemical compound NC1=CC=CC=C1.OC1=CC=CC=C1 DQLGIONSPPKALA-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/22—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The application relates to a preparation method of a phenolic resin molding material for a commutator, which relates to the technical field of high polymer materials, and the phenolic resin molding material comprises the following raw materials in parts by weight: 10-30 parts of high-ortho phenolic resin, 5-20 parts of aniline-phenolic resin, 1-4 parts of curing agent, 40-50 parts of reinforcing agent and 15-30 parts of mineral powder; wherein the content of the curing agent accounts for 8-15% of the total mass of the high ortho phenolic resin and the aniline-phenolic resin. The application prepares the phenolic resin molding material by combining the high ortho phenolic resin and the aniline-phenolic resin, can further accelerate the curing speed of the phenolic resin, shortens the curing time and improves the production efficiency.
Description
Technical Field
The application relates to the technical field of high polymer materials, in particular to a preparation method of a phenolic resin molding material for a commutator.
Background
Phenolic resin is colorless or yellow brown transparent matter, is prepared through polycondensation of phenol aldehyde or its derivative, and has weak acid and weak base resistance, strong acid decomposition, strong alkali corrosion, water insolubility, and dissolving in organic solvent, such as acetone, alcohol, etc. The phenolic resin has good mechanical property and heat resistance, and is widely applied to the industries of anti-corrosion engineering, adhesive, flame-retardant materials, grinding wheel manufacturing and the like.
The shaping material made of phenolic resin as base material is called phenolic plastic, is the most important thermosetting plastic, and is widely used as electric insulating material, furniture parts, daily necessities, artware, etc. The applied products are different, so that the performance requirements on the phenolic resin molding material are different, for example, the phenolic resin molding material applied to electronic elements has higher requirements on the curing speed, the temperature and the like. The curing speed of the phenolic resin molding material affects the performance and production efficiency of the product.
Commutators are an important component of electronic components, also known as commutators, on the armature of dc and ac commutators. In a dc motor, ac power in an armature winding is converted into dc power between brushes by brushes and a commutator. The phenolic resin molding material for the commutator needs to have excellent insulativity while ensuring high performance, and the phenolic resin molding material on the market at present has different insulativity due to different components, has poor insulativity and can conduct electricity, and can not meet the requirements of the commutator.
In addition, the curing speed of the currently used phenolic resin molding material is generally between 90s and 120s, the condition of mucous membrane is easy to generate during mold molding, the integrity of the phenolic resin molding material is reduced due to the fact that the curing speed is too low, the deformation and stress of a product are large, and the mechanical property and the production efficiency of the product are reduced.
Disclosure of Invention
The application provides a preparation method of a phenolic resin molding material for a commutator, which can further accelerate the curing speed of the phenolic resin molding material, reduce the condition of mucous membrane during mold molding, improve the integrity of the molding material, reduce the deformation and stress of the molding material, improve the production efficiency and be better suitable for products such as the commutator under the condition of improving the mechanical property and the insulativity of the phenolic resin molding material.
The application adopts the following technical scheme:
in a first aspect, the application provides a method for preparing a phenolic resin molding material for a commutator, wherein the phenolic resin molding material comprises the following raw materials in parts by weight: 10-30 parts of high-ortho phenolic resin, 5-20 parts of aniline-phenolic resin, 1-4 parts of curing agent, 40-50 parts of reinforcing agent and 15-30 parts of mineral powder; wherein, the content of the curing agent accounts for 8-15% of the total mass of the high ortho phenolic resin and the aniline-phenolic resin;
the preparation method of the phenolic resin molding material comprises the following steps:
uniformly mixing high ortho phenolic resin, aniline-phenolic resin, curing agent, reinforcing agent and mineral powder to prepare a predicted material, wherein the mixing time is 80-100 min;
kneading and extruding the expected material by adopting an extrusion molding process;
mixing the obtained extrudate, tabletting and crushing to prepare granules;
and (5) carrying out magnetic separation on the particles, screening and packaging.
At present, phenolic plastics commonly used in the market generally consist of common phenolic resin, curing agent and coloring agent, and the curing time is generally 3-5 minutes. Wherein the common phenolic resin is generally prepared by polycondensation of formaldehyde, phenol and an acidic or alkaline catalyst according to a certain proportion. The high ortho phenolic resin has more active sites and more curing time than the common phenolic resin; the aniline-phenolic resin is a phenolic resin prepared under the action of no acid, alkali and other catalysts, and takes aniline as a catalyst for phenolic condensation and simultaneously takes aniline as a reaction raw material. Aniline itself is also a good curing agent, which can accelerate the curing rate in the synthesis of aniline-phenolic resin.
The application uses the high ortho phenolic resin and the aniline-phenolic resin in a matching way, the aniline-phenolic resin is a solid thermosetting resin, and can be crosslinked and solidified by heating only, meanwhile, the activity of hydrogen on benzene ring in the aniline is larger than that of the benzene ring of phenol, and the aniline-phenolic resin can be subjected to similar phenolic condensation reaction with formaldehyde. Thus, the aniline-phenolic resin and the high ortho phenolic resin can be condensed and cured rapidly at a certain temperature under the condition of no curing agent or a small amount of curing agent. In the application, the curing time is further shortened by adding a small amount of curing agent, so that the curing time of the phenolic resin is shortened by 30% -40%. The reinforcing agent and the mineral powder can avoid the reduction of the mechanical properties of the high-ortho phenolic resin and the aniline-phenolic resin during the combination, and even further improve the mechanical properties of the phenolic resin molding material;
preferably, the preparation method of the high ortho phenolic resin comprises the following steps: phenol and formaldehyde with the molar ratio more than 1 are prepared under the condition that the pH value is 4-7; firstly, formaldehyde forms carbonium ion, and generates electrophilic substitution reaction on para position and ortho position of phenol to generate hydroxymethyl phenol; then the methylol phenol is quickly condensed with phenol to prepare the epoxy resin.
Preferably, zinc acetate and magnesium oxide are added in the preparation of the high ortho phenolic resin, and the mass ratio of the zinc acetate to the magnesium oxide is 100: (1-80). The zinc acetate is acidic and is used for synthesizing the thermoplastic solid high-ortho phenolic resin, so that the activity of phenol and formaldehyde can be further activated, the collar and site active points on the high-ortho phenolic resin are increased, the reaction of a curing agent and the high-ortho phenolic resin is facilitated, and the curing time is shortened; magnesium oxide is basic and is used to synthesize thermosetting liquid high ortho phenolic resins. The solid thermoplastic high ortho phenolic resin with high curing speed is synthesized by mixing zinc acetate and magnesium oxide, so that Ph is in the range of 4-7.
Preferably, the preparation method of the aniline-phenolic resin comprises the following steps: the aniline, phenol and formaldehyde with certain weight are put into a reaction vessel for polycondensation reaction, and the temperature of the reactor is 93-97 ℃. The heat resistance of the aniline-phenolic resin prepared by the method is obviously improved.
In addition, the addition amount of the curing agent exceeds 15% of the total amount of the high-ortho phenolic resin and the aniline-phenolic resin, so that the performance of a product is affected, and the excessive curing agent cannot play a curing effect, so that the phenolic resin molding material is softer. Therefore, the addition amount of the curing agent is preferably 12 percent of the total amount of the high ortho phenolic resin and the aniline-phenolic resin, so that the curing effect is maximized, the hardness of the phenolic resin molding material is not influenced, and the curing speed of the phenolic resin molding material is effectively accelerated.
In a second aspect, the present application uses an extrusion process to knead and extrude the anticipates, and uniformly mix the fixative, the reinforcing agent, the mineral powder and the anticipates; the extrudate is then further kneaded, which can make the expected mixture uniform and reduce the sticking, and make the quality of the phenolic resin molding material more uniform. The mixing time is preferably 90 minutes, which is advantageous for thorough mixing of the components.
The magnetic separation is used for screening magnetic substances such as iron in the particles, so that the particles have high insulativity. And then screening the particles, screening out fine powder in the particles, and avoiding the condition that dust pollutes the surrounding environment when in use, thereby being more convenient for using phenolic resin molding materials.
Optionally, in the extrusion process, the temperature of the conveying zone is 20 ℃ to 50 ℃, the temperature of the melting zone is 110 ℃ to 150 ℃, and the temperature of the plasticizing zone is 90 ℃ to 150 ℃.
The reciprocating single screw extruder used in the extrusion process is respectively provided with three operation areas, and the conveying areas are used for conveying raw materials, so that the temperature is not set to be too high, the temperature is preferably 35 ℃, and the raw materials are preheated so as to facilitate subsequent mixing. The melting zone mainly melts the raw materials of each component, and the raw materials are uniformly mixed after being melted. The melting zone temperature is preferably 140 c at which the components are sufficiently melted to facilitate mixing to form the desired product. The plasticizing zone is used to extrude the extrudate, preferably at 140 ℃, to avoid sticking the extrudate after cooling.
Optionally, the step of tabletting comprises compressing the extrudate into tablets having a thickness of 2m-4 mm;
and carrying out steel belt air cooling or water cooling on the pressed sheet for 20-30 min.
The mixed extrudate is thicker and is inconvenient to prepare into fine particles, so that the extrudate is pressed into tablets with the thickness of 3mm most appropriately, and the tablets are convenient to prepare into fine particles after being crushed. And then cooling the pressed sheet, wherein the brittleness of the cooled pressed sheet is improved, and the pressed sheet is easy to break into particles, so that the pressed sheet is convenient to prepare the phenolic resin molding material.
Optionally, the particle size of the particles is 0.4m-5mm, and the magnetic field strength is 20000Gs-26000Gs and the temperature is 5-15 ℃ in the process of carrying out magnetic separation on the particles.
The particles with fineness of more than 5mm are too coarse, the prepared molding material is rough, and the problem of poor uniformity of the phenolic resin molding material is easily caused; too thin of 0.4mm or more can reduce the mechanical properties of the phenolic molding material. The particle size of the particles is preferably 2.5m, so that the mechanical property of the phenolic resin molding material can be maintained, and the phenolic resin molding material is finer and more uniform.
The magnetic field intensity is more than 20000Gs, weak magnetic substances such as iron and titanium can be screened, and the insulativity of the molding material can be effectively improved after the weak magnetic substances are screened, so that the molding material is non-conductive, and the molding material is better suitable for a reversing machine.
Optionally, the curing agent is at least one selected from hexamethylenetetramine, salicylic acid and aniline.
The curing agent can neutralize free phenol and acidic substances in the high-ortho phenolic resin and the aniline-phenolic resin, and the hexamethylenetetramine, the salicylic acid and the aniline all contain active groups which react with hydroxyl active groups in the high-ortho phenolic resin and the aniline-phenolic resin side groups so as to promote curing and shorten curing time.
Optionally, the curing agent is hexamethylenetetramine, salicylic acid and aniline, wherein the mass ratio of the hexamethylenetetramine, the salicylic acid and the aniline is (0.5-1.5): 1:0.5.
the hexamethylene tetramine, the salicylic acid and the aniline are all provided with active groups which can react with hydroxyl active groups on the high-ortho phenolic resin and the aniline-phenolic resin side group to accelerate the curing speed of the expected substances. The mass ratio of hexamethylenetetramine, salicylic acid and aniline is preferably 1:1:0.5, the three components can mutually promote, improve the curing effect and further accelerate the curing speed of the phenolic resin.
Optionally, the mineral powder is silica powder, mica powder and inorganic salt whisker, wherein the mass ratio of the wollastonite to the mica powder to the inorganic salt whisker is (0-10): 10: (1-50).
The silica powder is powdery silica, has strong high temperature resistance, high electrical insulation strength, stable chemical property, water insolubility and acid and alkali corrosion resistance; the mica powder is a nonmetallic mineral, contains various components, has good insulativity, high temperature resistance and corrosion resistance, has strong adhesive force, and is an excellent additive; the inorganic salt whisker has high strength and high modulus. The addition of the three substances can enhance the toughness, high temperature resistance and corrosion resistance of the phenolic resin molding material, so that the curing time of the phenolic resin molding material is shortened and the mechanical property of the phenolic resin molding material is improved. The three materials have good insulativity, so that the insulativity of the phenolic resin is not affected when the mechanical property of the phenolic resin molding material is improved. The three components are compounded for use, so that the performance of the phenolic resin molding material can be better improved, and the quality of the phenolic resin molding material is further improved.
Optionally, the reinforcing agent is glass fiber, aramid fiber and basalt fiber, and the mass ratio of the glass fiber to the aramid fiber to the basalt fiber is 10: (0-10:): (1-100).
The glass fiber is used for reinforcing plastics and has good insulation property; the aramid fiber has ultrahigh strength and high modulus, and the modulus is 2-3 times of that of the glass fiber; basalt fiber is continuous fiber formed by high-speed drawing of a platinum-rhodium alloy wire-drawing bushing, and has high strength and high electrical insulation. The reinforcing agent can improve the mechanical property of the phenolic resin after being compounded, so that the phenolic resin has better heat resistance, corrosion resistance and high strength, and the service life of the phenolic resin molding material is prolonged.
Optionally, the phenolic resin molding material further comprises 3-7 parts by weight of organic modified montmorillonite.
The organically modified montmorillonite is a nano composite material, has ultrahigh mechanical properties, has higher tensile strength and bending strength and high wear resistance, and can effectively improve the mechanical properties of phenolic resin. In addition, the wear resistance of the phenolic resin material can be enhanced, and the service life of the phenolic plastic can be prolonged.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the application prepares the phenolic resin molding material by combining the high ortho phenolic resin and the aniline-phenolic resin, which can further accelerate the curing speed, shorten the curing time and improve the production efficiency;
2. in the application, when the phenolic resin material is prepared, the expected material is kneaded and extruded by adopting an extrusion molding process, and then the extrudate is mixed, so that the condition of sticking during mold molding can be reduced, the integrity of the molding material is improved, and the deformation and stress of the molding material are reduced;
3. the application carries out magnetic separation on the crushed particles in the process of preparing the phenolic resin material, screens out magnetic substances in the particles, and ensures that the particles are insulated, so that the application is better suitable for the reverser.
Drawings
FIG. 1 is a graph showing the performance test data of the phenolic resin molding material prepared in example 1 of the present application.
FIG. 2 is a graph showing the performance test data of the phenolic resin molding material prepared in comparative example 1 of the present application.
Detailed Description
The present application will be described in further detail with reference to examples. The specific description is: the following examples were conducted under conventional conditions or conditions recommended by the manufacturer, where specific conditions were not noted; the raw materials used in the following examples were all commercially available from ordinary sources except for the specific descriptions.
Examples
Example 1
The embodiment provides a preparation method of a phenolic resin molding material for a commutator, which comprises the following steps:
(1) Putting 20 parts of high ortho phenolic resin, 10 parts of aniline-resin, 2 parts of curing agent (the curing agent is hexamethylenetetramine, salicylic acid and aniline with the mass ratio of 1:1:0.5), 45 parts of reinforcing agent (the reinforcing agent is glass fiber, aramid fiber and brown Wu Qianwei with the mass ratio of 10:5:85), 20 parts of mineral powder (wollastonite with the mass ratio of 3:10:35 of mineral powder is mica powder and inorganic whisker salt) and 5 parts of organic modified montmorillonite into a mixer, and uniformly mixing to prepare a predicted material;
(2) Then the temperature of the output area of the reciprocating single screw extruder is set to 35 ℃, the temperature of the melting area is set to 140 ℃, the temperature of the plasticizing area is set to 140 ℃, the expected material is put into the reciprocating single screw extruder with the set temperature for kneading for 90min, and the extruded material is extruded after kneading.
(3) Putting the extrudate into a double-roll open mill for mixing;
(4) And (3) putting the mixed extrudate into a tablet press to press into 3mm tablets, carrying out steel belt air cooling on the tablets for 25min, and cooling the tablets to about 10 ℃.
(5) Crushing the cooled tabletting into particles with the particle size of 0.4-5 mm;
(6) Putting the prepared particles into a magnetic separator for magnetic separation, setting the magnetic field strength to 23000Gs, sucking out magnetic substances such as iron, titanium and the like in the particles, and enabling the particles to be insulating;
(7) And placing the particles subjected to magnetic separation in a vibrating screen, sieving out particles with the particle size of less than 0.4mm and more than 5mm, retaining the intermediate particles, and packaging the particles to prepare the phenolic resin molding material.
Examples 2-5 differ from example 1 only in the parts by weight of the high ortho phenolic resin and the aniline-phenolic resin, as shown in table 1:
table 1:
| high ortho phenolic resin | Aniline-phenolic resin | |
| Example 1 | 20 parts of | 10 parts of |
| Example 2 | 10 parts of | 5 parts of |
| Example 3 | 25 parts of | 15 parts of |
| Example 4 | 30 parts of | 10 parts of |
| Example 5 | 20 parts of | 20 parts of |
Examples 6 to 8 differ from example 1 only in the content of curing agents (curing agents being hexamethylenetetramine, salicylic acid and aniline in a mass ratio of 1:1:0.5), as shown in table 2:
table 2:
examples 9-11 differ from example 1 in the temperature of the zones of the reciprocating single screw extruder in step (2) as shown in Table 3:
table 3:
comparative example
Comparative example 1 differs from example 1 only in that comparative example 1 uses 30 parts of a common phenolic resin.
Comparative example 2 differs from example 1 only in that comparative example 2 uses 30 parts of high ortho phenolic resin.
Comparative example 3 differs from example 1 only in that comparative example 3 uses 30 parts of aniline-phenolic resin.
Comparative example 4 differs from example 1 only in that the temperature of each zone in the step (2) reciprocating single screw extruder was different, wherein the temperature of the output zone was set to 15 ℃, the temperature of the melting zone was set to 90 ℃, and the temperature of the plasticizing zone was set to 80 ℃.
Experimental method and experimental data
The experimental method comprises the following steps:
the mixture of the high ortho-position phenol resin and the aniline-phenol resin in the phenol resin molding materials prepared in examples 1 to 11 and comparative examples 1 to 3 of the present application was used as a sample, and the curing time was measured by using a GTII type glue curing time meter. The testing method comprises (1) setting the temperature of the gel curing time tester to 150 ℃, and preheating for about 30 min; (2) Gently wiping the heating disc by using release wax, and then wiping cleanly by using clean mirror wiping paper; (3) Taking about 0.3g of each sample by a small spoon, pouring the samples into a heating plate respectively, and immediately starting timing when the samples are in a melting state; (4) Stirring the resin clockwise or anticlockwise by using a toothpick, increasing the viscosity of the resin, and gently lifting the resin while scratching; (5) When the lifted resin is drawn and broken, the timing key is pressed down, and the timing is stopped immediately. Three groups of parallel samples are arranged for each sample, the curing time is measured respectively, the error is not more than 0.5s, the effective data can be calculated, and the average value is taken as a result.
Experimental data:
the curing times of the phenolic resin molding materials in examples 1 to 11 are shown in Table 4:
table 4:
experimental data for the phenolic resin molding materials of comparative examples 1 to 3 are shown in table 5:
table 5:
| curing time | |
| Comparative example 1 | 90s |
| Comparative example 2 | 70s |
| Comparative example 3 | 75s |
By combining example 1, comparative example 1 and tables 4 and 5, the reactive groups in the conventional phenolic resin are less than the high ortho phenolic resin of the present application, and the polycondensation reaction time of the fixing agent and the conventional phenolic resin is longer, resulting in longer curing time. Even if the common phenolic resin is prepared into the phenolic resin molding material by the preparation method, the curing time is still far longer than that of the phenolic resin molding material in the embodiment 1, so that the high ortho phenolic resin and the aniline-phenolic resin are used in a matching way, the curing speed can be increased, and the curing time can be shortened.
It can be seen from example 1, example 5, in combination with Table 1 that when the content of the high ortho phenolic resin or the aniline-phenolic resin is increased only, the curing time is prolonged, since when one of the components is excessive, the reactive groups in that component are also excessive, and the excessive reactive groups do not participate in the reaction, resulting in a prolonged curing time. However, when the contents of the high ortho phenolic resin and the aniline-phenolic resin are synchronously increased or decreased, the influence on the curing time of the phenolic resin molding material is small, and the total mass of the high ortho phenolic resin and the aniline-phenolic resin can be obtained in proportion to the curing time. When the high ortho phenolic resin is added, the aniline-phenolic resin is added, so that the active groups and the reactive groups in the aniline can be correspondingly reacted, the condition that the active groups are excessive and do not participate in reflection is avoided, and the influence on the curing time is reduced; when the high ortho-position phenolic resin is reduced, the aniline-phenolic resin is reduced, the excessive reaction groups are reduced, the reaction is not participated, and the curing speed of the phenolic resin molding material is improved.
As can be seen from examples 1, comparative example 1, examples 6 to 8, and in combination with tables 4 and 5, when the total mass of the high ortho phenolic resin and the aniline-phenolic resin is constant, reducing the amount of the curing agent will prolong the curing time, but the curing time is still far higher than that of the phenolic resin molding material in comparative example 1; when the curing agent is added, the curing time can be shortened; however, when the added curing agent exceeds 15% of the total mass of the high ortho phenolic resin and the aniline-phenolic resin molding material, the curing agent can reduce the hardness of the high ortho phenolic resin and the aniline-phenolic resin, so that the phenolic resin molding material is softer, the curing time is reduced, and therefore, the addition amount of the curing agent is controlled within a proper range, so that the effect of accelerating the curing speed of the curing agent is maximized.
As can be seen from examples 1, examples 9 to 11 in combination with table 4, the curing time will be prolonged when the temperature at which kneading and extrusion of the material is expected in step (2) is lowered; curing times are also prolonged when the temperature is increased. Therefore, the shortest curing time can be obtained only when the temperature for kneading and extruding the material is set at the temperature in example 1.
It can be seen from example 1, comparative examples 2 to 3, and tables 4 and 1 that the curing time was far lower than that of the phenolic resin molding material of example 1 when only the high ortho phenolic resin or the aniline-phenolic resin of the same quality was used. The high ortho phenolic resin and the aniline-phenolic resin can be matched and promoted mutually, the time of polycondensation reaction is shortened, the curing speed is further increased, and the curing time is effectively shortened.
As can be seen from examples 1 and 4, since the high ortho-position phenol-formaldehyde resin and the aniline-phenol-formaldehyde resin have high heat resistance, they have high viscosity after melting, and when the temperature of each zone in the reciprocating single screw extruder in step (2) is low, the above components are not sufficiently melted, so that a condition of sticking film occurs during film formation, and the integrity and mechanical properties of the phenol-formaldehyde resin molding material are reduced. Therefore, when the temperature is set to the temperature in example 1, the components can be sufficiently melted, the occurrence of sticking during film formation can be avoided, the integrity of the phenolic resin molding material can be improved, and the decrease in mechanical properties can be avoided.
Method for detecting mechanical property of phenolic resin molding material and experimental data thereof
The detection method comprises the following steps:
in the examples of the present application, the phenolic resin molding materials prepared in example 1 and comparative example 1 were used as test samples, and the crosslinking curing properties and mechanical properties of the phenolic resin molding materials prepared in example 1 and comparative example 1 were tested according to the GB1404-86 Standard of phenolic moulding materials.
The experimental conditions for detecting the crosslinking curing property of the phenolic resin molding material in example 1 are shown in table 6:
table 6:
the test conditions for the cross-linking curing property test of the phenolic resin molding material in comparative example 1 are shown in Table 7:
table 7:
performance test experimental data:
the test data of the cross-linking curing property test of the phenolic resin molding material in example 1 are shown in tables 7 and 8:
table 7:
| time of occurrence(s) | Torque (Nm) | Material temperature (. Degree. C.) | Rotating speed (R/min) | |
| Peak charge A | 8 | 36.3 | 131.6 | 29.8 |
| Torque minimum value B | 26 | 10.4 | 138.4 | 30.4 |
| Maximum torque C | 57 | 22.3 | 146.1 | 30.0 |
| Initiating crosslinking X1 | 20 | 13.4 | 136.6 | 30.2 |
| Stopping crosslinking X2 | 42 | 13.4 | 142.5 | 30.2 |
| Stop reaction Y | 46 | 15.4 | 143.8 | 30.0 |
Table 8:
| time sum(s) | Energy (Nm) | |
| Melting time A-B | 18 | 214.6 |
| Sample evaluation A-C | 49 | 450.6 |
| Retention times X1-X2 | 22 | 136.3 |
| Reaction time A-Y | 38 | 339.9 |
The test data of the cross-linking curing property test of the phenolic resin molding material in comparative example 1 are shown in tables 9 and 10:
table 9:
| time of occurrence(s) | Torque (Nm) | Material temperature (. Degree. C.) | Rotating speed (R/min) | |
| Peak charge A | 9 | 23.1 | 130.4 | 30.0 |
| Torque minimum value B | 29 | 6.1 | 137.5 | 30.2 |
| Maximum torque C | 92 | 20.3 | 146.8 | 30.0 |
| Initiating crosslinking X1 | 20 | 9.1 | 134.0 | 30.2 |
| Stopping crosslinking X2 | 55 | 9.1 | 141.4 | 30.2 |
| Stop reaction Y | 64 | 11.1 | 142.6 | 30.2 |
Table 10:
| time sum(s) | Energy (Nm) | |
| MeltingTime A-B | 20 | 136.4 |
| Sample evaluation A-C | 83 | 500.7 |
| Retention times X1-X2 | 35 | 128.8 |
| Reaction time A-Y | 55 | 277.4 |
The results of the mechanical property detection of the phenolic resin molding materials in example 1 and comparative example 1 are shown in Table 7:
table 11:
from example 1, comparative example 1, and the combination of tables 7 to 10 and fig. 1 and 2, it can be found that the phenolic resin molding material prepared in example 1 has shorter crosslinking initiation time and termination time than the phenolic resin molding material prepared in comparative example 1 in the case of performing crosslinking curability detection, and it is further revealed that the use of a high ortho phenolic resin molding material in combination with aniline-phenolic resin can improve the curing time of the phenolic resin molding material.
As can be seen from example 1, comparative example 1, and Table 11, the conventional phenolic resin molding material prepared in comparative example 1 has lower mechanical properties than the phenolic resin molding material prepared in example 1, and the time for crosslinking and curing A to C is longer. Therefore, the application can effectively shorten the crosslinking curing time by combining the high ortho phenolic resin with the aniline-phenolic resin. The reinforcing agent (glass fiber, aramid fiber and basalt fiber), mineral powder (silica powder, mica powder and inorganic salt whisker) and the organically modified montmorillonite are added in the application, so that the mechanical property of the phenolic resin molding material can be effectively enhanced under the condition of not influencing the crosslinking curing time, and the phenolic resin molding material is more suitable for a commutator.
The above embodiments are not intended to limit the scope of the present application, so: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.
Claims (10)
1. A preparation method of a phenolic resin molding material for a commutator is characterized by comprising the following steps: the phenolic resin molding material comprises the following raw materials in parts by weight: 10-30 parts of high-ortho phenolic resin, 5-20 parts of aniline-phenolic resin, 1-4 parts of curing agent, 40-50 parts of reinforcing agent and 15-30 parts of mineral powder; wherein the content of the curing agent accounts for 8% -15% of the total mass of the high ortho phenolic resin and the aniline-phenolic resin;
the preparation method of the phenolic resin molding material comprises the following steps:
uniformly mixing the high ortho phenolic resin, the aniline-phenolic resin, the curing agent, the reinforcing agent and the mineral powder to prepare a predicted material, wherein the mixing time is 80-100 min;
kneading and extruding the material to be expected by adopting an extrusion molding process;
mixing the obtained extrudate, tabletting and crushing to prepare granules;
and (5) carrying out magnetic separation on the particles, screening and packaging.
2. The method for producing a phenolic resin molding material according to claim 1, characterized in that: in the extrusion molding process, the temperature of the conveying area is 20-50 ℃, the temperature of the melting area is 110-150 ℃, and the temperature of the plasticizing area is 90-150 ℃.
3. The method for producing a phenolic resin molding material according to claim 1, characterized in that: the step of tabletting comprises compressing the extrudate into tablets having a thickness of 2mm to 4 mm;
and carrying out steel belt air cooling or water cooling on the pressed sheet for 20-30 min.
4. The method for producing a phenolic resin molding material according to claim 1, characterized in that: the particle size of the particles is 0.4mm-5mm, and the magnetic field strength is 20000Gs-26000Gs and the temperature is 5 ℃ to 15 ℃ in the process of carrying out magnetic separation on the particles.
5. The method for producing a phenolic resin molding material according to claim 1, characterized in that: the curing agent is at least one selected from hexamethylenetetramine, salicylic acid and aniline.
6. The method for producing a phenolic resin molding material according to claim 5, wherein: the curing agent is hexamethylenetetramine, salicylic acid and aniline, wherein the mass ratio of the hexamethylenetetramine to the salicylic acid to the aniline is (0.5-1.5): 1:0.5.
7. the method for producing a phenolic resin molding material according to claim 1, characterized in that: the mineral powder is silica powder, mica powder and inorganic salt whisker, and the mass ratio of the silica powder to the mica powder to the inorganic salt whisker is (0-10): 10: (1-50).
8. The method for producing a phenolic resin molding material according to claim 1, characterized in that: the reinforcing agent is glass fiber, aramid fiber and basalt fiber, and the mass ratio of the glass fiber to the aramid fiber to the basalt fiber is 10: (0-10:): (1-100).
9. The method for producing a phenolic resin molding material according to claim 1, characterized in that: the phenolic resin molding material also comprises 3-7 parts by weight of organic modified montmorillonite.
10. A phenolic resin molding material for a commutator, characterized in that: the phenolic resin molding material is produced according to the production method of any one of claims 1 to 9.
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