CN103937150A - Fibrilia-reinforced injection-type phenol aldehyde molding compound and preparation method thereof - Google Patents
Fibrilia-reinforced injection-type phenol aldehyde molding compound and preparation method thereof Download PDFInfo
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- CN103937150A CN103937150A CN201410157469.6A CN201410157469A CN103937150A CN 103937150 A CN103937150 A CN 103937150A CN 201410157469 A CN201410157469 A CN 201410157469A CN 103937150 A CN103937150 A CN 103937150A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
- B29B9/14—Making granules characterised by structure or composition fibre-reinforced
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
- B29B7/7461—Combinations of dissimilar mixers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/88—Adding charges, i.e. additives
- B29B7/90—Fillers or reinforcements, e.g. fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
- B29B2009/125—Micropellets, microgranules, microparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
- B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92514—Pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92561—Time, e.g. start, termination, duration or interruption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
- B29C2948/9259—Angular velocity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92609—Dimensions
- B29C2948/92638—Length
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92838—Raw material pre-treatment, e.g. drying or cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92942—Moulded article
Abstract
The invention discloses a fibrilia-reinforced injection-type phenol aldehyde molding compound and a preparation method thereof. The phenol aldehyde molding compound is mainly prepared from linear phenol aldehyde resin, hexamethylenetetramine, inorganic filler and fibrilia. The preparation method comprises the following steps: 1) weighing the raw materials for later use; 2) putting the inorganic filler and coupling agent in a ball mill or ball milling tank, and carrying out uniform ball milling, wherein the coupling agent accounts for 0.5-10 wt% of the inorganic filler, and the inorganic filler is one or combination of more than two of aluminum hydroxide, silicon micropowder, calcite, talcum, calcium carbonate, glass microballoon, kaolin and figuline powder; 3) pulverizing the hexamethylenetetramine, and uniformly mixing with the surface-treated inorganic filler and the other raw materials; 4) adding the mixture into a double screw extruder, and extruding; and 5) cooling the extruded stock, and pulverizing. The phenol aldehyde molding compound prepared by the method has the advantages of higher mechanical properties and lower water absorptivity.
Description
Technical field
The present invention relates to phenolaldehyde moulding compound, be specifically related to a kind of flaxen fiber and strengthen injection phenolic moulding plastics and preparation method thereof.
Background technology
Phenolaldehyde moulding compound is taking resol as base material, and be matrix material prepared by main raw material in conjunction with other stopping composition, it has, and cheap, heat-resisting, product size is stable, electrical insulating property is good, the over-all properties of the more high excellence of mechanical property, is widely used in electronics, electrical equipment, automobile and other industries [2].Along with economic development, the demand of high performance material improves constantly, also more and more higher to the performance requriements of phenolaldehyde moulding compound, and mechanical property and the thermotolerance etc. of such material are all had higher requirement.
In prior art, mostly in formula, coordinate and add strongthener to improve moulding compound thermotolerance or mechanical property, can in high-temperature field, be more widely used.As the publication number patent of invention that is CN1789327, a kind of blend taking trimeric cyanamide-P-F copolymer resins or melamine formaldehyde resin/phenol-formaldehyde resin is disclosed as matrix resin, selecting inorganic fibre and organic fibre is that toughener, inorganic mineral are filler, the injection-type trimeric cyanamide-P-F moulding compound that adopts composite crosslinking curing system to be prepared from.Though this material has higher heat-drawn wire (190 DEG C) and good insulating property, its mechanical property as resistance to impact shock and flexural strength all poor, wherein notched Izod impact strength is only 2.0～2.2kJ/m
2, flexural strength only between 70～80Mpa, is difficult to adapt to some to all higher occasions of thermotolerance and mechanical property requirements.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of new injection molding flaxen fiber that passes through and strengthens injection phenolic moulding plastics and preparation method thereof, and phenolaldehyde moulding compound mechanical property obtained by this method is higher, water-absorbent is lower.
Flaxen fiber of the present invention strengthens the preparation method of injection phenolic moulding plastics, wherein be used for preparing the raw material that this flaxen fiber strengthens injection phenolic moulding plastics and mainly contain lacquer resins, hexamethylenetetramine, mineral filler and flaxen fiber, the preparation method that this flaxen fiber strengthens injection phenolic moulding plastics specifically comprises the following steps:
1) take each raw material, for subsequent use;
2) get mineral filler coupling agent and carry out surface treatment, specifically by coupling agent with mineral filler is placed in ball mill or ball grinder ball milling is even, the consumption of described coupling agent is 0.5～10wt% of mineral filler consumption, and described mineral filler is one or more the combination being selected from aluminium hydroxide, silicon powder, calcite, talcum, calcium carbonate, glass microballon, kaolin and potter's clay powder;
3) get hexamethylenetetramine and pulverize, then mix with surface treated mineral filler and other raw material;
4) material mixing being dropped into twin screw extruder extrudes;
5) the cooling rear pulverizing of extruded stock, to obtain final product.
The method of the invention is first carried out ball milling modification processing by mineral filler with the coupling agent of specific consumption, effectively improve the interface compatibility between hydrophilic mineral filler and oil loving phenolic resin as matrix resin, make mineral filler in the time mixing with phenolic resin as matrix resin and other raw material, cohesive force between mineral filler and matrix and other raw material is obviously strengthened, thereby make plastics can the injection molding while, the mechanical property that can also make plastics is increased dramatically as shock strength, flexural strength etc., and water-absorbent is significantly reduced.
In above-mentioned preparation method, be used for preparing the raw material that described flaxen fiber strengthens injection phenolic moulding plastics and conventionally also comprise promotor and lubricant, further also can comprise dyestuff.Preparing proportioning between each raw material that described flaxen fiber strengthens injection phenolic moulding plastics can be with existing using flaxen fiber as strongthener and adopt the conventional proportioning raw materials of injection molding phenolaldehyde moulding compound identical, and the weight proportion of preferred each raw material is:
Lacquer resins 100;
Hexamethylenetetramine 10～20;
Mineral filler 20～90;
Length is the flaxen fiber 25～65 of 1～10mm;
Promotor 0.5～8;
Lubricant 1～8;
Dyestuff 0～10.
The weight proportion of each raw material is more preferably:
Lacquer resins 100;
Hexamethylenetetramine 13～18;
Mineral filler 30～80;
Length is the flaxen fiber 35～55 of 1～10mm;
Promotor 1～5;
Lubricant 2～5;
Dyestuff 0～6.
Promotor in above-mentioned raw materials can be one or more the combination being selected from magnesium hydroxide, calcium hydroxide, magnesium oxide and calcium oxide.In the time of above-mentioned two or more the combination of being chosen as of promotor, the proportioning between them can be any proportioning.
Lubricant in above-mentioned raw materials can be one or more the combination being selected from calcium stearate, Zinic stearas, ethylene stearylamide, stearic acid and stearin.In the time of above-mentioned two or more the combination of being chosen as of lubricant, the proportioning between them can be any proportioning.
Dyestuff in above-mentioned raw materials can be one or more the combination being selected from nigrosine, phthalocyanine blue, phthalocyanine green and iron oxide red.In the time of above-mentioned two or more the combination of being chosen as of dyestuff, the proportioning between them can be any proportioning.
Flaxen fiber described in above-mentioned raw materials can be sisal fibers, flax fiber or ramee, or arbitrarily two or more and with the combination of arbitrary proportion in them.Preferably selecting length is the flaxen fiber of 2～6mm.
Above-mentioned preparation method's step 2) in, preferably control the rotating speed 10～60rpm of ball mill or ball grinder, Ball-milling Time is 10～120min, so that the product of final molding can obtain better mechanical property and water-absorbent.
Above-mentioned preparation method's step 2) in, described coupling agent can be silane coupling agent, titanate coupling agent or aluminate coupling agent, the consumption of described coupling agent is preferably 3～8wt% of mineral filler consumption, more preferably 4～6wt% of mineral filler consumption.
Above-mentioned preparation method's step 2) in, described mineral filler is preferably selected from one or more the combination in silicon powder, calcite, talcum, calcium carbonate and glass microballon, the more preferably combination of one or more in calcite, calcium carbonate and glass microballon.In the time of above-mentioned two or more the combination of being chosen as of mineral filler, the proportioning between them can be any proportioning.
In above-mentioned preparation method's step 3), conventionally hexamethylenetetramine is crushed to and is not less than 80 orders.
In above-mentioned preparation method's step 4), in the time extruding with twin screw extruder, the barrel temperature that twin screw extruder is set is conventionally 75～100 DEG C, and screw rod revolution is 70～90rpm.
Above-mentioned preparation method's step 5) in, after extruded stock is cooling, being crushed to diameter is rule or the irregular granular of 1～6mm.
The present invention also comprises that the flaxen fiber being made by aforesaid method strengthens injection phenolic moulding plastics, and the simply supported beam unnotched impact strength of this moulding compound is at 10.0kJ/m
2above, simply supported beam notched Izod impact strength is at 2.9kJ/m
2above, flexural strength is more than 105Mpa.
The technique of the moulding compound that aforesaid method makes during with the injection molding of thermoset injector is as follows: die temperature is 150～190 DEG C, and barrel temperature is 80～100 DEG C, and injection pressure is 60～100MPa, and be 10～20s/mm set time.
Compared with prior art, the method of the invention is carried out ball-milling processing by the coupling agent with specific consumption to mineral filler, on the one hand, make coupling agent molecule evenly be wrapped in inorganic filler surface, reduce the possibility that reunion occurs between filler, improve the dispersiveness of filler, make mineral filler in the time mixing with phenolic resin as matrix resin and other raw material, cohesive force between mineral filler and matrix and other raw material is obviously strengthened, thereby make plastics can the injection molding while, can also make the mechanical property of plastics as shock strength, flexural strengths etc. are increased dramatically, on the other hand, the hydrophilic radical of coupling agent and the hydroxyl of filling surface interact and form hydrogen bond, have reduced the content of filling surface hydroxyl, thus hydroxyl and the interactional probability of moisture in air while having restricted curing molding, in addition, through coupling agent surface-treated filler in postorder mixing step, effectively improved the interface compatibility between filler and resin, filler and resin are closely linked, and have reduced the surface-area of filler, enable to reduce with the interactional free hydroxyl group of water, moreover coupling agent itself also forms hydrophobic coat at filling surface, can effectively slow down the rate of water absorption of plastics, therefore, the water-absorbent of gained plastics is significantly reduced.
Embodiment
With embodiment, the present invention is further described below, but the present invention is not limited to these embodiment.
In following embodiment, twin screw extruder used is thermoset parallel dual-screw extruding machine.
Umber described in following embodiment is weight part.
Embodiment 1
1) take following component for subsequent use: 3 parts of 25 parts of sisal fiberss, magnesium hydroxides, 1 part of calcium stearate that 100 parts of lacquer resinss (be novolac resin, lower with), 10 parts of hexamethylenetetramines, 80 parts of 400～600 object silicon powders, length are 2～5mm;
2) titanate coupling agent of getting silicon powder and being equivalent to its consumption 0.5% is placed in ball grinder and carries out ball milling, controls the rotating speed 10rpm of ball grinder, and Ball-milling Time is 10min;
3) get hexamethylenetetramine and be crushed to 80 orders, then mix with surface treated silicon powder and other component;
4) material mixing is dropped into twin screw extruder and extrude, the barrel temperature of described twin screw extruder is 75～90 DEG C, and screw rod revolution is 80rpm;
5) extruded stock is crushed to the irregular granular that diameter is 1～6mm after being cooled to normal temperature, obtains flaxen fiber of the present invention and strengthens injection phenolic moulding plastics.
Comparative example 1-1
1) with the step 1 of embodiment 1);
2) get the sisal fibers titanate coupling agent that is equivalent to its consumption 0.5% and carry out conventional surface treatment;
3) get hexamethylenetetramine and be crushed to 80 orders, then mix with surface treated sisal fibers and other component;
4) with the step 4 of embodiment 1);
5) extruded stock is crushed to the irregular granular that diameter is 1～6mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Comparative example 1-2
1) with the step 1 of embodiment 1);
2) get hexamethylenetetramine and be crushed to 80 orders, then mix with other component;
3) with the step 4 of embodiment 1);
4) extruded stock is crushed to the irregular granular that diameter is 1～6mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Embodiment 2
1) take following component for subsequent use: 2 parts of 5 parts of 45 parts of sisal fiberss, magnesium hydroxides, Zinic stearass, 5 parts of iron oxide reds that 100 parts of lacquer resinss, 15 parts of hexamethylenetetramines, 50 parts, 600～800 object calcite, length are 1～10mm;
2) aluminate coupling agent of getting calcite and being equivalent to its consumption 3% is placed in ball grinder and carries out ball milling, controls the rotating speed 50rpm of ball grinder, and Ball-milling Time is 80min;
3) get hexamethylenetetramine and be crushed to 100 orders, then mix with surface treated calcite and other component;
4) material mixing is dropped into twin screw extruder and extrude, the barrel temperature of described twin screw extruder is 90～100 DEG C, and screw rod revolution is 90rpm;
5) extruded stock is crushed to the irregular granular that diameter is 2～5mm after being cooled to normal temperature, obtains flaxen fiber of the present invention and strengthens injection phenolic moulding plastics.
Comparative example 2-1
1) with the step 1 of embodiment 2);
2) get the sisal fibers aluminate coupling agent that is equivalent to its consumption 3% and carry out conventional surface treatment;
3) get hexamethylenetetramine and be crushed to 100 orders, then mix with surface treated sisal fibers and other component;
4) with the step 4 of embodiment 2);
5) extruded stock is crushed to the irregular granular that diameter is 2～5mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Comparative example 2-2
1) with the step 1 of embodiment 2);
2) get hexamethylenetetramine and be crushed to 100 orders, then mix with other component;
3) with the step 4 of embodiment 2);
4) extruded stock is crushed to the irregular granular that diameter is 2～5mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Embodiment 3
1) take by weight percentage following component for subsequent use: 1 part, 55 parts of flax fibers, calcium oxide, 5 parts of Zinic stearass that 100 parts of lacquer resinss, 20 parts of hexamethylenetetramines, 30 parts, 100～300 object calcium carbonate, length are 5～10mm;
2) silane coupling agent of getting calcium carbonate and being equivalent to its consumption 5% is placed in ball grinder and carries out ball milling, controls the rotating speed 30rpm of ball grinder, and Ball-milling Time is 60min;
3) get hexamethylenetetramine and be crushed to 80 orders, then mix with surface treated calcium carbonate and other component;
4) material mixing is dropped into twin screw extruder and extrude, the barrel temperature of described twin screw extruder is 75～85 DEG C, and screw rod revolution is 90rpm;
5) extruded stock is crushed to the irregular granular that diameter is 4～6mm after being cooled to normal temperature, obtains flaxen fiber of the present invention and strengthens injection phenolic moulding plastics.
Comparative example 3-1
1) with the step 1 of embodiment 3);
2) get the flax fiber silane coupling agent that is equivalent to its consumption 5% and carry out conventional surface treatment;
3) get hexamethylenetetramine and be crushed to 80 orders, then mix with surface treated flax fiber and other component;
4) with the step 4 of embodiment 3);
5) extruded stock is crushed to the irregular granular that diameter is 4～6mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Comparative example 3-2
1) with the step 1 of embodiment 3);
2) get hexamethylenetetramine and be crushed to 80 orders, then mix with its component;
3) with the step 4 of embodiment 3);
4) extruded stock is crushed to the irregular granular that diameter is 4～6mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Embodiment 4
1) take by weight percentage following component for subsequent use: 8 parts, 35 parts of flax fibers, magnesium oxide, 0.5 part of stearic acid that 100 parts of lacquer resinss, 18 parts of hexamethylenetetramines, 20 parts of 600～800 object glass microballons, length are 1～6mm;
2) aluminate coupling agent of getting glass microballon and being equivalent to its consumption 6% is placed in ball grinder and carries out ball milling, controls the rotating speed 60rpm of ball grinder, and Ball-milling Time is 100min;
3) get hexamethylenetetramine and be crushed to 120 orders, then mix with surface treated glass microballon and other component;
4) material mixing is dropped into twin screw extruder and extrude, the barrel temperature of described twin screw extruder is 75～80 DEG C, and screw rod revolution is 85rpm;
5) extruded stock is crushed to the irregular granular that diameter is 6mm after being cooled to normal temperature, obtains flaxen fiber of the present invention and strengthens injection phenolic moulding plastics.
Comparative example 4-1
1) with the step 1 of embodiment 4);
2) get the flax fiber aluminate coupling agent that is equivalent to its consumption 6% and carry out conventional surface treatment;
3) get hexamethylenetetramine and be crushed to 120 orders, then mix with surface treated flax fiber and other component;
4) with the step 4 of embodiment 4);
5) extruded stock is crushed to the irregular granular that diameter is 6mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Comparative example 4-2
1) with the step 1 of embodiment 4);
2) get hexamethylenetetramine and be crushed to 120 orders, then mix with other component;
3) with the step 4 of embodiment 4);
4) extruded stock is crushed to the irregular granular that diameter is 6mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Embodiment 5
1) take by weight percentage following component for subsequent use: 8 parts of 0.5 part, 65 parts of ramees, calcium hydroxide, ethylene stearylamides, 8 parts of nigrosine that 100 parts of lacquer resinss, 16 parts of hexamethylenetetramines, 200～400 90 parts, object potter's clay powder, length are 5～8mm;
2) silane coupling agent of getting potter's clay powder and being equivalent to its consumption 8% is placed in ball grinder and carries out ball milling, controls the rotating speed 20rpm of ball grinder, and Ball-milling Time is 120min;
3) get hexamethylenetetramine and be crushed to 160 orders, then mix with surface treated potter's clay powder and other component;
4) material mixing is dropped into twin screw extruder and extrude, the barrel temperature of described twin screw extruder is 80～95 DEG C, and screw rod revolution is 75rpm;
5) extruded stock is crushed to the irregular granular that diameter is 2mm after being cooled to normal temperature, obtains flaxen fiber of the present invention and strengthens injection phenolic moulding plastics.
Comparative example 5-1
1) with the step 1 of embodiment 5);
2) get the ramee silane coupling agent that is equivalent to its consumption 8% and carry out conventional surface treatment;
3) get hexamethylenetetramine and be crushed to 160 orders, then mix with surface treated ramee and other component;
4) with the step 4 of embodiment 5);
5) extruded stock is crushed to the irregular granular that diameter is 2mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Comparative example 5-2
1) with the step 1 of embodiment 5);
2) get hexamethylenetetramine and be crushed to 160 orders, then mix with other component;
3) with the step 4 of embodiment 5);
4) extruded stock is crushed to the irregular granular that diameter is 2mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Embodiment 6
1) take by weight percentage following component for subsequent use: 3 parts, 50 parts of ramees, calcium oxide, 5 parts of glyceryl stearates that 100 parts of lacquer resinss, 13 parts of hexamethylenetetramines, 200～300 80 parts, object kaolin powder, length are 5～8mm;
2) silane coupling agent of getting kaolin powder and being equivalent to its consumption 10% is placed in ball grinder and carries out ball milling, controls the rotating speed 20rpm of ball grinder, and Ball-milling Time is 120min;
3) get hexamethylenetetramine and be crushed to 160 orders, then mix with surface treated kaolin powder and other component;
4) material mixing is dropped into twin screw extruder and extrude, the barrel temperature of described twin screw extruder is 80～100 DEG C, and screw rod revolution is 80rpm;
5) extruded stock is crushed to the irregular granular that diameter is 2～5mm after being cooled to normal temperature, obtains flaxen fiber of the present invention and strengthens injection phenolic moulding plastics.
Comparative example 6-1
1) with the step 1 of embodiment 5);
2) get the ramee silane coupling agent that is equivalent to its consumption 10% and carry out conventional surface treatment;
3) get hexamethylenetetramine and be crushed to 160 orders, then mix with surface treated ramee and other component;
4) with the step 4 of embodiment 5);
5) extruded stock is crushed to the irregular granular that diameter is 2～5mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Comparative example 6-2
1) with the step 1 of embodiment 5);
2) get hexamethylenetetramine and be crushed to 160 orders, then mix with other component;
3) with the step 4 of embodiment 5);
4) extruded stock is crushed to the irregular granular that diameter is 2～5mm after being cooled to normal temperature, and the flaxen fiber that obtains contrast strengthens injection phenolic moulding plastics.
Respectively by the prepared phenolaldehyde moulding compound of above-described embodiment 1～6, comparative example 1-1～comparative example 6-1 and comparative example 1-2～contrast row 6-2 respectively by thermoset injector by following technique injection molding: die temperature is 170 DEG C, barrel temperature is 90 DEG C, injection pressure is 60MPa, and be 20s/mm set time.The moulding compound of gained and German PF51 phenolaldehyde moulding compound carry out mechanical electric performance comparison, and result is as shown in following table 1, table 2 and table 3:
Table 1:
Table 2:
Table 3:
Above shock strength records according to GB/T1043;
Flexural strength records according to GB/T9341;
Load deformation temperature is more according to GB/T1634, and pressure is to record under 8.00MPa.
From above-mentioned table 1, table 2 and table 3, the phenolaldehyde moulding compound making by technique of the present invention has the mechanical electric performance close with external advanced same type of material, and shock strength, electrical strength and load deformation temperature wherein are obviously better than German PF51 material especially; In addition, the phenolaldehyde moulding compound that technique of the present invention makes is that in three kinds of techniques (technique of the present invention, to flaxen fiber process of surface treatment, any raw material is not carried out to the technique that surface treatment directly mixes), shock strength, flexural strength and water-absorbent performance are best; The phenolaldehyde moulding compound being made by technique of the present invention is compared with the moulding compound that flaxen fiber process of surface treatment is made, keep under the constant condition of other performance basic, (unnotched impact strength has at least improved 18.2% to have higher unnotched impact strength and flexural strength, flexural strength has at least improved 26.3%), and water-absorbent lower (water-absorbent has at least reduced by 18.5%).
Claims (10)
1. flaxen fiber strengthens the preparation method of injection phenolic moulding plastics, it is characterized in that: the raw material of preparing this flaxen fiber enhancing injection phenolic moulding plastics mainly contains lacquer resins, hexamethylenetetramine, mineral filler and flaxen fiber, and the preparation method that described flaxen fiber strengthens injection phenolic moulding plastics comprises the following steps:
1) take each raw material, for subsequent use;
2) get mineral filler coupling agent and carry out surface treatment, specifically by coupling agent with mineral filler is placed in ball mill or ball grinder ball milling is even, the consumption of described coupling agent is 0.5～10wt% of mineral filler consumption, and described mineral filler is one or more the combination being selected from aluminium hydroxide, silicon powder, calcite, talcum, calcium carbonate, glass microballon, kaolin and potter's clay powder;
3) get hexamethylenetetramine and pulverize, then mix with surface treated mineral filler and other raw material;
4) material mixing being dropped into twin screw extruder extrudes;
5) the cooling rear pulverizing of extruded stock, to obtain final product.
2. preparation method according to claim 1, is characterized in that: step 2) in, the rotating speed 10～60rpm of described ball mill or ball grinder, Ball-milling Time is 10～120min.
3. preparation method according to claim 1, is characterized in that: step 2) in, the consumption of described coupling agent is 4～6wt% of mineral filler consumption.
4. preparation method according to claim 1, is characterized in that: the barrel temperature of described twin screw extruder is 75～100 DEG C, and screw rod revolution is 70～90rpm.
5. according to the preparation method described in any one in claim 1～4, it is characterized in that: the raw material that the described flaxen fiber of preparation strengthens injection phenolic moulding plastics also comprises promotor, lubricant and dyestuff.
6. preparation method according to claim 5, is characterized in that: the weight proportion that the described flaxen fiber of preparation strengthens the raw material of injection phenolic moulding plastics is:
Lacquer resins 100;
Hexamethylenetetramine 10～20;
Mineral filler 20～90;
Length is the flaxen fiber 25～65 of 1～10mm;
Promotor 0.5～8;
Lubricant 1～8;
Dyestuff 0～10.
7. preparation method according to claim 6, is characterized in that: the weight proportion that the described flaxen fiber of preparation strengthens each raw material of injection phenolic moulding plastics is:
Lacquer resins 100;
Hexamethylenetetramine 13～18;
Mineral filler 30～80;
Length is the flaxen fiber 35～55 of 1～10mm;
Promotor 1～5;
Lubricant 2～5;
Dyestuff 0～6.
8. preparation method according to claim 6, is characterized in that: described promotor being is selected from one or more the combination in magnesium hydroxide, calcium hydroxide, magnesium oxide and calcium oxide.
9. preparation method according to claim 6, is characterized in that: described lubricant is one or more the combination being selected from calcium stearate, Zinic stearas, ethylene stearylamide, stearic acid and stearin.
10. the flaxen fiber that in claim 1～9, described in any one, method prepares strengthens injection phenolic moulding plastics.
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