CN103937151A - Preparation method of cotton-fiber-reinforced injection-type phenol aldehyde molding compound - Google Patents
Preparation method of cotton-fiber-reinforced injection-type phenol aldehyde molding compound Download PDFInfo
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- CN103937151A CN103937151A CN201410165136.8A CN201410165136A CN103937151A CN 103937151 A CN103937151 A CN 103937151A CN 201410165136 A CN201410165136 A CN 201410165136A CN 103937151 A CN103937151 A CN 103937151A
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Abstract
The invention discloses a preparation method of a cotton-fiber-reinforced injection-type phenol aldehyde molding compound. The phenol aldehyde molding compound is mainly prepared from linear phenol aldehyde resin, hexamethylenetetramine, inorganic filler and cotton fiber. 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 ceramic 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 preparation method of cotton fiber reinforced injection type phenolic molding compound.
Background technology
Phenolaldehyde moulding compound raw material is easy to get, with low cost, there is mechanical strength compared with features such as high, stable performances and be widely used, wherein the phenolaldehyde moulding compound using cotton fibre as strongthener can reach good wear resisting property and mechanical property, as the patent of invention that the publication number patent of invention that is CN1640930 and publication number are CN1752136, all disclose by adding cotton fibre or similar substance to improve the shock resistance of material and the technical scheme of wear resistance.But all can only adopt the molding mode of mold pressing because their selected formulas are determining them, and each parameter in compression molding process manually controlled by operator mostly, have the deficiency that moulding process is poor, production efficiency is low.The patent of invention that before the applicant, the publication number of application is CN102417692A, cotton fiber reinforced injection type phenolic molding compound of a kind of injection moldable and preparation method thereof is disclosed, the method is taking lacquer resins as body material, select the cotton fibre of length-specific as strongthener, and only taking hexamethylenetetramine as solidifying agent, by adding mineral filler and the promotor of suitable consumption, make plastics in thering is fast setting ability, can keep again the good thermal stability of plastics in injector barrel, thereby make these plastics can injection molding; Product by the relative compression molding of product of the method obtained by molding has better mechanical property.But the mechanical property of the method obtained by molding product is special and water-absorbent is still not ideal enough.
Summary of the invention
The technical problem to be solved in the present invention is using cotton fibre as the injection molding phenolaldehyde moulding compound mechanical property of strongthener and the dissatisfactory deficiency of water-absorbent for existing, a kind of new preparation method who passes through injection molding cotton fiber reinforced injection type phenolic molding compound is provided, and phenolaldehyde moulding compound mechanical property obtained by this method is higher, water-absorbent is lower.
The preparation method of cotton fiber reinforced injection type phenolic molding compound of the present invention, the raw material that is wherein used for preparing this cotton fiber reinforced injection type phenolic molding compound mainly contains lacquer resins, hexamethylenetetramine, mineral filler and cotton fibre, and the preparation method of this cotton fiber reinforced injection type phenolic molding compound 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, the raw material that is used for preparing described cotton fiber reinforced injection type phenolic molding compound also comprises promotor and lubricant conventionally, further also can comprise dyestuff.Preparing proportioning between each raw material of described cotton fiber reinforced injection type phenolic molding compound can be with existing using cotton fibre as strongthener and adopt the conventional proportioning raw materials of injection molding phenolaldehyde moulding compound identical, and the weight proportion of concrete each raw material can be:
Lacquer resins 100;
Hexamethylenetetramine 10～20;
Mineral filler 20～90;
Length is the cotton fibre 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 cotton fibre 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.
Cotton fibre described in above-mentioned raw materials is preferably the cotton fibre that length is 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.
Above-mentioned preparation method's step 3) in, conventionally hexamethylenetetramine is crushed to and is not less than 80 orders.
Above-mentioned preparation method's step 4) in, in the time extruding with twin screw extruder, the barrel temperature that twin screw extruder is set is conventionally 75～100 DEG C, 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 cotton fiber reinforced injection type phenolic molding compound being made by the inventive method, its simply supported beam unnotched impact strength 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: 5 parts of 5 parts of 35 parts, cotton fibre, magnesium hydroxides, calcium stearates, 6 parts of nigrosine that 100 parts of lacquer resinss (be novolac resin, lower with), 13 parts of hexamethylenetetramines, 80 parts of 400 object silicon powders, length are 2mm;
2) titanate coupling agent of getting silicon powder and being equivalent to its consumption 1% is placed in ball grinder and carries out ball milling, controls the rotating speed 50rpm of ball grinder, and Ball-milling Time is 20min;
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 75～100 DEG C, and screw rod revolution is 70rpm;
5) extruded stock is crushed to the irregular granular that diameter is 1～6mm after being cooled to normal temperature, obtains cotton fiber reinforced injection type phenolic molding compound of the present invention.
Comparative example 1
1) with the step 1 of embodiment 1);
2) taking cotton fiber carries out conventional surface treatment with the titanate coupling agent that is equivalent to its consumption 1%;
3) get hexamethylenetetramine and be crushed to 80 orders, then mix with surface treated cotton fibre 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, obtains the cotton fiber reinforced injection type phenolic molding compound of contrast.
Embodiment 2
1) take following component for subsequent use: 3 parts of 2 parts of 45 parts, cotton fibre, magnesium hydroxides, Zinic stearass, 4 parts of iron oxide reds that 100 parts of lacquer resinss, 15 parts of hexamethylenetetramines, 50 parts, 600 object calcite, length are 3mm;
2) aluminate coupling agent of getting calcite and being equivalent to its consumption 4% 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 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 75～95 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 cotton fiber reinforced injection type phenolic molding compound of the present invention.
Comparative example 2
1) with the step 1 of embodiment 2);
2) taking cotton fiber carries out conventional surface treatment with the aluminate coupling agent that is equivalent to its consumption 4%;
3) get hexamethylenetetramine and be crushed to 100 orders, then mix with surface treated cotton fibre 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, obtains the cotton fiber reinforced injection type phenolic molding compound of contrast.
Embodiment 3
1) take by weight percentage following component for subsequent use: 1 part, 55 parts, cotton fibre, calcium oxide, 2 parts of stearic acid that 100 parts of lacquer resinss, 18 parts of hexamethylenetetramines, 30 parts, 300 object calcium carbonate, length are 5mm;
2) silane coupling agent of getting calcium carbonate 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 120min;
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 80～100 DEG C, and screw rod revolution is 77rpm;
5) extruded stock is crushed to the irregular granular that diameter is 4～6mm after being cooled to normal temperature, obtains cotton fiber reinforced injection type phenolic molding compound of the present invention.
Comparative example 3
1) with the step 1 of embodiment 3);
2) taking cotton fiber carries out conventional surface treatment with the silane coupling agent that is equivalent to its consumption 0.5%;
3) get hexamethylenetetramine and be crushed to 80 orders, then mix with surface treated cotton fibre 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, obtains the cotton fiber reinforced injection type phenolic molding compound of contrast.
Embodiment 4
1) take by weight percentage following component for subsequent use: 8 parts, 25 parts, cotton fibre, magnesium oxide, 8 parts of glyceryl stearates that 100 parts of lacquer resinss, 20 parts of hexamethylenetetramines, 90 parts of 800 object glass microballons, length are 10mm;
2) aluminate coupling agent of getting glass microballon and being equivalent to its consumption 10% 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 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 78～99 DEG C, and screw rod revolution is 80rpm;
5) extruded stock is crushed to the irregular granular that diameter is 6mm after being cooled to normal temperature, obtains cotton fiber reinforced injection type phenolic molding compound of the present invention.
Comparative example 4
1) with the step 1 of embodiment 4);
2) taking cotton fiber carries out conventional surface treatment with the aluminate coupling agent that is equivalent to its consumption 10%;
3) get hexamethylenetetramine and be crushed to 120 orders, then mix with surface treated cotton fibre 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, obtains the cotton fiber reinforced injection type phenolic molding compound of contrast.
Embodiment 5
1) take by weight percentage following component for subsequent use: 0.5 part of 65 parts, cotton fibre, magnesium hydroxide, 1 part of ethylene stearylamide that 100 parts of lacquer resinss, 10 parts of hexamethylenetetramines, 600 20 parts, object potter's clay powder, length are 8mm;
2) silane coupling agent of getting potter's clay powder and being equivalent to its consumption 3% 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 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 81～96 DEG C, and screw rod revolution is 83rpm;
5) extruded stock is crushed to the irregular granular that diameter is 2mm after being cooled to normal temperature, obtains cotton fiber reinforced injection type phenolic molding compound of the present invention.
Comparative example 5
1) with the step 1 of embodiment 5);
2) taking cotton fiber carries out conventional surface treatment with the silane coupling agent that is equivalent to its consumption 3%;
3) get hexamethylenetetramine and be crushed to 160 orders, then mix with surface treated cotton fibre 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, obtains the cotton fiber reinforced injection type phenolic molding compound of contrast.
Embodiment 6
1) take by weight percentage following component for subsequent use: 5 parts, 35 parts, cotton fibre, calcium oxide, 3 parts of Zinic stearass that 100 parts of lacquer resinss, 12 parts of hexamethylenetetramines, 50 parts, 200～600 object aluminium hydroxide, length are 2～5mm;
2) silane coupling agent of getting aluminium hydroxide and being equivalent to its consumption 8% is placed in ball grinder and carries out ball milling, controls the rotating speed 40rpm of ball grinder, and Ball-milling Time is 80min;
3) get hexamethylenetetramine and be crushed to 160 orders, then mix with surface treated aluminium hydroxide and other component;
4) material mixing is dropped into twin screw extruder and extrude, the barrel temperature of described twin screw extruder is 81～96 DEG C, and screw rod revolution is 83rpm;
5) extruded stock is crushed to the irregular granular that diameter is 3～5mm after being cooled to normal temperature, obtains cotton fiber reinforced injection type phenolic molding compound of the present invention.
Comparative example 6
1) with the step 1 of embodiment 6);
2) taking cotton fiber carries out conventional surface treatment with the silane coupling agent that is equivalent to its consumption 8%;
3) get hexamethylenetetramine and be crushed to 160 orders, then mix with surface treated cotton fibre and other component;
4) with the step 4 of embodiment 6);
5) extruded stock is crushed to the irregular granular that diameter is 3～5mm after being cooled to normal temperature, obtains the cotton fiber reinforced injection type phenolic molding compound of contrast.
Embodiment 7
Except being calcium carbonate by the consumption of silane coupling agent 6%, other is all identical with embodiment 3.
Respectively by prepared above-described embodiment 1～7 phenolaldehyde moulding compound and the prepared phenolaldehyde moulding compound of comparative example 1～6 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 and table 2:
Table 1:
Table 2:
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 and table 2, 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 compared with the moulding compound that cotton fibre process of surface treatment is made, keep under the constant condition of other performance basic, (unnotched impact strength has at least improved 12.9% to have higher unnotched impact strength and flexural strength, flexural strength has at least improved 10.2%), and water-absorbent lower (water-absorbent has at least reduced by 23.7%).
Claims (10)
1. the preparation method of cotton fiber reinforced injection type phenolic molding compound, it is characterized in that: the raw material of preparing this cotton fiber reinforced injection type phenolic molding compound mainly contains lacquer resins, hexamethylenetetramine, mineral filler and cotton fibre, and the preparation method of described cotton fiber reinforced injection type phenolic molding compound 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: step 2) in, described mineral filler is one or more the combination being selected from silicon powder, calcite, talcum, calcium carbonate and glass microballon.
5. preparation method according to claim 1, is characterized in that: step 4) in, the barrel temperature of described twin screw extruder is 75～100 DEG C, screw rod revolution is 70～90rpm.
6. according to the preparation method described in any one in claim 1～5, it is characterized in that: the raw material of the cotton fiber reinforced injection type phenolic molding compound described in preparation also comprises promotor, lubricant and dyestuff.
7. preparation method according to claim 6, is characterized in that: the weight proportion of the raw material of the cotton fiber reinforced injection type phenolic molding compound described in preparation is:
Lacquer resins 100;
Hexamethylenetetramine 10～20;
Mineral filler 20～90;
Length is the cotton fibre 25～65 of 1～10mm;
Promotor 0.5～8;
Lubricant 1～8;
Dyestuff 0～10.
8. preparation method according to claim 7, is characterized in that: the weight proportion of each raw material of the cotton fiber reinforced injection type phenolic molding compound described in preparation is:
Lacquer resins 100;
Hexamethylenetetramine 13～18;
Mineral filler 30～80;
Length is the cotton fibre 35～55 of 1～10mm;
Promotor 1～5;
Lubricant 2～5;
Dyestuff 0～6.
9. preparation method according to claim 7, 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.
10. preparation method according to claim 7, 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.
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| CN112761017A (en) * | 2020-12-31 | 2021-05-07 | 广东华凯科技股份有限公司 | Method for preparing high-hardness fiberboard with bamboo fiber as raw material |
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| CN102417692A (en) * | 2011-11-08 | 2012-04-18 | 桂林电器科学研究院 | Cotton fiber reinforced injection type phenolic molding compound and preparation method thereof |
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Effective date of registration: 20180111 Address after: 541004 the Guangxi Zhuang Autonomous Region Dongcheng Qixing District, Guilin City Road No. 8 Patentee after: Guilin Jinge Electrotechnical Electronic Material Science & Technology Co., Ltd. Address before: 541004 the Guangxi Zhuang Autonomous Region Dongcheng Qixing District, Guilin City Road No. 8 Patentee before: Guilin Electrical Equipment Scientific Research Institute Co., Ltd. |