CN103937151B - The preparation method of cotton fiber reinforced injection type phenolic molding compound - Google Patents
The preparation method of cotton fiber reinforced injection type phenolic molding compound Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of cotton fiber reinforced injection type phenolic molding compound.Preparing raw material main novolak resin, hexamethylenetetramine, inorganic filler and the cotton fiber of this phenolaldehyde moulding compound, the preparation method of this phenolaldehyde moulding compound comprises the following steps: 1) weigh each raw material, standby；2) taking inorganic filler and coupling agent, to be placed in ball milling in ball mill or ball grinder uniform, the consumption of described coupling agent is the 0.5～10wt% of inorganic filler consumption, and described inorganic filler is one or more the combination in aluminium hydroxide, silicon powder, calcite, Talcum, calcium carbonate, glass microballoon, Kaolin and potter's clay powder；3) take hexamethylenetetramine to pulverize, then mix homogeneously with surface treated inorganic filler and other raw material；4) material mixed is put into double screw extruder extrusion；5) pulverize after extruded stock cooling, to obtain final product.Phenolaldehyde moulding compound mechanical property obtained by this method is higher, water absorption is lower.
Description
Technical field
The present invention relates to phenolaldehyde moulding compound, be specifically related to a kind of cotton fiber reinforced injection type phenolic molding compound
Preparation method.
Background technology
Phenolaldehyde moulding compound raw material is easy to get, with low cost, there is the features such as higher, the stable performance of mechanical strength
And be widely used, wherein can reach the most resistance to using cotton fiber as the phenolaldehyde moulding compound of reinforcing material
Mill performance and mechanical property, such as patent of invention and Publication No. CN1752136 of Publication No. CN1640930
Patent of invention, all disclose by adding cotton fiber or the like to improve the shock resistance of material
Technical scheme with wearability.But all can only use mold pressing owing to they selected formula decide them
Molding mode, and each parameter during compression molding is mostly by operator's Non-follow control, there is molding
The deficiency that technique is poor, production efficiency is low.Publication No. CN102417692A of application before the applicant
Patent of invention, discloses cotton fiber reinforced injection type phenolic molding compound and the preparation thereof of a kind of injection moldable
Method, the method, with linear phenol-aldehyde resin as matrix material, selects the cotton fiber of length-specific as enhancing
Material, and only with hexamethylenetetramine as firming agent, by adding inorganic filler and the promotion of suitable consumption
Agent, make that plastics can keep again plastics while having quick setting capabilities in injector barrel is good
Heat stability, so that these plastics can injection moulding；Relatively molded by the product of the method obtained by molding
The product of molding has more preferable mechanical property.But the mechanical property of the method obtained by molding product is special and inhales
Aqueous is the most not ideal enough.
Summary of the invention
The technical problem to be solved in the present invention is for existing injection molding using cotton fiber as reinforcing material
Phenolaldehyde moulding compound mechanical property and the dissatisfactory deficiency of water absorption, it is provided that a kind of new by being injected into
The preparation method of the cotton fiber reinforced injection type phenolic molding compound of type, phenolaldehyde moulding compound obtained by this method
Mechanical property is higher, water absorption is lower.
The preparation method of cotton fiber reinforced injection type phenolic molding compound of the present invention, is wherein used for preparing
The raw material main novolak resin of this cotton fiber reinforced injection type phenolic molding compound, hexamethylenetetramine,
Inorganic filler and cotton fiber, the preparation method of this cotton fiber reinforced injection type phenolic molding compound specifically include with
Lower step:
1) each raw material is weighed, standby；
2) take inorganic filler coupling agent and carry out surface process, specifically coupling agent and inorganic filler are placed in
In ball mill or ball grinder, ball milling is uniform, the consumption of described coupling agent be inorganic filler consumption 0.5～
10wt%, described inorganic filler be selected from aluminium hydroxide, silicon powder, calcite, Talcum, calcium carbonate,
One or more combination in glass microballoon, Kaolin and potter's clay powder；
3) take hexamethylenetetramine to pulverize, then mix with surface treated inorganic filler and other raw material
Close uniformly；
4) material mixed is put into double screw extruder extrusion；
5) pulverize after extruded stock cooling, to obtain final product.
The inorganic filler coupling agent of specific consumption is first carried out ball milling modification process by the method for the invention,
It is effectively increased the interface compatibility between hydrophilic inorganic filler and oil loving phenolic resin as matrix resin, makes
Inorganic filler when mixing with phenolic resin as matrix resin and other raw material, inorganic filler and matrix and other raw material
Between cohesive force be remarkably reinforced, so that plastics are can be while injection moulding, moreover it is possible to make to mould
Mechanical property such as impact strength, the bending strength etc. of material are increased dramatically, and water absorption is greatly reduced.
In above-mentioned preparation method, the raw material being used for preparing described cotton fiber reinforced injection type phenolic molding compound leads to
Often also include accelerator and lubricant, may also include dyestuff further.Prepare described cotton fiber and strengthen injection
Proportioning between each raw material of type phenolaldehyde moulding compound as reinforcing material and can be adopted using cotton fiber with existing
Identical by the convenient source proportioning of injection molding phenolaldehyde moulding compound, the weight proportion of concrete each raw material can
To be:
Linear phenol-aldehyde resin 100；
Hexamethylenetetramine 10～20；
Inorganic filler 20～90；
The cotton fiber 25～65 of a length of 1～10mm；
Accelerator 0.5～8；
Lubricant 1～8；
Dyestuff 0～10.
The weight proportion of each raw material is more preferably:
Linear phenol-aldehyde resin 100；
Hexamethylenetetramine 13～18；
Inorganic filler 30～80；
The cotton fiber 35～55 of a length of 1～10mm；
Accelerator 1～5；
Lubricant 2～5；
Dyestuff 0～6.
Accelerator in above-mentioned raw materials can be selected from magnesium hydroxide, calcium hydroxide, magnesium oxide and calcium oxide
In one or more combination.It is chosen as above two or two or more combinations when accelerator
Time, the proportioning between them can be any proportioning.
Lubricant in above-mentioned raw materials can be selected from calcium stearate, zinc stearate, ethylene stearmide,
One or more combination in stearic acid and tristerin.When lubricant be chosen as above-mentioned
During two or more combination, the proportioning between them can be any proportioning.
Dyestuff in above-mentioned raw materials can be the one in nigrosine, phthalocyanine blue, phthalocyanine green and iron oxide red
Or two or more combinations.When being chosen as above two or two or more combinations of dyestuff, they it
Between proportioning can be any proportioning.
Cotton fiber described in above-mentioned raw materials is preferably the cotton fiber of a length of 2～6mm.
The step 2 of above-mentioned preparation method) in, preferably control ball mill or the rotating speed 10 of ball grinder～
60rpm, Ball-milling Time is 10～120min, so that the product of final molding is obtained in that more preferable mechanics
Performance and water absorption.
The step 2 of above-mentioned preparation method) in, described coupling agent can be silane coupler, titanate esters
Coupling agent or aluminate coupling agent, the consumption of described coupling agent is preferably the 3～8wt% of inorganic filler consumption,
More preferably the 4～6wt% of inorganic filler consumption.
The step 2 of above-mentioned preparation method) in, described inorganic filler is preferably selected from silicon powder, Fang Xie
One or more combination in stone, Talcum, calcium carbonate and glass microballoon, more preferably side
One or more combination in Xie Shi, calcium carbonate and glass microballoon.When being chosen as of inorganic filler
When above two or two or more combinations, the proportioning between them can be any proportioning.
The step 3 of above-mentioned preparation method) in, generally it is crushed to hexamethylenetetramine be not less than 80 mesh.
The step 4 of above-mentioned preparation method) in, when extruding with double screw extruder, generally arrange
The barrel temperature of double screw extruder is 75～100 DEG C, and screw rod revolution is 70～90rpm.
The step 5 of above-mentioned preparation method) in, it is crushed to the rule of a diameter of 1～6mm after extruded stock cooling
Or irregular granular.
The cotton fiber reinforced injection type phenolic molding compound prepared by the inventive method, its simply supported beam non-notch rushes
Hit intensity is at 10.0kJ/m2Above, simply supported beam notch impact strength is at 2.9kJ/m2Above, bending strength exists
More than 105Mpa.
Technique during the moulding compound thermoset injection machine injection moulding that said method prepares is as follows: mould temperature
Degree is 150～190 DEG C, and barrel temperature is 80～100 DEG C, and injection pressure is 60～100MPa, during solidification
Between be 10～20s/mm.
Compared with prior art, the method for the invention by with the coupling agent of specific consumption to inorganic filler
Carry out ball-milling treatment, on the one hand, make coupling agent molecule uniformly be wrapped in inorganic filler surface, reduce and fill out
Occur between material reunite probability, improve the dispersibility of filler, make inorganic filler with phenolic resin base
When body and other raw material mix, the cohesive force between inorganic filler and matrix and other raw material is substantially increased
By force, so that plastics are can be while injection moulding, moreover it is possible to make plastics mechanical property such as impact strength,
Bending strengths etc. are increased dramatically；On the other hand, the hydrophilic group of coupling agent and the hydroxyl of filling surface
Interact and form hydrogen bond, reduce the content of filling surface hydroxyl, thus hydroxyl when constraining curing molding
The probability that base interacts with moisture in air；It addition, the filler through coupling agent surface treatment mixes at postorder
Closing in step, the interface compatibility being effectively increased between filler and resin, filler is combined closely with resin
Together, reduce the surface area of filler, enable the free hydroxyl group with aqueous phase interaction and reduce, furthermore,
Coupling agent itself also forms hydrophobic coat at filling surface, can effectively slow down the rate of water absorption of plastics, therefore,
The water absorption of gained plastics is greatly reduced.
Detailed description of the invention
With embodiment, the present invention is further described below, but the invention is not limited in that these are implemented
Example.
Double screw extruder used in following embodiment is thermosetting parallel dual-screw extruding machine.
Number described in following embodiment is weight portion.
Embodiment 1
1) following component is weighed standby: linear phenol-aldehyde resin (i.e. thermoplastic phenolic resin, lower same) 100
Part, 35 parts of the cotton fiber of hexamethylenetetramine 13 parts, the silicon powder 80 parts of 400 mesh, a length of 2mm,
5 parts of magnesium hydroxide, calcium stearate 5 parts, nigrosine 6 parts；
2) take silicon powder and be equivalent to the titanate coupling agent of its consumption 1% and be placed in ball grinder and carry out ball
Mill, controls the rotating speed 50rpm of ball grinder, and Ball-milling Time is 20min；
3) take hexamethylenetetramine and be crushed to 80 mesh, then with surface treated silicon powder and other group
Divide mix homogeneously；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is 75～100 DEG C, and screw rod revolution is 70rpm；
5) the irregular granular of a diameter of 1～6mm, i.e. get Ben Fa it are crushed to after extruded stock is cooled to room temperature
Bright described cotton fiber reinforced injection type phenolic molding compound.
Comparative example 1
1) with the step 1 of embodiment 1)；
2) taking cotton fiber carries out conventional surface process with the titanate coupling agent being equivalent to its consumption 1%；
3) take hexamethylenetetramine and be crushed to 80 mesh, then with surface treated cotton fiber and other group
Divide mix homogeneously；
4) with the step 4 of embodiment 1)；
5) it is crushed to the irregular granular of a diameter of 1～6mm after extruded stock is cooled to room temperature, is contrasted
Cotton fiber reinforced injection type phenolic molding compound.
Embodiment 2
1) weigh following component standby: linear phenol-aldehyde resin 100 parts, hexamethylenetetramine 15 parts, 600
50 parts of purpose calcite, 45 parts of the cotton fiber of a length of 3mm, 2 parts of magnesium hydroxide, zinc stearate 3
Part, iron oxide red 4 parts；
2) take calcite and be equivalent to the aluminate coupling agent of its consumption 4% and be placed in ball grinder and carry out ball
Mill, controls the rotating speed 60rpm of ball grinder, and Ball-milling Time is 100min；
3) take hexamethylenetetramine and be crushed to 100 mesh, then with surface treated calcite and other
Component mix homogeneously；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is 75～95 DEG C, and screw rod revolution is 90rpm；
5) the irregular granular of a diameter of 2～5mm, i.e. get Ben Fa it are crushed to after extruded stock is cooled to room temperature
Bright described cotton fiber reinforced injection type phenolic molding compound.
Comparative example 2
1) with the step 1 of embodiment 2)；
2) taking cotton fiber carries out conventional surface process with the aluminate coupling agent being equivalent to its consumption 4%；
3) take hexamethylenetetramine and be crushed to 100 mesh, then with surface treated cotton fiber and other
Component mix homogeneously；
4) with the step 4 of embodiment 2)；
5) it is crushed to the irregular granular of a diameter of 2～5mm after extruded stock is cooled to room temperature, is contrasted
Cotton fiber reinforced injection type phenolic molding compound.
Embodiment 3
1) following component is weighed by weight percentage standby: linear phenol-aldehyde resin 100 parts, six methines
Tetramine 18 parts, the calcium carbonate 30 parts of 300 mesh, 55 parts of the cotton fiber of a length of 5mm, calcium oxide 1 part,
Stearic acid 2 parts；
2) take calcium carbonate and be equivalent to the silane coupler of its consumption 0.5% and be placed in ball grinder and carry out ball
Mill, controls the rotating speed 10rpm of ball grinder, and Ball-milling Time is 120min；
3) take hexamethylenetetramine and be crushed to 80 mesh, then with surface treated calcium carbonate and other group
Divide mix homogeneously；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is 80～100 DEG C, and screw rod revolution is 77rpm；
5) the irregular granular of a diameter of 4～6mm, i.e. get Ben Fa it are crushed to after extruded stock is cooled to room temperature
Bright described cotton fiber reinforced injection type phenolic molding compound.
Comparative example 3
1) with the step 1 of embodiment 3)；
2) taking cotton fiber carries out conventional surface process with the silane coupler being equivalent to its consumption 0.5%；
3) take hexamethylenetetramine and be crushed to 80 mesh, then with surface treated cotton fiber and other group
Divide mix homogeneously；
4) with the step 4 of embodiment 3)；
5) it is crushed to the irregular granular of a diameter of 4～6mm after extruded stock is cooled to room temperature, is contrasted
Cotton fiber reinforced injection type phenolic molding compound.
Embodiment 4
1) following component is weighed by weight percentage standby: linear phenol-aldehyde resin 100 parts, six methines
Tetramine 20 parts, the glass microballoon 90 parts of 800 mesh, 25 parts of the cotton fiber of a length of 10mm, magnesium oxide 8
Part, glyceryl stearate 8 parts；
2) take glass microballoon and be equivalent to the aluminate coupling agent of its consumption 10% and be placed in ball grinder and carry out
Ball milling, controls the rotating speed 10rpm of ball grinder, and Ball-milling Time is 10min；
3) take hexamethylenetetramine and be crushed to 120 mesh, then with surface treated glass microballoon and
Its component mix homogeneously；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is 78～99 DEG C, and screw rod revolution is 80rpm；
5) it is crushed to the irregular granular of a diameter of 6mm after extruded stock is cooled to room temperature, obtains the present invention
Described cotton fiber reinforced injection type phenolic molding compound.
Comparative example 4
1) with the step 1 of embodiment 4)；
2) taking cotton fiber carries out conventional surface process with the aluminate coupling agent being equivalent to its consumption 10%；
3) take hexamethylenetetramine and be crushed to 120 mesh, then with surface treated cotton fiber and other
Component mix homogeneously；
4) with the step 4 of embodiment 4)；
5) it is crushed to the irregular granular of a diameter of 6mm after extruded stock is cooled to room temperature, obtains contrast
Cotton fiber reinforced injection type phenolic molding compound.
Embodiment 5
1) following component is weighed by weight percentage standby: linear phenol-aldehyde resin 100 parts, six methines
Tetramine 10 parts, 20 parts of the potter's clay powder of 600 mesh, 65 parts of the cotton fiber of a length of 8mm, magnesium hydroxide
0.5 part, ethylene stearmide 1 part；
2) take potter's clay powder and be equivalent to the silane coupler of its consumption 3% and be placed in ball grinder and carry out ball
Mill, controls the rotating speed 30rpm of ball grinder, and Ball-milling Time is 60min；
3) take hexamethylenetetramine and be crushed to 160 mesh, then with surface treated potter's clay powder and
Its component mix homogeneously；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is 81～96 DEG C, and screw rod revolution is 83rpm；
5) it is crushed to the irregular granular of a diameter of 2mm after extruded stock is cooled to room temperature, obtains the present invention
Described cotton fiber reinforced injection type phenolic molding compound.
Comparative example 5
1) with the step 1 of embodiment 5)；
2) taking cotton fiber carries out conventional surface process with the silane coupler being equivalent to its consumption 3%；
3) take hexamethylenetetramine and be crushed to 160 mesh, then with surface treated cotton fiber and other
Component mix homogeneously；
4) with the step 4 of embodiment 5)；
5) it is crushed to the irregular granular of a diameter of 2mm after extruded stock is cooled to room temperature, obtains contrast
Cotton fiber reinforced injection type phenolic molding compound.
Embodiment 6
1) following component is weighed by weight percentage standby: linear phenol-aldehyde resin 100 parts, six methines
Tetramine 12 parts, 200～600 mesh aluminium hydroxide 50 parts, a length of 2～5mm 35 parts of cotton fiber,
Calcium oxide 5 parts, zinc stearate 3 parts；
2) take aluminium hydroxide and be equivalent to the silane coupler of its consumption 8% and be placed in ball grinder and carry out ball
Mill, controls the rotating speed 40rpm of ball grinder, and Ball-milling Time is 80min；
3) take hexamethylenetetramine and be crushed to 160 mesh, then with surface treated aluminium hydroxide and
Its component mix homogeneously；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is 81～96 DEG C, and screw rod revolution is 83rpm；
5) the irregular granular of a diameter of 3～5mm, i.e. get Ben Fa it are crushed to after extruded stock is cooled to room temperature
Bright described cotton fiber reinforced injection type phenolic molding compound.
Comparative example 6
1) with the step 1 of embodiment 6)；
2) taking cotton fiber carries out conventional surface process with the silane coupler being equivalent to its consumption 8%；
3) take hexamethylenetetramine and be crushed to 160 mesh, then with surface treated cotton fiber and other
Component mix homogeneously；
4) with the step 4 of embodiment 6)；
5) it is crushed to the irregular granular of a diameter of 3～5mm after extruded stock is cooled to room temperature, is contrasted
Cotton fiber reinforced injection type phenolic molding compound.
Embodiment 7
Except by the consumption of silane coupler is calcium carbonate in addition to 6%, other is the most same as in Example 3.
Respectively by obtained by the phenolaldehyde moulding compound obtained by above-described embodiment 1～7 and comparative example 1～6
Phenolaldehyde moulding compound respectively with thermoset injection machine by following technique injection moulding: mold temperature is 170 DEG C,
Barrel temperature is 90 DEG C, and injection pressure is 60MPa, and hardening time is 20s/mm.The moulding compound of gained
Mechanical electric performance comparison is carried out, shown in the following Tables 1 and 2 of result with German PF51 phenolaldehyde moulding compound:
Table 1:
Table 2:
Above impact strength records according to GB/T1043；
Bending 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 Tables 1 and 2, the phenolaldehyde moulding compound prepared by technique of the present invention have with
The mechanical electric performance that external advanced same type of material is close, impact strength therein, electrical strength and load
Deformation temperature is substantially better than Germany's PF51 material especially；It addition, the phenolic aldehyde mould that technique of the present invention prepares
Plastics, compared with the moulding compound preparing cotton fiber process of surface treatment, keep other performance constant basic
Under conditions of, (unnotched impact strength at least carries to have higher unnotched impact strength and bending strength
High by 12.9%, bending strength at least improves 10.2%), and water absorption is lower, and (water absorption at least reduces
23.7%).
Claims (9)
1. the preparation method of cotton fiber reinforced injection type phenolic molding compound, it is characterised in that: preparation should
The raw material main novolak resin of cotton fiber reinforced injection type phenolic molding compound, six methines four
Amine, inorganic filler and cotton fiber, the preparation method bag of described cotton fiber reinforced injection type phenolic molding compound
Include following steps:
1) each raw material is weighed, standby；
2) take inorganic filler coupling agent and carry out surface process, specifically coupling agent and inorganic filler are put
In ball mill or ball grinder, ball milling is uniform, and the consumption of described coupling agent is inorganic filler consumption
0.5～10wt%, described inorganic filler is calcium carbonate；
3) take hexamethylenetetramine to pulverize, then with surface treated inorganic filler and other raw material
Mix homogeneously；
4) material mixed is put into double screw extruder extrusion；
5) pulverize after extruded stock cooling, to obtain final product.
Preparation method the most according to claim 1, it is characterised in that: step 2) in, described
The rotating speed 10～60rpm of ball mill or ball grinder, Ball-milling Time is 10～120min.
Preparation method the most according to claim 1, it is characterised in that: step 2) in, institute
State consumption is inorganic filler consumption the 4～6wt% of coupling agent.
Preparation method the most according to claim 1, it is characterised in that: step 4) in, institute
The barrel temperature stating double screw extruder is 75～100 DEG C, and screw rod revolution is 70～90rpm.
5. according to the preparation method according to any one of Claims 1 to 4, it is characterised in that: preparation
The raw material of described cotton fiber reinforced injection type phenolic molding compound also includes accelerator, lubricant and dye
Material.
Preparation method the most according to claim 5, it is characterised in that: the cotton fibre described in preparation
The weight proportion of the raw material that dimension strengthens injection phenolic moulding plastics is:
Linear phenol-aldehyde resin 100；
Hexamethylenetetramine 10～20；
Inorganic filler 20～90；
The cotton fiber 25～65 of a length of 1～10mm；
Accelerator 0.5～8；
Lubricant 1～8；
Dyestuff 0～10.
Preparation method the most according to claim 6, it is characterised in that: the cotton fibre described in preparation
The weight proportion of each raw material that dimension strengthens injection phenolic moulding plastics is:
Linear phenol-aldehyde resin 100；
Hexamethylenetetramine 13～18；
Inorganic filler 30～80；
The cotton fiber 35～55 of a length of 1～10mm；
Accelerator 1～5；
Lubricant 2～5；
Dyestuff 0～6.
Preparation method the most according to claim 6, it is characterised in that: described accelerator is
One or more combination in magnesium hydroxide, calcium hydroxide, magnesium oxide and calcium oxide.
Preparation method the most according to claim 6, it is characterised in that: described lubricant is
In calcium stearate, zinc stearate, ethylene stearmide, stearic acid and tristerin one
Kind or two or more combinations.
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| CN101747585A (en) * | 2008-12-16 | 2010-06-23 | 宝山钢铁股份有限公司 | Method for preparing thermosetting plastic with coal gangue modified phenolic resin |
| CN102115653A (en) * | 2009-12-31 | 2011-07-06 | 比亚迪股份有限公司 | Binding agent composition, preparation method and application thereof |
| 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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2014
- 2014-04-20 CN CN201410165136.8A patent/CN103937151B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101747585A (en) * | 2008-12-16 | 2010-06-23 | 宝山钢铁股份有限公司 | Method for preparing thermosetting plastic with coal gangue modified phenolic resin |
| CN102115653A (en) * | 2009-12-31 | 2011-07-06 | 比亚迪股份有限公司 | Binding agent composition, preparation method and application thereof |
| 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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