CN105778375A - Halogen-free flame retardant DAP molding compound capable of being prepared through injection molding and preparation method thereof - Google Patents
Halogen-free flame retardant DAP molding compound capable of being prepared through injection molding and preparation method thereof Download PDFInfo
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- CN105778375A CN105778375A CN201610366840.9A CN201610366840A CN105778375A CN 105778375 A CN105778375 A CN 105778375A CN 201610366840 A CN201610366840 A CN 201610366840A CN 105778375 A CN105778375 A CN 105778375A
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- C08L31/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid; Compositions of derivatives of such polymers
- C08L31/06—Homopolymers or copolymers of esters of polycarboxylic acids
- C08L31/08—Homopolymers or copolymers of esters of polycarboxylic acids of phthalic acid
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/14—Peroxides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The invention discloses a halogen-free flame retardant DAP molding compound capable of being prepared through injection molding and a preparation method thereof. The halogen-free flame retardant DAP molding compound capable of being prepared through injection molding is prepared from, by weight, 20-35% of DAP resin, 1-10% of a crosslinking agent, 0.01-0.06% of a polymerization inhibitor, 0.2-1.5% of a fire retardant, 25-65% of filler, 1-3% of a releasing agent and 15-30% of reinforced fiber. The molding compound will not be subjected to crosslinking curing within the barrel temperature range lower than 100 DEG C, a nozzle will not be blocked in the plasticizing process, and continuous molding can be performed; during follow-up injection molding, rapid reaction can be performed under high temperature, and meanwhile it can be ensured that the molding compound is rapidly cured in a mold; the obtained molding compound is high in surface resistance, volume resistance and bending strength, the thermal deformation temperature is higher than 240 DEG C, and the flame retardance can reach the UL-94-V-0 level.
Description
Technical field
The present invention relates to duroplastic moulding materials, be specifically related to a kind of injection moldable halogen-free flameproof DAP molding
Material and preparation method thereof.
Background technology
Along with electric and electronic component develop towards miniaturization and ultrathin direction, to be applied to this type of zero
The flame-retardancy requirements of DAP (diallyl phthalate) moulding compound of parts is more and more higher.Prior art institute
The DAP mold compound curing temperature prepared with curing system is low, the time is short, uses thermoset injection machine molding,
May in barrel crosslinking curing the most, cause nozzle to block, therefore, existing DAP moulding compound can only be adopted
With molding or the moulding process of transmission.But, mold and transfer molding exist the deficiency that production efficiency is low,
Limit the use of DAP moulding compound.There are no at present injection moldable halogen-free flameproof DAP moulding compound and
The relevant report of preparation method.
Summary of the invention
The technical problem to be solved in the present invention be for DAP moulding compound in prior art can only use mold pressing or
The deficiency of crimping and transfer processes molding, it is provided that a kind of injection moldable halogen-free flameproof DAP moulding compound and preparation side thereof
Method, this moulding compound does not contains halogen and excellent fireproof performance, can also use injection moulding simultaneously.
Injection moldable halogen-free flameproof DAP moulding compound of the present invention, by weight percentage by following
Component forms:
DAP resin 20%-35%；
Cross-linking agent 1%-10%；
Polymerization inhibitor 0.01%-0.06%；
Fire retardant 0.2%-1.5%；
Filler 25%-65%；
Releasing agent 1%-3%
Reinforcing fiber 15%-30%.
In technique scheme:
The selection of described cross-linking agent is same as the prior art, preferably benzoyl peroxide diisopropylbenzene (DIPB) and/or peroxide
Change t-butyl perbenzoate.It is chosen as benzoyl peroxide diisopropylbenzene (DIPB) and the tertiary fourth of perbenzoic acid when cross-linking agent
During the combination of ester, the proportioning between them can be any proportioning.
Described polymerization inhibitor is the one in hydroquinone, tert-butyl hydroquinone and 1,4-benzoquinone or two
Plant above combination, when the combination being chosen as the above material of above two of polymerization inhibitor, between them
Proportioning can be any proportioning.
Described fire retardant is the most halogen-containing fire retardant in prior art, is preferably selected from Firebrake ZB, red
One or more combination in phosphorus and tripolycyanamide.It is chosen as more than above two when fire retardant
During the combination of material, the proportioning between them can be any proportioning.
The selection of described filler is same as the prior art, be preferably selected from calcium carbonate, silica flour, Kaolin,
One or more combination in aluminium hydroxide and magnesium hydroxide.It is chosen as above two when filler
During the combination of above material, the proportioning between them can be any proportioning.
The selection of described releasing agent is same as the prior art, be preferably selected from calcium stearate, zinc stearate,
One or more combination in magnesium stearate and stearic acid.It is chosen as above two when releasing agent
During the combination of above material, the proportioning between them can be any proportioning.
Described reinforcing fiber can be alkali-free glass fibre, basalt fibre or acicular wollastonite, or
It is the heatproof organic fiber such as chopped aramid fiber, polyester fiber or nylon fiber of a length of 1mm to 6mm,
Or the most two or more combination in above-mentioned selection.It is chosen as more than above two when reinforcing fiber
During the combination of material, the proportioning between them can be any proportioning.
DAP resin described in technical scheme of the present invention is diallyl phthalate resin.
The present invention also provides for the preparation method of above-mentioned injection moldable halogen-free flameproof DAP moulding compound, including with
Lower step:
1) each component is weighed by formula, standby；
2) take filler coupling agent and carry out conventional surface process；
3) take DAP resin, surface treated filler and other component mix homogeneously, mixed
Material；
4) gained mixed material is put into double screw extruder extrusion；
5) pulverize after extruded stock cooling, to obtain final product.
The step 2 of said method) in, described coupling agent can be selected from silane coupler, titanate esters occasionally
Connection agent and aluminate coupling agent in any one, wherein from silane coupler, titanate coupling agent and aluminum
The selection of acid esters coupling agent is same as the prior art.The consumption of described coupling agent is usually amount of filler
0.5%-3%.
The step 4 of said method) in, when extruding with double screw extruder, twin screw is generally set
The barrel temperature of extruder is 75-100 DEG C, and screw rod revolution is 100-120rpm.
The step 5 of said method) in, it is crushed to the rule or not of a diameter of 2mm-5mm after extruded stock cooling
The granular of rule.
The moulding compound that said method prepares uses technique during thermoset injection machine injection moulding as follows: mould
Temperature is 170-185 DEG C, and barrel temperature is 60-70 DEG C, and nozzle temperature is 70-85 DEG C, and injection pressure is
30-60MPa, hardening time is 30-50s/mm.
Compared with prior art, the present invention DAP resin and various components are carried out reasonably combined after add
The polymerization inhibitor of special ratios, it is ensured that gained moulding compound will not be handed in the range of the barrel temperature less than 100 DEG C
Connection solidification so that it is will not block up nozzle in plasticizing process, can be continuously shaped；Height when subsequent injections molding
Can fast reaction under the conditions of temperature, it is ensured that moulding compound solidifies the most rapidly, only overcome DAP moulding compound
Can use and mold or the deficiency of transfer molding；The moulding compound surface resistivity prepared by formula of the present invention
More than 2.0E+15 Ω, specific insulation is more than 1.0E+12 Ω m, and bending strength is more than 90MPa, heat
Deformation temperature is more than 240 degrees Celsius, and fire resistance can reach UL-94-V-0 level (0.8mm).
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, to be more fully understood that the present invention
Content, but the present invention is not limited to following example.
Embodiment 1
1) each component is weighed by following percentage by weight standby: DAP resin 25%, benzoyl peroxide diisopropylbenzene (DIPB)
5%, hydroquinone 0.03%, Firebrake ZB 1.5%, aluminium hydroxide 52.47%, zinc stearate 1%, chopped is gathered
Ester fiber 15%；
2) take the filler silane coupler being equivalent to its consumption 0.5% and carry out conventional surface process；
3) take DAP resin to mix homogeneously with surface treated filler and other component；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is for 75-80 DEG C, and screw rod revolution is 100rpm；
5) pulverize after extruded stock cooling, i.e. obtain injection moldable halogen-free flameproof DAP mould of the present invention
Plastics.
Embodiment 2
1) each component is weighed by following percentage by weight standby: DAP resin 35%, the tertiary fourth of perbenzoic acid
Ester 6%, tert-butyl hydroquinone 0.02%, red phosphorus 1.5%, magnesium hydroxide 38.98%, calcium stearate 1.5%,
Glass fibre 17%；
2) take the filler silane coupler being equivalent to its consumption 1% and carry out conventional surface process；
3) take DAP resin to mix homogeneously with surface treated filler and other component；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is for 95-100 DEG C, and screw rod revolution is 110rpm；
5) pulverize after extruded stock cooling, i.e. obtain injection moldable halogen-free flameproof DAP of the present invention molding
Material.
Embodiment 3
1) each component is weighed by following percentage by weight standby: DAP resin 27.5%, perbenzoic acid uncle
Butyl ester 5%, 1,4-benzoquinone 0.06%, tripolycyanamide 0.5%, magnesium hydroxide 40.44%, stearic acid 1.5%,
Basalt fibre 25%；
2) take the filler aluminate coupling agent being equivalent to its consumption 2% and carry out conventional surface process；
3) take DAP resin to mix homogeneously with surface treated filler and other component；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is for 85-95 DEG C, and screw rod revolution is 120rpm；
5) pulverize after extruded stock cooling, i.e. obtain injection moldable halogen-free flameproof DAP of the present invention molding
Material.
Embodiment 4
1) each component is weighed by following percentage by weight standby: DAP resin 23%, benzoyl peroxide diisopropylbenzene (DIPB)
4%, hydroquinone 0.01%, Firebrake ZB 0.2%, silica flour 39.79%, stearic acid 3%, acicular wollastonite
30%；
2) take the filler aluminate coupling agent being equivalent to its consumption 3% and carry out conventional surface process；
3) take DAP resin to mix homogeneously with surface treated filler and other component；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is for 80-90 DEG C, and screw rod revolution is 100rpm；
5) pulverize after extruded stock cooling, i.e. obtain injection moldable halogen-free flameproof DAP of the present invention molding
Material.
Embodiment 5
1) each component is weighed by following percentage by weight standby: DAP resin 20%, benzoyl peroxide diisopropylbenzene (DIPB)
2%, tert-butyl hydroquinone 0.01%, red phosphorus 1%, Kaolin 57.99%, magnesium stearate 2%, chopped virtue
Synthetic fibre fiber 17%；
2) take the filler titanate coupling agent being equivalent to its consumption 2% and carry out conventional surface process；
3) take DAP resin to mix homogeneously with surface treated filler and other component；
4) material mixed is put into double screw extruder extrusion, the barrel temperature of described double screw extruder
Degree is for 90-95 DEG C, and screw rod revolution is 115rpm；
5) pulverize after extruded stock cooling, i.e. obtain injection moldable halogen-free flameproof DAP of the present invention molding
Material.
The injection moldable halogen-free flameproof DAP moulding compound thermosetting respectively above-described embodiment 1-5 prepared
Injector is by following moulding process injection moulding: mold temperature is 170 DEG C, and barrel temperature is 75 DEG C, spray
Mouth temperature is 85 DEG C, and injection pressure is 60MPa, and hardening time is 40s/mm.Each embodiment is the most continuously
Molding 4h, each 120 moulds, forming process is continuous, smooth, product good rigidly smooth, hot full, bright,
Qualification rate is all higher than 96%.
The moulding compound prepared above-described embodiment 1-5 respectively is tested, and acquired results is as shown in the table:
Claims (8)
1. an injection moldable halogen-free flameproof DAP moulding compound, it is characterised in that: percentage by weight
It is made up of following component than meter:
DAP resin 20%-35%；
Cross-linking agent 1%-10%；
Polymerization inhibitor 0.01%-0.06%；
Fire retardant 0.2%-1.5%；
Filler 25%-65%；
Releasing agent 1%-3%；
Reinforcing fiber 15%-30%.
Injection moulding halogen-free flameproof DAP moulding compound the most according to claim 1, its feature exists
In: described cross-linking agent is benzoyl peroxide diisopropylbenzene (DIPB) and/or peroxidized t-butyl perbenzoate.
Injection moulding halogen-free flameproof DAP moulding compound the most according to claim 1, its feature exists
In: described polymerization inhibitor be the one in hydroquinone, tert-butyl hydroquinone and 1,4-benzoquinone or
Two or more combinations.
Injection moulding halogen-free flameproof DAP moulding compound the most according to claim 1, its feature exists
In: described fire retardant is one or more in Firebrake ZB, red phosphorus and tripolycyanamide
Combination.
Injection moulding halogen-free flameproof DAP moulding compound the most according to claim 1, its feature exists
In: described filler is in calcium carbonate, silica flour, Kaolin, aluminium hydroxide and magnesium hydroxide
One or more combination.
Injection moulding halogen-free flameproof DAP moulding compound the most according to claim 1, its feature exists
In: described releasing agent is in calcium stearate, zinc stearate, magnesium stearate and stearic acid
Kind or two or more combinations.
Injection moulding halogen-free flameproof DAP moulding compound the most according to claim 1, its feature exists
In: described reinforcing fiber is glass fibre, basalt fibre or acicular wollastonite, or length
For the chopped aramid fiber of 1mm to 6mm, polyester fiber, nylon fiber, or above-mentioned any two
Plant the combination of above material.
8. the preparation method of injection moldable halogen-free flameproof DAP moulding compound described in claim 1, bag
Include following steps:
1) each component is weighed by formula, standby；
2) take filler coupling agent and carry out conventional surface process；
3) take DAP resin, surface treated filler and other component mix homogeneously, mixed
Compound material；
4) gained mixed material is put into double screw extruder extrusion；
5) pulverize after extruded stock cooling, to obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610366840.9A CN105778375A (en) | 2016-05-27 | 2016-05-27 | Halogen-free flame retardant DAP molding compound capable of being prepared through injection molding and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610366840.9A CN105778375A (en) | 2016-05-27 | 2016-05-27 | Halogen-free flame retardant DAP molding compound capable of being prepared through injection molding and preparation method thereof |
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| CN105778375A true CN105778375A (en) | 2016-07-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610366840.9A Pending CN105778375A (en) | 2016-05-27 | 2016-05-27 | Halogen-free flame retardant DAP molding compound capable of being prepared through injection molding and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591406A (en) * | 2018-06-13 | 2019-12-20 | 郑州深澜动力科技有限公司 | Low-density high-flame-retardant SMC battery pack material, preparation method thereof and battery pack |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1389880A (en) * | 1972-07-28 | 1975-04-09 | Fmc Corp | Diallyl phthalate moulding compositions |
-
2016
- 2016-05-27 CN CN201610366840.9A patent/CN105778375A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1389880A (en) * | 1972-07-28 | 1975-04-09 | Fmc Corp | Diallyl phthalate moulding compositions |
Non-Patent Citations (3)
| Title |
|---|
| 周殿明 主编: "《注塑工艺员手册》", 31 August 2009, 机械工业出版社 * |
| 山西省化工研究所 编: "《塑料橡胶加工助剂》", 31 October 2002, 化学工业出版社 材料科学与工程出版中心 * |
| 李光 主编: "《高分子材料加工工艺学》", 28 February 2010, 中国纺织出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591406A (en) * | 2018-06-13 | 2019-12-20 | 郑州深澜动力科技有限公司 | Low-density high-flame-retardant SMC battery pack material, preparation method thereof and battery pack |
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Application publication date: 20160720 |