CN102993632A - Preparation method of halogen-free flame-retardant phenolic composite material - Google Patents

Preparation method of halogen-free flame-retardant phenolic composite material Download PDF

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Publication number
CN102993632A
CN102993632A CN2012103005440A CN201210300544A CN102993632A CN 102993632 A CN102993632 A CN 102993632A CN 2012103005440 A CN2012103005440 A CN 2012103005440A CN 201210300544 A CN201210300544 A CN 201210300544A CN 102993632 A CN102993632 A CN 102993632A
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parts
halogen
preparation
phenolic composite
free flameproof
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CN2012103005440A
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朱雪忠
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CHANGSHU CHIKUSHI MACHINERY Co Ltd
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CHANGSHU CHIKUSHI MACHINERY Co Ltd
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Abstract

The invention discloses a preparation method of a halogen-free flame-retardant phenolic composite material, and belongs to the technical field of preparation of thermosetting molding materials. The preparation method comprises the following steps of: firstly, putting 28-35 parts of mineral filler, 17-22 parts of reinforced fiber and 0.7-1.1 parts of surface treating agent weighed according to the weight parts into a stirring container, and mixing for 10-20 minutes; then putting 32-36 parts of phenolic resin, 3-4 parts of polymethyl methacrylate resin, 2.5-5.5 parts of a curing agent, 0.8-1.5 parts of a curing accelerant, 5-7 parts of a flame retardant agent, 1.5-2.5 parts of an antibacterial agent and 0.8-1.6 parts of a mold releasing agent weighed according to the weight parts into the stirring container, mixing for 35-45 minutes, then transferring the materials to an open mill, and carrying out hot mixing for 4-8 minutes; and finally, carrying out piece pulling, cooling and grinding to obtain the halogen-free flame-retardant phenolic composite material. The halogen-free flame-retardant phenolic composite material disclosed by the invention has the characteristics of good strength, convenient formation, good flame retardancy and the like; and by test, the bending strength is 85MPa, the heat distortion temperature is 240 DEG C, and the flame retardancy reaches UL-94-V-0 grade (0.8mm).

Description

The preparation method of the phenolic composite of halogen-free flameproof
Technical field
The invention belongs to the duroplastic moulding materials preparing technical field, be specifically related to a kind of preparation method of phenolic composite of halogen-free flameproof.
Background technology
Phenolic composite excellent performance and be widely used in daily necessities field, but the performance that the flame retardant properties of phenolic composite, antibacterium corrode always receives the concern of industry, and the phase is got improvement, lag behind people's requirement in view of the flame retardant resistance of the phenolic composite of the halogen-free flameproof in the prior art and germ resistance etc., therefore the phenolic composite of exploring the halogen-free flameproof that is prepared into to remedy these shortcomings has positive realistic meaning, through the applicant's exploration and trial for many years, be about to the technical scheme of introducing below having formed.
Summary of the invention
Task of the present invention is to provide a kind of preparation method of phenolic composite of halogen-free flameproof, and the phenolic composite of the halogen-free flameproof that is obtained by the method has significant fire-retardant and antibacterium erosion effect.
Task of the present invention is finished like this, a kind of preparation method of phenolic composite of halogen-free flameproof, it is 28 ~ 35 parts of the mineral fillers that will take by weighing by weight first, 0.7 ~ 1.1 part of 17 ~ 22 parts of fortifying fibres and surface treatment agent are put into and are mixed 10-20min in the stirred vessel, 32 ~ 36 parts in the resol that will take by weighing by weight again, 3 ~ 4 parts of plexiglasses, 2.5 ~ 5.5 parts in solidifying agent, 0.8 ~ 1.5 part of curing catalyst, 0.8 ~ 1.6 part of 5 ~ 7 parts of fire retardants and 1.5 ~ 2.6 parts of antiseptic-germicides and releasing agent are put into and are mixed 35-45min in the stirred vessel, then be transferred to mill and carry out heat mixing 4-8min, at last successively through pulling-on piece, cool off and pulverizing, obtain the phenolic composite of halogen-free flameproof.
In a specific embodiment of the present invention, described resol is the resol that acid system is produced.
In another specific embodiment of the present invention, the molecular weight of described plexiglass is 50,000.
In another specific embodiment of the present invention, described solidifying agent is hexamethylene tetramine; Described curing catalyst is zinc oxide.
In another specific embodiment of the present invention, described fire retardant is ammonium polyphosphate; Described antiseptic-germicide is 2-sulfenyl-1-pyridine oxide zinc.
Also have in the specific embodiment of the present invention, described releasing agent is calcium stearate; Described mineral filler is calcium carbonate or aluminium hydroxide.
More of the present invention and in specific embodiment, described surface treatment agent is anilinomethyl triethoxysilane.
In of the present invention and then specific embodiment, described fortifying fibre is the alkali free glass fibre of length 3mm.
The phenolic composite of the halogen-free flameproof of the inventive method preparation have excellent antibacterial effect and have that intensity is good, the characteristics such as convenient formation and good flame resistance, through test, flexural strength 85MPa, 240 ℃ of heat-drawn wires, flame retardant properties reach UL-94-V-0 level (0.8mm).
Embodiment
Embodiment 1:
35 parts in the calcium carbonate that will take by weighing by weight first, length is that 0.7 part of 22 parts of the alkali free glass fibres of 3mm and anilinomethyl triethoxysilane is put into and mixed 10-20min in the stirred vessel, rotating speed 400-450n/min, 36 parts in the resol that is obtained by acid system production that will take by weighing by weight again, molecular weight is 3 parts of 50,000 plexiglasses, 4 parts of hexamethylene tetramines, 0.8 part in zinc oxide, 7 parts of ammonium polyphosphates, 0.8 part of 2 parts of 2-sulfenyls-1-pyridine oxide zinc and calcium stearate are put into and are mixed 35-45min in the stirred vessel, then be transferred to mill and carry out heat mixing 4-8min, at last successively through pulling-on piece, cool off and pulverizing, obtain the phenolic composite of halogen-free flameproof.
Embodiment 2:
28 parts of hydroxide Lu that will take by weighing by weight first, length is that 0.9 part of 19 parts of the alkali free glass fibres of 3mm and anilinomethyl triethoxysilane is put into and mixed 10-20min in the stirred vessel, rotating speed 400-450n/min, 32 parts in the resol that is obtained by acid system production that will take by weighing by weight again, molecular weight is 3.2 parts of 50,000 plexiglasses, 5.5 parts of hexamethylene tetramines, 1.0 parts in zinc oxide, 5 parts of ammonium polyphosphates, 1.0 parts of 1.5 parts of 2-sulfenyls-1-pyridine oxide zinc and calcium stearates are put into and are mixed 35-45min in the stirred vessel, then be transferred to mill and carry out heat mixing 4-8min, at last successively through pulling-on piece, cool off and pulverizing, obtain the phenolic composite of halogen-free flameproof.
Embodiment 3:
31 parts in the calcium carbonate that will take by weighing by weight first, length is that 1.1 parts of 17 parts of the alkali free glass fibres of 3mm and anilinomethyl triethoxysilanes are put into and mixed 10-20min in the stirred vessel, rotating speed 400-450n/min, 33 parts in the resol that is obtained by acid system production that will take by weighing by weight again, molecular weight is 3.6 parts of 50,000 plexiglasses, 2.5 parts of hexamethylene tetramines, 1.2 parts in zinc oxide, 5.5 parts of ammonium polyphosphates, 1.3 parts of 2.6 parts of 2-sulfenyls-1-pyridine oxide zinc and calcium stearates are put into and are mixed 35-45min in the stirred vessel, then be transferred to mill and carry out heat mixing 4-8min, at last successively through pulling-on piece, cool off and pulverizing, obtain the phenolic composite of halogen-free flameproof.
Embodiment 4:
24 parts in the calcium carbonate that will take by weighing by weight first, length is that 1.0 parts of 21 parts of the alkali free glass fibres of 3mm and anilinomethyl triethoxysilanes are put into and mixed 10-20min in the stirred vessel, rotating speed 400-450n/min, 35 parts in the resol that is obtained by acid system production that will take by weighing by weight again, molecular weight is 4 parts of 50,000 plexiglasses, 3.5 parts of hexamethylene tetramines, 1.5 parts in zinc oxide, 6.5 parts of ammonium polyphosphates, 1.6 parts of 2.1 parts of 2-sulfenyls-1-pyridine oxide zinc and calcium stearates are put into and are mixed 35-45min in the stirred vessel, then be transferred to mill and carry out heat mixing 4-8min, at last successively through pulling-on piece, cool off and pulverizing, obtain the phenolic composite of halogen-free flameproof.
The phenolic composite of the halogen-free flameproof that is obtained by above-described embodiment 1-4 has the technique effect shown in the following table after tested:
Figure BDA0000204424611

Claims (8)

1. A kind of preparation method of phenolic composite of halogen-free flameproof, it is characterized in that it is 28 ~ 35 parts of the mineral fillers that will take by weighing by weight first, 0.7 ~ 1.1 part of 17 ~ 22 parts of fortifying fibres and surface treatment agent are put into and are mixed 10-20min in the stirred vessel, 32 ~ 36 parts in the resol that will take by weighing by weight again, 3 ~ 4 parts of plexiglasses, 2.5 ~ 5.5 parts in solidifying agent, 0.8 ~ 1.5 part of curing catalyst, 0.8 ~ 1.6 part of 5 ~ 7 parts of fire retardants and 1.5 ~ 2.6 parts of antiseptic-germicides and releasing agent are put into and are mixed 35-45min in the stirred vessel, then be transferred to mill and carry out heat mixing 4-8min, at last successively through pulling-on piece, cool off and pulverizing, obtain the phenolic composite of halogen-free flameproof.
2. The preparation method of the phenolic composite of halogen-free flameproof according to claim 1 is characterized in that described resol is the resol that acid system is produced.
3. The preparation method of the phenolic composite of halogen-free flameproof according to claim 1, the molecular weight that it is characterized in that described plexiglass is 50,000.
4. The preparation method of the phenolic composite of halogen-free flameproof according to claim 1 is characterized in that described solidifying agent is hexamethylene tetramine; Described curing catalyst is zinc oxide.
5. The preparation method of the phenolic composite of halogen-free flameproof according to claim 1 is characterized in that described fire retardant is ammonium polyphosphate; Described antiseptic-germicide is 2-sulfenyl-1-pyridine oxide zinc.
6. The preparation method of the phenolic composite of halogen-free flameproof according to claim 1 is characterized in that described releasing agent is calcium stearate; Described mineral filler is calcium carbonate or aluminium hydroxide.
7. The preparation method of the phenolic composite of halogen-free flameproof according to claim 1 is characterized in that described surface treatment agent is anilinomethyl triethoxysilane.
8. The preparation method of the phenolic composite of halogen-free flameproof according to claim 1 is characterized in that described fortifying fibre is the alkali free glass fibre of length 3mm
CN2012103005440A 2012-08-22 2012-08-22 Preparation method of halogen-free flame-retardant phenolic composite material Pending CN102993632A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105061984A (en) * 2015-09-18 2015-11-18 南通联恒新材料有限公司 Flame-retardant antimicrobial phenolic plastic
CN105694082A (en) * 2016-03-17 2016-06-22 合肥晨煦信息科技有限公司 Preparation method of high temperature resistant and corrosion resistant composite material
CN106117958A (en) * 2016-06-30 2016-11-16 禹州市远大塑料电器有限责任公司 A kind of antibacterial phenolaldehyde moulding compound
CN106117957A (en) * 2016-06-30 2016-11-16 禹州市远大塑料电器有限责任公司 A kind of fire-retardant antibacterial phenolaldehyde moulding compound

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1412240A (en) * 2001-10-16 2003-04-23 上海欧亚合成材料有限公司 Antibacterial phenolic moulding plastics
CN101343397A (en) * 2008-08-22 2009-01-14 常熟东南塑料有限公司 Halogen-free flame-proof phenolic plastic

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1412240A (en) * 2001-10-16 2003-04-23 上海欧亚合成材料有限公司 Antibacterial phenolic moulding plastics
CN101343397A (en) * 2008-08-22 2009-01-14 常熟东南塑料有限公司 Halogen-free flame-proof phenolic plastic

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105061984A (en) * 2015-09-18 2015-11-18 南通联恒新材料有限公司 Flame-retardant antimicrobial phenolic plastic
CN105694082A (en) * 2016-03-17 2016-06-22 合肥晨煦信息科技有限公司 Preparation method of high temperature resistant and corrosion resistant composite material
CN106117958A (en) * 2016-06-30 2016-11-16 禹州市远大塑料电器有限责任公司 A kind of antibacterial phenolaldehyde moulding compound
CN106117957A (en) * 2016-06-30 2016-11-16 禹州市远大塑料电器有限责任公司 A kind of fire-retardant antibacterial phenolaldehyde moulding compound

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Application publication date: 20130327