CN102993630A - Preparation method of halogen-free flame-retardant no-ammonia-release phenolic glass reinforced plastic material - Google Patents
Preparation method of halogen-free flame-retardant no-ammonia-release phenolic glass reinforced plastic material Download PDFInfo
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- CN102993630A CN102993630A CN2012103004927A CN201210300492A CN102993630A CN 102993630 A CN102993630 A CN 102993630A CN 2012103004927 A CN2012103004927 A CN 2012103004927A CN 201210300492 A CN201210300492 A CN 201210300492A CN 102993630 A CN102993630 A CN 102993630A
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Abstract
The invention discloses a preparation method of a halogen-free flame-retardant no-ammonia-release phenolic glass reinforced plastic material, and belongs to the technical field of preparation of high-molecular materials. The preparation method comprises the following steps of: firstly, putting 40-44 parts of phenolic resin, 26-30 parts of thermosetting phenol resin, 4-5 parts of epoxy resin, 1.8-3.2 parts of metallic oxide, 1.5-2.6 parts of composite mold-releasing agent, 45-49 parts of mineral filler, 3-5 parts of silicon carbide and 28-33 parts of reinforced fiber weighed according to the weight parts into a container with a stirring device; mixing 20-30 minutes, and controlling the rotating speed of the stirring device to be 400-600n/min, thereby obtaining a mixture; transferring the mixture to an open mill for open milling for 12-16 minutes; then carrying out piece pulling, cooling to normal temperature, and grinding to obtain the halogen-free flame-retardant no-ammonia-release phenolic glass reinforced plastic material. The halogen-free flame-retardant no-ammonia-release phenolic glass reinforced plastic material has the advantages that the heat resistance is good, the strength is ideal and the ammonia can not be released in forming; and by test, the bending strength is more than 85MPa, the heat distortion temperature is higher than or equal to 240 DEG C, and the flame retardancy reaches V-0 grade (UL-94-V-01.6mm).
Description
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to a kind of phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof.
Background technology
Can discharge a certain amount of ammonia when the resol moulding, ammonia has strong impulse, impacts to production environment.In addition, the flame retardant resistance of the resol in prior art shortcoming.In view of this, help to make the phenolic fiberglass reinforced plastics material of preparation to overcome described shortcoming and have positive effect.For this reason, the applicant has done trial repeatedly, has formed technical scheme described below.
Summary of the invention
Task of the present invention is to provide a kind of phenolic fiberglass reinforced plastics material preparation method that discharges without ammonia of halogen-free flameproof, and the phenolic fiberglass reinforced plastics material that is obtained by the method discharges ammonia when helping avoid moulding, be conducive to significantly improve flame retardant effect and be of value to and improve mechanical and physical performance.
Task of the present invention is finished like this, a kind of phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof, it is 40 ~ 44 parts in the resol that will take by weighing by weight, 26 ~ 30 parts of heat-reactive phenolic resins, 4 ~ 5 parts of Resins, epoxy, 1.8 ~ 3.2 parts of metal oxides, 1.5 ~ 2.6 parts of compound releasing agents, 45 ~ 49 parts of mineral fillers, 3 ~ 5 parts in silicon carbide, mix 20-30min in 28 ~ 33 parts of containers of putting into whipping appts of fortifying fibre, the rotating speed of whipping appts is controlled to be 400-600n/min, obtain compound, compound is transferred to mill opens refining 12-16min, then carry out pulling-on piece, be cooled to normal temperature and pulverizing, obtain the phenolic fiberglass reinforced plastics material without ammonia release of halogen-free flameproof.
In a specific embodiment of the present invention, described resol is the resol of Catalyzed by Oxalic Acid; Described heat-reactive phenolic resin is the resol of base catalysis.
In another specific embodiment of the present invention, described Resins, epoxy is bisphenol A epoxide resin; Described metal oxide is zinc oxide.
In another specific embodiment of the present invention, described compound releasing agent is that 30% calcium stearate and mass percent are 70% composite composition of Zinic stearas by mass percent.
In another specific embodiment of the present invention, described mineral filler is calcium carbonate.
Also have in the specific embodiment of the present invention, described silicon carbide is that length-to-diameter ratio is 150～200 silicon carbide fiber.
More of the present invention and in specific embodiment, described fortifying fibre is that length is the glass fibre of 6mm.
In of the present invention and then specific embodiment, described fire retardant is ammonium polyphosphate or melamine pyrophosphate.
The phenolic fiberglass reinforced plastics material that discharges without ammonia of the halogen-free flameproof of the inventive method preparation has that resistance toheat is good, intensity is desirable, can not discharge the strong point of ammonia during moulding; Through test, more than the flexural strength 85MPa, heat-drawn wire is more than or equal to 240 ℃, and flame retardant resistance reaches V-0 grade (UL-94-V-0 1.6mm).
Embodiment
Embodiment 1:
With 40 parts in the resol of the Catalyzed by Oxalic Acid that takes by weighing by weight, 28 parts in the resol of alkali (NaOH) catalysis, 4 parts of bisphenol A epoxide resins, 3.2 parts in zinc oxide, be that 30% calcium stearate and mass percent are 2 parts of 70% the composite compound releasing agents that forms of Zinic stearas by mass percent, 49 parts in calcium carbonate, length-to-diameter ratio is 5 parts of 150～200 silicon carbide fibers, length is to mix 20-30min in 30 parts in the glass fibre of 6mm and 7 parts of containers of putting into whipping appts of ammonium polyphosphate, the rotating speed of whipping appts is 400-600n/min, obtain compound, compound is transferred to mill opens refining 12-16min, then carry out successively pulling-on piece, be cooled to normal temperature and pulverizing, obtain the phenolic fiberglass reinforced plastics material without ammonia release of halogen-free flameproof.
Embodiment 2:
With 44 parts in the resol of the Catalyzed by Oxalic Acid that takes by weighing by weight, 26 parts in the resol of alkali (NaOH) catalysis, 5 parts of bisphenol A epoxide resins, 1.8 parts in zinc oxide, be that 30% calcium stearate and mass percent are 1.5 parts of 70% the composite compound releasing agents that forms of Zinic stearas by mass percent, carbonic acid Ca45 part, length-to-diameter ratio is 3.5 parts of 150～200 silicon carbide fibers, length is to mix 20-30min in 28 parts in the glass fibre of 6mm and 10 parts of containers of putting into whipping appts of melamine pyrophosphate, the rotating speed of whipping appts is 400-600n/min, obtain compound, compound is transferred to mill opens refining 12-16min, then carry out successively pulling-on piece, be cooled to normal temperature and pulverizing, obtain the phenolic fiberglass reinforced plastics material without ammonia release of halogen-free flameproof.
Embodiment 3:
With 43 parts in the resol of the Catalyzed by Oxalic Acid that takes by weighing by weight, 30 parts in the resol of alkali (NaOH) catalysis, 4.4 parts of bisphenol A epoxide resins, 2.4 parts in zinc oxide, be that 30% calcium stearate and mass percent are 2.6 parts of 70% the composite compound releasing agents that forms of Zinic stearas by mass percent, 47 parts in calcium carbonate, length-to-diameter ratio is 4.5 parts of 150～200 silicon carbide fibers, length is to mix 20-30min in 29 parts in the glass fibre of 6mm and 9 parts of containers of putting into whipping appts of ammonium polyphosphate, the rotating speed of whipping appts is 400-600n/min, obtain compound, compound is transferred to mill opens refining 12-16min, then carry out successively pulling-on piece, be cooled to normal temperature and pulverizing, obtain the phenolic fiberglass reinforced plastics material without ammonia release of halogen-free flameproof.
Embodiment 4:
With 42 parts in the resol of the Catalyzed by Oxalic Acid that takes by weighing by weight, 27 parts in the resol of alkali (NaOH) catalysis, 4.8 parts of bisphenol A epoxide resins, 2.8 parts in zinc oxide, be that 30% calcium stearate and mass percent are 1.8 parts of 70% the composite compound releasing agents that forms of Zinic stearas by mass percent, 46 parts in calcium carbonate, length-to-diameter ratio is 3.0 parts of 150～200 silicon carbide fibers, length is to mix 20-30min in 28.5 parts in the glass fibre of 6mm and 8 parts of containers of putting into whipping appts of ammonium polyphosphate, the rotating speed of whipping appts is 400-600n/min, obtain compound, compound is transferred to mill opens refining 12-16min, then carry out successively pulling-on piece, be cooled to normal temperature and pulverizing, obtain the phenolic fiberglass reinforced plastics material without ammonia release of halogen-free flameproof.
The phenolic fiberglass reinforced plastics material that discharges without ammonia 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:
Claims (8)
1.
A kind of phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof, it is characterized in that it is 40 ~ 44 parts in the resol that will take by weighing by weight, 26 ~ 30 parts of heat-reactive phenolic resins, 4 ~ 5 parts of Resins, epoxy, 1.8 ~ 3.2 parts of metal oxides, 1.5 ~ 2.6 parts of compound releasing agents, 45 ~ 49 parts of mineral fillers, 3 ~ 5 parts in silicon carbide, mix 20-30min in 28 ~ 33 parts of containers of putting into whipping appts of fortifying fibre, the rotating speed of whipping appts is controlled to be 400-600n/min, obtain compound, compound is transferred to mill opens refining 12-16min, then carry out pulling-on piece, be cooled to normal temperature and pulverizing, obtain the phenolic fiberglass reinforced plastics material without ammonia release of halogen-free flameproof.
2.
The phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof according to claim 1 is characterized in that described resol is the resol of Catalyzed by Oxalic Acid; Described heat-reactive phenolic resin is the resol of base catalysis.
3.
The phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof according to claim 1 is characterized in that described Resins, epoxy is bisphenol A epoxide resin; Described metal oxide is zinc oxide.
4.
The phenolic fiberglass reinforced plastics material preparation method that discharges without ammonia of halogen-free flameproof according to claim 1 is characterized in that described compound releasing agent is that 30% calcium stearate and mass percent are 70% composite composition of Zinic stearas by mass percent.
5.
The phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof according to claim 1 is characterized in that described mineral filler is calcium carbonate.
6.
The phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof according to claim 1 is characterized in that described silicon carbide is that length-to-diameter ratio is 150～200 silicon carbide fiber.
7.
The phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof according to claim 1 is characterized in that described fortifying fibre is that length is the glass fibre of 6mm.
8.
The phenolic fiberglass reinforced plastics material preparation method without ammonia release of halogen-free flameproof according to claim 1 is characterized in that described fire retardant is ammonium polyphosphate or melamine pyrophosphate
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| CN201210300492.7A CN102993630B (en) | 2012-08-22 | 2012-08-22 | Preparation method of halogen-free flame-retardant no-ammonia-release phenolic glass reinforced plastic material |
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| CN102993630B CN102993630B (en) | 2014-03-05 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072951A (en) * | 2014-06-18 | 2014-10-01 | 安徽宁国市高新管业有限公司 | High-performance glass fiber reinforced plastic composite material |
| CN105086366A (en) * | 2015-08-10 | 2015-11-25 | 南通德瑞森复合材料有限公司 | Glass fiber reinforced plastic |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1062150A (en) * | 1991-12-20 | 1992-06-24 | 西北工业大学 | Flame-retardant glass fibre reinforced plastic materals |
| CN101148912A (en) * | 2006-09-18 | 2008-03-26 | 陈天云 | Sandwich foam heat-insulating board directly synthesized from bakelite fiber glass resin |
| CN102134370A (en) * | 2011-01-11 | 2011-07-27 | 宁波华缘复合新材料有限公司 | Phenolic glass steel and subway evacuation platform made of same |
-
2012
- 2012-08-22 CN CN201210300492.7A patent/CN102993630B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1062150A (en) * | 1991-12-20 | 1992-06-24 | 西北工业大学 | Flame-retardant glass fibre reinforced plastic materals |
| CN101148912A (en) * | 2006-09-18 | 2008-03-26 | 陈天云 | Sandwich foam heat-insulating board directly synthesized from bakelite fiber glass resin |
| CN102134370A (en) * | 2011-01-11 | 2011-07-27 | 宁波华缘复合新材料有限公司 | Phenolic glass steel and subway evacuation platform made of same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072951A (en) * | 2014-06-18 | 2014-10-01 | 安徽宁国市高新管业有限公司 | High-performance glass fiber reinforced plastic composite material |
| CN104072951B (en) * | 2014-06-18 | 2016-08-24 | 安徽宁国市高新管业有限公司 | A kind of high-performance glass steel composite material |
| CN105086366A (en) * | 2015-08-10 | 2015-11-25 | 南通德瑞森复合材料有限公司 | Glass fiber reinforced plastic |
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| CN102993630B (en) | 2014-03-05 |
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Inventor after: Wang Haiqiang Inventor before: Zhu Xuezhong |
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Effective date of registration: 20170508 Address after: 266109, Qingdao, Shandong Chengyang District, Liuting Road, double Road West Airport Industrial Park, No. 1 South Road Patentee after: QINGDAO BAISHIYOU COMPOSITE MATERIAL MANUFACTURING CO.,LTD. Address before: Unit 2101-K No. 9 Beek building 518000 Guangdong city of Shenzhen province Nanshan District Guangdong streets High-tech Zone Central Road Research Patentee before: Shenzhen Gao Hang Intellectual Property Operation Co.,Ltd. Effective date of registration: 20170508 Address after: Unit 2101-K No. 9 Beek building 518000 Guangdong city of Shenzhen province Nanshan District Guangdong streets High-tech Zone Central Road Research Patentee after: Shenzhen Gao Hang Intellectual Property Operation Co.,Ltd. Address before: 215511 Jiangsu city of Suzhou province Changshou City Mei Li Town (Tongjiang Road North Road maintenance in) Patentee before: CHANGSHU CHIKUSHI MACHINERY Co.,Ltd. |