CN102321340B - High-strength halogen-free epoxy molding compound, and preparation method thereof - Google Patents
High-strength halogen-free epoxy molding compound, and preparation method thereof Download PDFInfo
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- CN102321340B CN102321340B CN 201110274707 CN201110274707A CN102321340B CN 102321340 B CN102321340 B CN 102321340B CN 201110274707 CN201110274707 CN 201110274707 CN 201110274707 A CN201110274707 A CN 201110274707A CN 102321340 B CN102321340 B CN 102321340B
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Abstract
The invention discloses a high-strength halogen-free epoxy molding compound, and a preparation method thereof. The molding compound comprises raw materials of: 100 parts of modified epoxy resin, 0 to 100 parts of epoxy resin, 20 to 100 parts of a curing agent, 140 to 250 parts of a strengthening material, 100 to 250 parts of a filling material, 100 to 250 parts of a fire retardant and CTI modifier, and 10 to 50 parts of an auxiliary agent. The preparation method comprises steps that: the materials are well mixed, crushed, mixed, fused and mixed, cooled and crushed, and packaged. The preparation method of the modified epoxy resin comprises steps that: 100 parts of epoxy resin and 5 to 20 parts of liquid rubber are mixed for 4 to 6 hours under a temperature of 100 DEG C to 130 DEG C, the product is cooled, and the product is crushed to a size below 20 meshes. The invention is advantages in that: with the high-strength halogen-free epoxy molding compound prepared by the invention, the produced product has high mechanical strength, small molding shrinkage, good high/low temperature impact resistance, excellent electrical property under bad surroundings, and environment friendliness.
Description
Technical field
The present invention relates to a kind of reinforced epoxy molding compound and preparation method thereof, relate in particular to a kind of HS Halogen epoxy molding plastic that is applied to car electrics and encapsulation of wet type solenoid and moulding and preparation method thereof.
Background technology
In present car electrics and encapsulation of wet type solenoid and the employed material of moulding, reinforced epoxy molding compound has purposes widely.Reinforced epoxy molding compound is the special kinds in the epoxy molding plastic, and it had both had the wet fastness and the excellent electrical of general epoxy molding plastic, had higher physical strength again, so reinforced epoxy molding compound has irreplaceable purposes in a lot of fields.
But present its shortcoming of this reinforced epoxy molding compound is: the fragility of material is big, and molding shrinkage is big, and the creepage trace index (CTI) of material is low, can not satisfy the requirement of specialty products fully; And along with the lifting of environmental protection concept, original bromine-antimony fire retardant systems also is limited to use gradually.
Summary of the invention
The purpose of this invention is to provide a kind of HS Halogen epoxy molding plastic and preparation method thereof; Its main ingredient comprises modified epoxy, epoxy resin, linear phenolic resin, spun glass, synthon, silica powder, oxyhydroxide and auxiliary agent, to overcome the deficiency of mentioning in the above-mentioned prior art.
For realizing above-mentioned purpose, the present invention realizes through following technical scheme:
A kind of HS Halogen epoxy molding plastic, the proportioning of its feed composition is: 100 parts of modified epoxies, 0 ~ 100 part of epoxy resin; 20 ~ 100 parts in solidifying agent, 140 ~ 250 parts of strongtheners, 100 ~ 250 parts of fillers; 100 ~ 250 parts of fire retardant and CTI properties-correcting agent, 10 ~ 50 parts of auxiliary agents.
Said modified epoxy is the mixture of epoxy resin and fluid rubber, wherein 83 ~ 95 parts of epoxy resin, 5～17 parts of fluid rubbers.
Said fluid rubber is the TOUGHENING MODIFICATION OF EPOXY RESINS material, comprises Zylox, terminal hydroxy group rubber, nbr carboxyl terminal.
Said epoxy resin is one or more the mixture in bisphenol f type epoxy resin, F type epoxy resin, ortho-cresol type epoxy resin, the bisphenol A type epoxy resin.
Said solidifying agent is a linear phenolic resin, and softening temperature is 70 ~ 95 ℃.
Said filler is one or both the mixture in amorphous silica powder and the powdered quartz powder.
Said fire retardant and CTI properties-correcting agent are oxyhydroxide, the mixture of one or both in preferred especially white lake and the Marinco H.
Said strongthener is the mixture of spun glass and synthon, wherein 120 ~ 200 parts in spun glass, 20 ~ 50 parts of synthon.
Said synthon are chopped strand, and fiber length is 0.5～6.0 ㎜, preferred KevLar fiber, nylon fiber and trevira.
Said spun glass is alkali free glass fibre or middle alkali short glass fiber, and glass length is 0.5 ~ 6.0mm.
Said auxiliary agent is releasing agent and curing catalyst, and releasing agent comprises Triple Pressed Stearic Acid and saponified, montanic acid wax thereof and saponified, POLISHING WAX-103 thereof etc., and curing catalyst comprises promotor commonly used such as tertiary amines.
A kind of method for preparing HS Halogen epoxy molding plastic as claimed in claim 1, process through following steps:
(1) pulverize: resinous material is crushed to below 20 orders, and auxiliary powder is broken to below 200 orders;
(2) mix: each component is carried out the powder mixing after by 100 parts of modified epoxies, 0 ~ 100 part of epoxy resin, 20 ~ 100 parts in solidifying agent, 140 ~ 250 parts of strongtheners, 100 ~ 250 parts of fillers, fire retardant and 100 ~ 250 parts of CTI properties-correcting agent, 10 ~ 50 parts of meterings of auxiliary agent;
(3) melting mixing: add the screw type mixing equipment through the blended material by certain feed rate, continuous fusion mixes, 70 ~ 105 ℃ of mixing temperatures;
(4) cooling is pulverized: through cooling, utilize kibbler to pulverize;
(5) packing: directly be crushed to and make the finished product packing below the particle 2cm; Or after being crushed to below the particle 0.5mm, pack again after the first premolding.
The preparation method of said modified epoxy is: 100 parts of epoxy resin, 5～20 parts of fluid rubbers were mixed 4～6 hours down at 100 ℃～130 ℃, and cooling is crushed to below 20 orders.
Above feed composition all by weight.
Beneficial effect of the present invention is: the epoxy molding plastic that utilizes the preparation method of HS Halogen epoxy molding plastic of the present invention to obtain, the product of manufacturing has the physical strength height, molding shrinkage is little, moulding product high-low temperature resistant impact is good, advantage such as good, environmental protection of electrical property under the severe environment.
Embodiment
| Component | Concrete material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples |
| Modified epoxy | ? | 100 | 100 | 100 | 0 |
| Epoxy resin | ? | 0 | 10 | 10 | 100 |
| Solidifying agent | Linear phenolic resin | 40 | 40 | 40 | 40 |
| Strongthener | Spun glass | 120 | 145 | 120 | 145 |
| Strongthener | Synthon | 25 | 20 | 35 | 0 |
| Filler | Silicon-dioxide | 140 | 150 | 130 | 250 |
| Fire retardant and CTI properties-correcting agent | White lake | 100 | 0 | 50 | 0 |
| Fire retardant and CTI properties-correcting agent | Marinco H | 0 | 100 | 50 | 0 |
| Auxiliary agent | ? | 15 | 15 | 15 | 15 |
Above feed composition all by weight.
Embodiment 1:
A kind of method for preparing HS Halogen epoxy molding plastic, process HS Halogen epoxy molding plastic through following steps:
(1) pulverize: resinous material is crushed to below 20 orders, and auxiliary powder is broken to below 200 orders;
(2) mix: each component is pressed 100 parts of modified epoxies, 0 part of epoxy resin, and 40 parts of linear phenolic resins, 120 parts in spun glass, 25 parts of synthon, 40 parts of silica 1s, 100 parts in white lake carries out powder and mixes after 15 parts of meterings of auxiliary agent;
(3) melting mixing: add the screw type mixing equipment through the blended material by certain feed rate, continuous fusion mixes, 70 ~ 105 ℃ of mixing temperatures;
(4) cooling is pulverized: through cooling, utilize kibbler to pulverize;
(5) packing: directly be crushed to and make the finished product packing below the particle 2cm; Or after being crushed to below the particle 0.5mm, pack again after the first premolding.
The preparation method of said modified epoxy is: 100 parts of epoxy resin, 10 parts of fluid rubbers were mixed 4～6 hours down at 100 ℃～130 ℃, and cooling is crushed to below 20 orders.
Above feed composition all by weight.
Embodiment 2:
A kind of method for preparing HS Halogen epoxy molding plastic, process through following steps:
(1) pulverize: resinous material is crushed to below 20 orders, and auxiliary powder is broken to below 200 orders;
(2) mix: each component is pressed 100 parts of modified epoxies, 10 parts of epoxy resin, and 40 parts of linear phenolic resins, 145 parts in spun glass, 20 parts of synthon, 50 parts of silica 1s, 100 parts of Marinco Hs carry out powder and mix after 15 parts of meterings of auxiliary agent;
(3) melting mixing: add the screw type mixing equipment through the blended material by certain feed rate, continuous fusion mixes, 70 ~ 105 ℃ of mixing temperatures;
(4) cooling is pulverized: through cooling, utilize kibbler to pulverize;
(5) packing: directly be crushed to and make the finished product packing below the particle 2cm; Or after being crushed to below the particle 0.5mm, pack again after the first premolding.
The preparation method of said modified epoxy is: 100 parts of epoxy resin, 15 parts of fluid rubbers were mixed 4～6 hours down at 100 ℃～130 ℃, and cooling is crushed to below 20 orders.
Above feed composition all by weight.
Embodiment 3:
A kind of method for preparing HS Halogen epoxy molding plastic, process through following steps:
(1) pulverize: resinous material is crushed to below 20 orders, and auxiliary powder is broken to below 200 orders;
(2) mix: each component is pressed 100 parts of modified epoxies, 10 parts of epoxy resin, 40 parts of linear phenolic resins; 120 parts in spun glass, 35 parts of synthon, 30 parts of silica 1s; 50 parts in white lake, 50 parts of Marinco Hs carry out powder and mix after 15 parts of meterings of auxiliary agent;
(3) melting mixing: add the screw type mixing equipment through the blended material by certain feed rate, continuous fusion mixes, 70 ~ 105 ℃ of mixing temperatures;
(4) cooling is pulverized: through cooling, utilize kibbler to pulverize;
(5) packing: directly be crushed to and make the finished product packing below the particle 2cm; Or after being crushed to below the particle 0.5mm, pack again after the first premolding.
The preparation method of said modified epoxy is: 100 parts of epoxy resin, 10 parts of fluid rubbers were mixed 4～6 hours down at 100 ℃～130 ℃, and cooling is crushed to below 20 orders.
Above feed composition all by weight.
Do not use modified epoxy, synthon, fire retardant and CTI properties-correcting agent in the Comparative Examples, the evaluating characteristics of prepared epoxy molding plastic is to be used for that to carry out characteristic correlated with above-mentioned three embodiment as follows.
| Test event | Embodiment one | Embodiment two | Embodiment three | Comparative Examples |
| Flexural strength (Mpa) | 180 | 168 | 173 | 160 |
| Shock strength (KJ/ ㎡) | 15 | 13 | 16 | 11 |
| Tensile strength (Mpa) | 108 | 96 | 105 | 85 |
| Cure shrinkage (%) | 0.18 | 0.22 | 0.16 | 0.42 |
| CTI(V) | 400 | 400 | 400 | 175 |
All with the moulding of transfer mould molding mode, actual conditions is following in the making of the used sample of above-mentioned evaluating characteristics:
Preheating temperature: 70 ~ 90 ℃
Die temperature: 160 ± 5 ℃
Injection pressure: 7 ~ 8Mpa
Clamp time: 200 seconds
After fixing condition: 170 ℃ * 4hrs.
In addition, in the evaluating characteristics, flexural strength is according to the GB/T9341 standard testing, and shock strength is according to the GB/T1043 standard testing, and tensile strength is tested according to GB/T1040, and cure shrinkage is tested according to GB/T1404, and CTI presses the GB/T4207 test.
Claims (5)
1. HS Halogen epoxy molding plastic; It is characterized in that: the proportioning of its feed composition is: 100 parts of modified epoxies, 0～100 part of epoxy resin, 20～100 parts in solidifying agent; 140～250 parts of strongtheners; 100～250 parts of fillers, 100～250 parts of fire retardant and CTI properties-correcting agent, 10～50 parts of auxiliary agents; Wherein said modified epoxy is the mixture of epoxy resin and fluid rubber; Wherein 83～95 parts of epoxy resin, 5～17 parts of fluid rubbers; Said fluid rubber is the TOUGHENING MODIFICATION OF EPOXY RESINS material, comprises Zylox, terminal hydroxy group rubber, nbr carboxyl terminal; Said solidifying agent is a linear phenolic resin, and softening temperature is 70～95 ℃; Said filler is one or both the mixture in amorphous silica powder and the powdered quartz powder; Said strongthener is the mixture of spun glass and synthon, wherein 120～200 parts in spun glass, 20～50 parts of synthon; Said fire retardant and CTI properties-correcting agent are oxyhydroxide.
2. HS Halogen epoxy molding plastic as claimed in claim 1 is characterized in that: said epoxy resin is one or more in bisphenol f type epoxy resin, ortho-cresol type epoxy resin, the bisphenol A type epoxy resin.
3. HS Halogen epoxy molding plastic as claimed in claim 1 is characterized in that: said auxiliary agent is releasing agent and curing catalyst, and said releasing agent is one or more of Triple Pressed Stearic Acid and saponified, montanic acid wax thereof and saponified, POLISHING WAX-103 thereof.
4. HS Halogen epoxy molding plastic as claimed in claim 1 is characterized in that: said synthon are chopped strand, and fiber length is 0.5～6.0 ㎜; Said spun glass is alkali free glass fibre or middle alkali short glass fiber, and glass length is 0.5～6.0mm.
5. the preparation method of a HS Halogen epoxy molding plastic as claimed in claim 1 is characterized in that: process through following steps:
(1) pulverize: resinous material is crushed to below 20 orders, and auxiliary powder is broken to below 200 orders;
(2) mix: each component is carried out powder after by 100 parts of modified epoxies, 0～100 part of epoxy resin, 20～100 parts in solidifying agent, 140～250 parts of strongtheners, 100～250 parts of fillers, fire retardant and 100～250 parts of CTI properties-correcting agent, 10～50 parts of meterings of auxiliary agent and is mixed;
(3) melting mixing: add the screw type mixing equipment through the blended material by certain feed rate, continuous fusion mixes, 70～105 ℃ of mixing temperatures;
(4) cooling is pulverized: through cooling, utilize kibbler to pulverize;
(5) packing: directly be crushed to and make the finished product packing below the particle 2cm; Or after being crushed to below the particle 0.5mm, pack again after the first premolding.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110274707 CN102321340B (en) | 2011-09-16 | 2011-09-16 | High-strength halogen-free epoxy molding compound, and preparation method thereof |
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| CN 201110274707 CN102321340B (en) | 2011-09-16 | 2011-09-16 | High-strength halogen-free epoxy molding compound, and preparation method thereof |
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| CN102321340B true CN102321340B (en) | 2012-12-05 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103087465A (en) * | 2013-03-01 | 2013-05-08 | 无锡创达电子有限公司 | Phenolic resin moulding compound |
| CN103525010A (en) * | 2013-09-25 | 2014-01-22 | 吴江市天源塑胶有限公司 | High-strength engineering plastic |
| CN107353598A (en) * | 2017-08-22 | 2017-11-17 | 江苏中鹏新材料股份有限公司 | Glass epoxy molding plastic and preparation method thereof |
| CN107841091A (en) * | 2017-11-03 | 2018-03-27 | 常州通和建筑工程有限公司 | A kind of preparation method of obdurability epoxy fill-sealing materials |
| CN109370160A (en) * | 2018-10-31 | 2019-02-22 | 科化新材料泰州有限公司 | A kind of epoxy molding plastic and preparation method thereof that powder fiber is modified |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865345A (en) * | 2006-06-26 | 2006-11-22 | 重庆中田化工有限公司 | Reinforced rubber sheet basal body composite resin for car |
| CN101343398A (en) * | 2008-08-22 | 2009-01-14 | 常熟东南塑料有限公司 | Halogen-free flame-proof glass fiber reinforcement epoxy molding compound |
| CN101528797A (en) * | 2006-10-24 | 2009-09-09 | Sika技术股份公司 | Derivatized solid epoxy resin and uses thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATE534703T1 (en) * | 2005-08-24 | 2011-12-15 | Henkel Kgaa | EPOXY COMPOSITIONS WITH IMPROVED IMPACT RESISTANCE |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865345A (en) * | 2006-06-26 | 2006-11-22 | 重庆中田化工有限公司 | Reinforced rubber sheet basal body composite resin for car |
| CN101528797A (en) * | 2006-10-24 | 2009-09-09 | Sika技术股份公司 | Derivatized solid epoxy resin and uses thereof |
| CN101343398A (en) * | 2008-08-22 | 2009-01-14 | 常熟东南塑料有限公司 | Halogen-free flame-proof glass fiber reinforcement epoxy molding compound |
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Owner name: WUXI CHUANGDA NEW MATERIAL CO., LTD. Free format text: FORMER NAME: WUXI CHUANGDA ELECTRONIC CO., LTD. |
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Address after: 214028 South Road, New District, Jiangsu, Wuxi, No. 201-1 Patentee after: WUXI CHUANGDA ADVANCED MATERIALS CO., LTD. Address before: 214028 South Road, New District, Jiangsu, Wuxi, No. 201-1 Patentee before: Wuxi Chuangda Electronics Co.,Ltd. |