CN101089043A - Prepn process of high-performace unsaturated resin SMC/glass fiber composite material - Google Patents
Prepn process of high-performace unsaturated resin SMC/glass fiber composite material Download PDFInfo
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- CN101089043A CN101089043A CN 200610010149 CN200610010149A CN101089043A CN 101089043 A CN101089043 A CN 101089043A CN 200610010149 CN200610010149 CN 200610010149 CN 200610010149 A CN200610010149 A CN 200610010149A CN 101089043 A CN101089043 A CN 101089043A
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Abstract
The preparation process of high performance unsaturated resin SMC/glass fiber composite material includes the following steps: adding malonic acid, diol, dibasic anhydride in certain molar proportion into the reactor and introducing inert gas to produce polycondensation reaction at 190-210 deg.c; addig diol and alcoholysis inhibitor for further reaction until reaching the reaction terminal of acidity 2 mgKOH/g; cooling and diluting to obtain unsaturated polyester resin; adding styrene, isocyanate as thickener, glass fiber, aluminum hydroxide and other stuffing and assistant, mixing to form resin paste; spreading the resin paste between two layers of polyethylene film, and curing at room temperature for 3-8 hr to obtain the composite material. The high performance unsaturated resin SMC/glass fiber composite material has high impact strength.
Description
Technical field: the preparation technology who the present invention relates to high-performance unsaturated polyester/glass fiber compound material.
Background technology: along with the fast development of general unsaturated polyester SMC, the insulation industry begins to use on a large scale this product.As this product be widely used in that bus insulation frame, insulation thick stick bridge joint line in automatically controlled, the controller switching equipment fastened, coil rack, insulator, switch chassis, cease spark cover, electrical equipment case etc.The middle core of SMC molding sheet material is made up of the chopped strand that fully floods through resin paste (or felt), and upper and lower surface covers with polyethylene film.Contain unsaturated polyester resin, initiator, chemical thickening material in its resin paste, various compositions such as low shrinkage additive, filler, releasing agent, tinting material.It produces with moulding process roughly as follows: weak point cuts the raw yarn felt or the thick fibre of glass is laid on the PE film that has evenly applied resin paste in advance, covers the PE film that another layer applied resin paste then thereon, has formed a kind of " sandwich " structure.Rolling was collected in the fully kneading of resin paste and glass (or felt) then when it passed through Dilvar zone, carried out necessary maturation process.Made sheet material reach tack-free after, can be cut into certain size on request, throw off the PE film on two sides, be stacked in the extrusion forming of heating in the metal pair mould by certain requirement.One of gordian technique of preparation SMC is the thickening of resin, and general unsaturated polyester is generally used the magnesium oxide thickening, and end carboxyl and magnesium oxide coordination type by polyester reticulate structure, and then make the viscosity increase of polyester.Though this thickening material price is low, but thickening rate is slow, and factor such as magnesian granularity, dispersiveness, activity also has considerable influence to the thickening properties of unsaturated polyester resin, thereby causes its thickening effectiveness instability, and the SMC product strength and the toughness of production are not high.
Summary of the invention: the preparation method who the purpose of this invention is to provide a kind of high-performance unsaturated polyester/glass fiber compound material of isocyanic ester thickening.Diisocyanate compound thickening unsaturated polyester is the thickening technology that occurs recently, it and the reaction of hydroxyl unsaturated polyester generate a kind of alternately netted fragment of dispersive, this technology can faster, more effectively be controlled viscosity, and the pressing shrinking percentage is low, the shock strength height obtains the obdurability material easily.The present invention in turn joins in reactor by certain mole proportioning propanedioic acid, dibasic alcohol, dibasic acid anhydride, feed rare gas element simultaneously, carry out polycondensation (polyesterification reaction) in the time of 190-210 ℃, keep acid anhydrides excessive when feeding intake, add dibasic alcohol and alcoholysis inhibitor then, continue to react to acidity be about 2mgKOH/g, promptly reach reaction end, obtain containing the unsaturated polyester resin of terminal hydroxy group and active alpha-H side group after the cooling dilution; Add vinylbenzene then, then in reactor, add isocyanic ester thickening material and other filler and auxiliary agent, uniform mixing prepares resin paste, be spread out on the polyethylene film, add a cover the layer of polyethylene film above, room temperature cure 3-8hr reaches the viscosity of expection, and rolling promptly obtains the composite product that this project is developed.Described synthetic unsaturated polyester ester terminal mostly is hydroxyl; Described alcoholysis inhibitor is ZnO/ZnCl
2Inhibitor; Described thickening material is the isocyanic ester thickening material; Synthetic terminal hydroxy group unsaturated polyester resin of the present invention, different with traditional unsaturated polyester resin is, introduced and had active alpha-propanedioic acid of H side group, this α-H side group can form unsettled urea groups chemical bond with-NCO group in thickening, and this unsettled urea groups chemical bond can be opened in the mold process of later stage SMC, short-term produces the thinning phenomenon of resin paste, finally make mould pressing process be able under lower pressure, carry out, adopt the high-performance unsaturated polyester/glass fiber compound material of present technique preparation to compare shock strength raising 30-50% with synthetic unsaturated polyester matrix material under the equal conditions.
Embodiment one: present embodiment drops into 1mol propanedioic acid, 1.1mol propylene glycol successively in reactor, the 1mol dibasic acid anhydride, feed rare gas element simultaneously, heating, begin to stir when solid materials begins to melt in the question response still, progressively slowly be warming up to 160 ℃, keep this temperature after 30 minutes.Be warming up to 190～210 ℃ and keep this temperature more gradually.Treat that acid number does not have considerable change (this moment, head temperature descended near room temperature), be chilled to below 200 ℃, add 1.1mol dibasic alcohol and 0.05mol alcoholysis inhibitor ZnO/ZnCl
2, slowly be warming up to 190～210 ℃, continue to react to acid number and reach about 15mgKOH/g.This moment, acid number descended slowly, stopped logical nitrogen.Begin to vacuumize, control vacuum tightness from low to high, temperature is controlled in 200 ℃, up to acid number 2mg KOH/g, then add 2mol vinylbenzene, add 2mol isocyanic ester thickening material, 300g glass fibre, 100g aluminium hydroxide and other filler and auxiliary agent then, uniform mixing is prepared resin paste, is spread out on the polyethylene film, add a cover the layer of polyethylene film above, room temperature cure 3-8hr reaches the viscosity of expection, and rolling is stored.
Embodiment two: present embodiment drops into 0.5mol propanedioic acid, 0.5mol propylene glycol, 0.5mol dibasic acid anhydride successively in reactor, feed rare gas element simultaneously, heating.Begin to stir when solid materials begins to melt in the question response still, progressively slowly be warming up to 160 ℃, keep this temperature after 30 minutes.Be warming up to 190～210 ℃ and keep this temperature more gradually, treat that acid number does not have considerable change (this moment, head temperature descended near room temperature), be chilled to below 200 ℃, add 0.5mol dibasic alcohol and 0.01mol alcoholysis inhibitor ZnO/ZnCl
2, slowly be warming up to 190～210 ℃, continue to react to acid number and reach about 15mgKOH/g.This moment, acid number descended slowly, stopped logical nitrogen.Begin to vacuumize, control vacuum tightness from low to high, temperature is controlled in 200 ℃, up to acid number 5mg KOH/g, then add 1mol vinylbenzene, add 1mol isocyanic ester thickening material, 200g glass fibre, 60g aluminium hydroxide and other filler and auxiliary agent then, uniform mixing is prepared resin paste, is spread out on the polyethylene film, add a cover the layer of polyethylene film above, room temperature cure 3-8hr reaches the viscosity of expection, and rolling is stored.
Claims (7)
1, a kind of preparation method of high-performace unsaturated resin SMC/glass fiber compound material, it is characterized in that carrying out precondensation by propanedioic acid, dibasic alcohol, dibasic acid anhydride, keep acid anhydrides excessive when feeding intake, react to acidity be 15mgKOH/g, obtain holding the carboxyl unsaturated polyester, add the end-blocking dibasic alcohol then, and keep alcohol excessive, add the alcoholysis inhibitor, continue reaction, obtain containing the unsaturated polyester resin of terminal hydroxy group and active alpha-H side group after the cooling dilution until certain acid number; Add vinylbenzene then, then add isocyanic ester thickening material, glass fibre, aluminium hydroxide and other filler and auxiliary agent, uniform mixing prepares resin paste, be spread out on the polyethylene film, add a cover the layer of polyethylene film above, room temperature cure 3-8hr reaches the viscosity of expection, rolling is also stored, and promptly makes matrix material of the present invention.
2,, it is characterized in that described unsaturated polyester ester terminal mostly is hydroxyl according to the preparation method of the described a kind of high-performace unsaturated resin SMC/glass fiber compound material of claim one.
3,, it is characterized in that described terminal hydroxy group unsaturated polyester contains active alpha-H side group according to the preparation method of the described a kind of high-performace unsaturated resin SMC/glass fiber compound material of claim one.
4,, it is characterized in that described alcoholysis inhibitor is ZnO/ZnCl according to the preparation method of the described a kind of high-performace unsaturated resin SMC/glass fiber compound material of claim one
2Inhibitor.
5,, it is characterized in that described thickening material is the isocyanic ester thickening material according to the preparation method of the described a kind of high-performace unsaturated resin SMC/glass fiber compound material of claim one.
6, according to the preparation method of the described a kind of high-performace unsaturated resin SMC/glass fiber compound material of claim one, the building-up reactions endpoint acid number that it is characterized in that described terminal hydroxy group unsaturated polyester resin is 2mgKOH/g.
7, according to the preparation method of the described a kind of high-performace unsaturated resin SMC/glass fiber compound material of claim one, the building-up reactions endpoint acid number that it is characterized in that described terminal hydroxy group unsaturated polyester resin is 5mgKOH/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610010149 CN101089043A (en) | 2006-06-13 | 2006-06-13 | Prepn process of high-performace unsaturated resin SMC/glass fiber composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610010149 CN101089043A (en) | 2006-06-13 | 2006-06-13 | Prepn process of high-performace unsaturated resin SMC/glass fiber composite material |
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| CN101089043A true CN101089043A (en) | 2007-12-19 |
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| CN 200610010149 Pending CN101089043A (en) | 2006-06-13 | 2006-06-13 | Prepn process of high-performace unsaturated resin SMC/glass fiber composite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101927570A (en) * | 2010-05-11 | 2010-12-29 | 合肥华欣自控设备成套厂 | Method for preparing SMC composite material with high finish surface |
| CN101941320A (en) * | 2010-08-16 | 2011-01-12 | 上海中技桩业股份有限公司 | Method for preparing composite material end plate for pre-stressed pile |
| CN103013072A (en) * | 2012-12-04 | 2013-04-03 | 常州瑞禧电力设备有限公司 | High-temperature early-warning protective hood |
| CN113174126A (en) * | 2021-05-13 | 2021-07-27 | 河北英丽达新材料科技有限公司 | High-performance SMC molding compound and preparation method thereof |
-
2006
- 2006-06-13 CN CN 200610010149 patent/CN101089043A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101927570A (en) * | 2010-05-11 | 2010-12-29 | 合肥华欣自控设备成套厂 | Method for preparing SMC composite material with high finish surface |
| CN101941320A (en) * | 2010-08-16 | 2011-01-12 | 上海中技桩业股份有限公司 | Method for preparing composite material end plate for pre-stressed pile |
| CN101941320B (en) * | 2010-08-16 | 2012-12-19 | 上海中技桩业股份有限公司 | Method for preparing composite material end plate for pre-stressed pile |
| CN103013072A (en) * | 2012-12-04 | 2013-04-03 | 常州瑞禧电力设备有限公司 | High-temperature early-warning protective hood |
| CN113174126A (en) * | 2021-05-13 | 2021-07-27 | 河北英丽达新材料科技有限公司 | High-performance SMC molding compound and preparation method thereof |
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