CN101613442A - A kind of suitable large glass steel construction layer is with hanging down volatilization unsaturated polyester resin and method for making thereof - Google Patents
A kind of suitable large glass steel construction layer is with hanging down volatilization unsaturated polyester resin and method for making thereof Download PDFInfo
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- CN101613442A CN101613442A CN200910012662A CN200910012662A CN101613442A CN 101613442 A CN101613442 A CN 101613442A CN 200910012662 A CN200910012662 A CN 200910012662A CN 200910012662 A CN200910012662 A CN 200910012662A CN 101613442 A CN101613442 A CN 101613442A
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Abstract
The present invention relates to macromolecular compound.A kind ofly be used to make large glass steel construction layer and be dissolved in the formulated a kind of unsaturated polyester resin of vinylbenzene by propylene glycol, ethylene glycol, hexanodioic acid, phthalic anhydride, cis-butenedioic anhydride to terminal through condensation reaction with low volatilization unsaturated polyester resin; Add N20 type aerosil, M30 exothermic peak inhibitor and 0.02 part of B20 tensio-active agent again in unsaturated polyester resin, the thixotropy index and the viscosity that evenly reach specified requirement by the stirrer high speed dispersion get final product.Advantage of the present invention is: not only be fit to hand and stick with paste and sprayup process, but also have sag prevention, water tolerance height, exothermic peak is low, the vinylbenzene volatile quantity is low characteristics, be applicable to large-scale thick product glass fiber reinforced plastics products such as fan shroud, glass reinforced plastic ships and light boats, product strength height, good weatherability, water-tolerant.
Description
One, technical field
The present invention relates to a kind of unsaturated polyester resin, especially relate to glass reinforced plastic, the invention still further relates to the method for making of resin in addition with hanging down the volatilization unsaturated polyester resin.
Two, background technology
Glass reinforced plastic is a kind of matrix material, and it is to be matrix with the resin, and glass fibre is that strongthener is composited, and is also referred to as glass filament reinforced plastics, and mainly have following characteristics: 1. light weight is high-strength, and tensile strength is 4 times～6 times of ordinary steel.2. corrosion-resistant, anti-aging, be work-ing life 50 years.3. easy-formation, designability are strong.4. good insulation performance and thermotolerance are arranged.
Along with the continuous development and the extension of glass reinforced plastic industry, large glass steel work such as glass reinforced plastic ships and light boats and wind-power electricity generation cabin cover has also obtained to develop flourishingly in recent years.Meanwhile, market and user also have higher requirement with the quality of unsaturated polyester resin to glass reinforced plastic.But traditional fiber glass resin is because shortcomings such as heat release peak height, poor toughness can only be fit to make small-sized glass fiber reinforced plastics product; On the other hand, volatile poisonous vinylbenzene can produce very big harm to workmen's health in the resin, and vinylbenzene is dispersed in the air, also can cause serious environmental to pollute.
Three, summary of the invention
The objective of the invention is to overcome the problems referred to above, provide a kind of suitable large glass steel construction layer, fill a prescription rationally, be fit to hand and stick with paste or sprayup process, can make goods have sag prevention, low-styrene volatilization, hang down exothermic peak again with low volatilization unsaturated polyester resin.The present invention also provides its method for making in addition, and technology is simple, is easy to operate and control.
The technical scheme that the present invention is adopted for achieving the above object is: a kind of suitable large glass steel construction layer is with hanging down the volatilization unsaturated polyester resin, and its component by following portions by weight is formulated: propylene glycol 110-130, ethylene glycol 8-15, hexanodioic acid 3-6, phthalic anhydride 130-150, cis-butenedioic anhydride 50-70, vinylbenzene 130-150, B20 polyethylene glycols tensio-active agent 0.01-0.05, M30 exothermic peak inhibitor 10-25, N20 aerosil 0.3-0.8.
Described a kind of suitable large glass steel construction layer is preferably by the component of following portions by weight formulated: propylene glycol 115-120, ethylene glycol 9-12, hexanodioic acid 3-5, phthalic anhydride 135-145, cis-butenedioic anhydride 50-60, vinylbenzene 140-150, B20 polyethylene glycols tensio-active agent 0.01-0.03, M30 exothermic peak inhibitor 15-25, N20 aerosil 0.5-0.7 with low volatilization unsaturated polyester resin.
Described a kind of suitable large glass steel construction layer is with hanging down the volatilization unsaturated polyester resin, and best is formulated by the component of following portions by weight: propylene glycol 119, ethylene glycol 11, hexanodioic acid 4, phthalic anhydride 140, cis-butenedioic anhydride 54, vinylbenzene 150, B20 polyethylene glycols tensio-active agent 0.02, M30 exothermic peak inhibitor 20, N20 aerosil 0.6.
Described M30 exothermic peak inhibitor adopts alpha-methyl styrene.
A kind of suitable large glass steel construction layer of the present invention method for making of low volatilization unsaturated polyester resin, earlier with the synthetic unsaturated polyester resin of propylene glycol, ethylene glycol, hexanodioic acid, phthalic anhydride, cis-butenedioic anhydride and vinylbenzene, add N20 type aerosil, M30 exothermic peak inhibitor and B20 polyethylene glycols tensio-active agent again in unsaturated polyester resin, the thixotropy index and the viscosity that evenly reach specified requirement by the stirrer high speed dispersion get final product.
Described concrete method for making:
1. synthetic unsaturated polyester resin: the propylene glycol of 119Kg, the ethylene glycol of 11Kg, the hexanodioic acid of 4Kg, the phthalic anhydride of 140Kg and the cis-butenedioic anhydride of 54Kg are dropped in the 350L reactor successively; (flow is 0.5m to logical nitrogen
3/ h) 10 minutes, make to be in nitrogen envelope state in the reactor, open to stir and begin and heat up, insulation is 1 hour when being warming up to 155-160 ℃, logical water coolant in vertical (type) condenser immediately when heating up in a steamer water outlet, and control to heat up in a steamer a temperature be 100-102 ℃.Insulation continues to be warming up to 205-210 ℃ of reaction after finishing; When heating up in a steamer a temperature when beginning to descend, gradually reduce cooling water flow in the vertical (type) condenser until closing fully, sampling and testing then, when the solid acid number begins to vacuumize during for 48-52mgKOH/g, beginning is evacuated down to-80kPa with-1.5kPa; The vacuum tightness of maintenance-80kPa is 26-31mgKOH/g until the solid acid number, and cone-plate viscosity (No. 2 rotor 10 changes 125 ℃) 6.0-7.0Pas removes vacuum, is cooled to 175 ℃; The polyester that reaction is good slowly dilutes in adding cinnamic dilution still, and the dilution temperature is 65-75 ℃, will dilute the interior resin temperature of still after dilution finishes and reduce to 30-40 ℃ and obtain unsaturated polyester resin;
2. in the unsaturated polyester resin that the N20 aerosil adding the first step is made, mixing speed being adjusted to 2000 changes again/hour, after the high speed dispersion 1 hour, add B20 polyethylene glycols tensio-active agent and M30 exothermic peak inhibitor, continue high speed dispersion after 30 minutes, sampling viscosimetric, thixotroping value, gel time and exothermic peak are adjusted its work is corresponding according to detected result, promptly make to be fit to large glass steel construction layer with hanging down the volatilization unsaturated polyester resin.
Large glass steel construction layer land used volatilization unsaturated polyester resin of the present invention, composition of raw materials is reasonable, and used raw material unsaturated polyester resin adopts propylene glycol, ethylene glycol, hexanodioic acid, phthalic anhydride, cis-butenedioic anhydride and vinylbenzene synthetic; Wherein propylene glycol is a kind of dibasic alcohol, and easy and diprotic acid participates in esterification, gives characteristics such as resin physical strength height, water-tolerant; Ethylene glycol is a kind of dibasic alcohol, and easy and diprotic acid participates in esterification, gives characteristics such as resin physical strength height, water-tolerant; Hexanodioic acid is a kind of diprotic acid, and easy and dibasic alcohol generation esterification is given characteristics such as resin flexible toughness; The phthalic anhydride full name is a Tetra hydro Phthalic anhydride, easy and dibasic alcohol generation esterification, and part replaces cis-butenedioic anhydride can regulate the degree of unsaturation of unsaturated polyester, gives the resin excellent mechanical property; The cis-butenedioic anhydride full name is a MALEIC ANHYDRIDE, and easy and dibasic alcohol generation esterification provides the unsaturated polyester unsaturated double-bond, gives the resin excellent mechanical property; Vinylbenzene is the thinner of unsaturated polyester, and the two keys on the vinylbenzene in the vinyl can be used for the crosslinked of vibrin, makes resin solidification have excellent mechanical property.
The component that the present invention cooperates with unsaturated polyester is reasonable, and B20 polyethylene glycols tensio-active agent is a kind of addition type high effective additives, has and good, the thermally-stabilised characteristics such as good of unsaturated polyester resin solvability.Its physicochemical characteristic is as follows:
Outward appearance: faint yellow pasty state.Boiling point: 176 ℃.Flash-point: 70 ℃.Relative density: 0.86 (water=1).Solvability: water insoluble, be dissolved in alcohol, ether, benzene kind solvent.
M30 exothermic peak inhibitor (alpha-methyl styrene) is a kind of double bond containing organic solvent, and is good with resin compatible, the exothermic peak temperature in the time of can effectively reducing resin solidification, and simultaneously, shrinking percentage in the time of can reducing resin solidification improves snappiness.Its physical and chemical performance is as follows:
Outward appearance: colourless to little yellow transparent liquid.Density (25 ℃ of g/cm
3): 0.905-0.915.
Refractive index (20 ℃): 1.53864.Boiling range: 165-169 ℃.
Solvability: water insoluble, dissolve in pure and mild ether.
Advantages such as it is big that N20 type aerosil has specific surface area, and thixotropic property is good, and fineness is low.Its physicochemical characteristic is as follows:
Specific surface area: 〉=200m
2/ g.Outward appearance: white low-density powder inclusion-free.PH value: 3.3～6.0.Free-water :≤5 (110 ℃, 2 hours).
The B20 polyethylene glycols tensio-active agent that adopts has suppressed the vinylbenzene volatilization under the condition that does not influence resin solidification and product strength; Unsaturated polyester resin vinylbenzene volatile quantity is 5-10%, and this resin vinylbenzene volatile quantity is 2-5%; The present invention adopts N20 type aerosil that the sag prevention performance of resin is improved, and makes product be fit to hand and sticks with paste and sprayup process; The present invention adopts M30 exothermic peak inhibitor, too high goods cracking that causes of heat release and local generation of bad phenomenon such as burning when effectively having avoided because of resin solidification.
Technology of the present invention is simple, be easy to operate and control, not only be fit to hand and stick with paste and sprayup process, but also have sag prevention, water tolerance height, characteristics that exothermic peak is low, be applicable to large-scale thick product glass fiber reinforced plastics products such as fan shroud, glass reinforced plastic ships and light boats, product strength height, good weatherability, water-tolerant.
Four, embodiment
Below in conjunction with specific embodiment the present invention is described in further detail, but the invention is not restricted to specific embodiment.
Embodiment 1:
Be fit to large glass steel construction layer with hanging down the volatilization unsaturated polyester resin, its preparation of raw material by following weight forms: propylene glycol 119Kg, ethylene glycol 11Kg, hexanodioic acid 4Kg, phthalic anhydride 140Kg, cis-butenedioic anhydride 54Kg, vinylbenzene 150Kg, B20 polyethylene glycols tensio-active agent 0.02Kg, alpha-methyl styrene 20Kg, N20 aerosil 0.55Kg.
Concrete method for making is as follows:
1. the propylene glycol of 119Kg, the ethylene glycol of 11Kg, the hexanodioic acid of 4Kg, the phthalic anhydride of 140Kg and the cis-butenedioic anhydride of 54Kg are dropped in the 350L reactor successively.
2. (flow is 0.5m to logical nitrogen
3/ h) 10 minutes, make to be in nitrogen envelope state in the reactor, open to stir and begin and heat up, insulation is 1 hour when being warming up to 155-160 ℃, logical water coolant in vertical (type) condenser immediately when heating up in a steamer water outlet, and control to heat up in a steamer a temperature be 100-102 ℃.Insulation continues to be warming up to 205-210 ℃ of reaction after finishing.
3. when heating up in a steamer a temperature when beginning to descend, gradually reduce cooling water flow in the vertical (type) condenser until closing fully, sampling and testing then, when the solid acid number begins to vacuumize during for 48-52mgKOH/g, beginning is evacuated down to-80kPa with-1.5kPa.
4. the vacuum tightness of maintenance-80kPa is 26-31mgKOH/g until the solid acid number, and cone-plate viscosity (No. 2 rotor 10 changes 125 ℃) 6.0-7.0Pas removes vacuum, is cooled to 175 ℃.
The polyester that 5. will react good slowly dilutes in adding cinnamic dilution still, and the dilution temperature is 65-75 ℃, will dilute the interior resin temperature of still after dilution finishes and reduce to 30-40 ℃, makes unsaturated polyester resin.
6. the N20 aerosil with 0.55Kg adds in the above-mentioned unsaturated polyester resin that makes, mixing speed being adjusted to 2000 changes again/hour, after the high speed dispersion 1 hour, add the B20 polyethylene glycols tensio-active agent of 0.02Kg and the alpha-methyl styrene of 20Kg, continue high speed dispersion after 30 minutes, sampling viscosimetric, thixotroping value, gel time and exothermic peak are adjusted its work is corresponding according to detected result, promptly make to be fit to large glass steel construction layer with hanging down the volatilization unsaturated polyester resin.
Embodiment 2-6
Adopt embodiment 1 described method for making to make and be fit to large glass steel construction layer with hanging down the volatilization unsaturated polyester resin, concrete starting ester ratio sees Table 1, the suitable large glass steel construction layer that then embodiment 1-6 is made is made into casting matrix and surveys its every index with low volatilization unsaturated polyester resin, sees Table 1.
The prescription of table 1 embodiment 1-6 and casting matrix index
(raw material unit K g)
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Propylene glycol | ??119 | ??120 | ??119 | ??119 | ??112 | ??128 |
| Ethylene glycol | ??11 | ??10 | ??11 | ??11 | ??8 | ??15 |
| Hexanodioic acid | ??4 | ??5 | ??3 | ??4 | ??3 | ??6 |
| Phthalic anhydride | ??140 | ??138 | ??140 | ??140 | ??130 | ??150 |
| Cis-butenedioic anhydride | ??54 | ??55 | ??53 | ??54 | ??50 | ??70 |
| Vinylbenzene | ??150 | ??150 | ??150 | ??150 | ??135 | ??150 |
| The N20 aerosil | ??0.55 | ??0.6 | ??0.6 | ??0.6 | ??0.3 | ??0.7 |
| B20 polyethylene glycols tensio-active agent | ??0.02 | ??0.02 | ??0.02 | ??0.02 | ??0.01 | ??0.05 |
| Alpha-methyl styrene | ??20 | ??20 | ??19 | ??20 | ??12 | ??25 |
| Acid number mgKOH/g | ??21.46 | ??22.12 | ??20.17 | ??19.20 | ??21.34 | ??18.18 |
| Viscosity Pas | ??0.20 | ??0.21 | ??0.21 | ??0.20 | ??0.24 | ??0.19 |
| Gel time (25 ℃) min | ??18.6 | ??17.6 | ??18.4 | ??18.3 | ??15.8 | ??21.5 |
| Exothermic peak ℃ | ??104 | ??108 | ??104 | ??105 | ??115 | ??116 |
| The thixotroping value | ??3.52 | ??3.78 | ??3.72 | ??3.64 | ??3.10 | ??4.32 |
| Solids content % | ??56.35 | ??56.28 | ??57.18 | ??56.26 | ??59.23 | ??54.24 |
| Ba Keer hardness | ??45 | ??46 | ??45 | ??46 | ??46 | ??47 |
| Tensile strength MPa | ??59 | ??60 | ??62 | ??60 | ??56 | ??61 |
| Tensile modulus GPa | ??3.63 | ??3.62 | ??3.70 | ??3.67 | ??3.61 | ??3.63 |
| Elongation at break % | ??2.5 | ??2.4 | ??2.3 | ??2.5 | ??2.2 | ??2.1 |
| Flexural strength MPa | ??110 | ??105 | ??108 | ??112 | ??92 | ??95 |
| Modulus in flexure GPa | ??4.2 | ??4.2 | ??4.1 | ??4.2 | ??4.2 | ??4.1 |
| Thermal denaturation temperature ℃ | ??72 | ??70 | ??68 | ??70 | ??66 | ??67 |
| Water-intake rate % | ??0.13 | ??0.14 | ??0.10 | ??0.13 | ??0.15 | ??0.19 |
| Vinylbenzene volatile quantity % | ??2.4 | ??2.5 | ??2.4 | ??2.5 | ??4.5 | ??3.8 |
Embodiment 1-6 records the index of each parameter and detects according to seeing Table 2.
Table 2
Large glass steel construction layer of the present invention as can be seen from Table 1 is fit to the making of large-scale thick product glass fiber reinforced plastics product with the heat release peak height of low volatilization unsaturated polyester resin; Stretching and bending property are also better, the physical strength height; The vinylbenzene volatile quantity is low, meets environmental protection requirement, is fit to hand and sticks with paste and sprayup process, can satisfy client's service requirements.
Claims (6)
1, a kind of suitable large glass steel construction layer is with hanging down the volatilization unsaturated polyester resin, and it is characterized in that: its component by following portions by weight is formulated: propylene glycol 110-130, ethylene glycol 8-15, hexanodioic acid 3-6, phthalic anhydride 130-150, cis-butenedioic anhydride 50-70, vinylbenzene 130-150, B20 polyethylene glycols tensio-active agent 0.01-0.05, M30 exothermic peak inhibitor 10-25, N20 aerosil 0.3-0.8.
2, a kind of suitable large glass steel construction layer according to claim 1 is with hanging down the volatilization unsaturated polyester resin, and it is characterized in that: its component by following portions by weight is formulated: propylene glycol 115-120, ethylene glycol 9-12, hexanodioic acid 3-5, phthalic anhydride 135-145, cis-butenedioic anhydride 50-60, vinylbenzene 140-150, B20 polyethylene glycols tensio-active agent 0.01-0.03, M30 exothermic peak inhibitor 15-25, N20 aerosil 0.5-0.7.
3, a kind of suitable large glass steel construction layer according to claim 1 is with hanging down the volatilization unsaturated polyester resin, and it is characterized in that: its component by following portions by weight is formulated: propylene glycol 119, ethylene glycol 11, hexanodioic acid 4, phthalic anhydride 140, cis-butenedioic anhydride 54, vinylbenzene 150, B20 polyethylene glycols tensio-active agent 0.02, M30 exothermic peak inhibitor 20, N20 aerosil 0.6.
4, according to the low volatilization unsaturated polyester resin of the arbitrary described a kind of suitable large glass steel construction layer of claim 1-3, it is characterized in that: M30 exothermic peak inhibitor adopts alpha-methyl styrene.
5, a kind of suitable large glass steel construction layer method for making of low volatilization unsaturated polyester resin, it is characterized in that: earlier with the synthetic unsaturated polyester resin of propylene glycol, ethylene glycol, hexanodioic acid, phthalic anhydride, cis-butenedioic anhydride and vinylbenzene, add N20 type aerosil, alpha-methyl styrene and B20 polyethylene glycols tensio-active agent again in unsaturated polyester resin, the thixotropy index and the viscosity that evenly reach specified requirement by the stirrer high speed dispersion get final product.
6, a kind of suitable large glass steel construction layer according to claim 5 is characterized in that: 1. synthetic unsaturated polyester resin: the propylene glycol of 119Kg, the ethylene glycol of 11Kg, the hexanodioic acid of 4Kg, the phthalic anhydride of 140Kg and the cis-butenedioic anhydride of 54Kg are dropped in the 350L reactor successively with the method for making of low volatilization unsaturated polyester resin; (flow is 0.5m to logical nitrogen
3/ h) 10 minutes, make to be in nitrogen envelope state in the reactor, open to stir and begin and heat up, insulation is 1 hour when being warming up to 155-160 ℃, logical water coolant in vertical (type) condenser immediately when heating up in a steamer water outlet, and control to heat up in a steamer a temperature be 100-102 ℃.Insulation continues to be warming up to 205-210 ℃ of reaction after finishing; When heating up in a steamer a temperature when beginning to descend, gradually reduce cooling water flow in the vertical (type) condenser until closing fully, sampling and testing then, when the solid acid number begins to vacuumize during for 48-52mgKOH/g, beginning is evacuated down to-80kPa with-1.5kPa; The vacuum tightness of maintenance-80kPa is 26-31mgKOH/g until the solid acid number, and cone-plate viscosity (No. 2 rotor 10 changes 125 ℃) 6.0-7.0Pas removes vacuum, is cooled to 175 ℃; The polyester that reaction is good slowly dilutes in adding cinnamic dilution still, and the dilution temperature is 65-75 ℃, will dilute in the still resin temperature after dilution finishes and reduce to 30-40 ℃ and get unsaturated polyester resin;
2. in the unsaturated polyester resin that the N20 aerosil adding the first step is made, mixing speed being adjusted to 2000 changes again/hour, after the high speed dispersion 1 hour, add B20 polyethylene glycols tensio-active agent and M30 exothermic peak inhibitor, continue high speed dispersion after 30 minutes, sampling viscosimetric, thixotroping value, gel time and exothermic peak are adjusted its work is corresponding according to detected result, promptly make to be fit to large glass steel construction layer with hanging down the volatilization unsaturated polyester resin.
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| CN102268168A (en) * | 2010-12-25 | 2011-12-07 | 河南科技大学 | Composite material of unsaturated polyester resins with low styrene emission |
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| CN102863592B (en) * | 2012-10-18 | 2014-11-26 | 常州华日新材有限公司 | Preparation method for transparent thixotropic unsaturated polyester resin |
| CN103524686A (en) * | 2013-09-30 | 2014-01-22 | 常州天马瑞盛复合材料有限公司 | Unsaturated polyester resin dedicated to manufacturing fiber reinforced plastic refrigerator car integral carriage board and preparation method thereof |
| CN113087887A (en) * | 2021-03-30 | 2021-07-09 | 江阴市建恒化工有限公司 | Marine ortho-benzene type unsaturated polyester resin and preparation method thereof |
| CN113336899A (en) * | 2021-06-10 | 2021-09-03 | 江阴市建恒化工有限公司 | Unsaturated polyester resin for rapid pultrusion process and preparation method thereof |
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Open date: 20091230 |