CN104926998A - Unsaturated polyester resin used for bulk molding compound and preparation method thereof - Google Patents
Unsaturated polyester resin used for bulk molding compound and preparation method thereof Download PDFInfo
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- CN104926998A CN104926998A CN201510052333.3A CN201510052333A CN104926998A CN 104926998 A CN104926998 A CN 104926998A CN 201510052333 A CN201510052333 A CN 201510052333A CN 104926998 A CN104926998 A CN 104926998A
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Abstract
The invention discloses unsaturated polyester resin used for a bulk molding compound and a preparation method thereof. The resin is mainly prepared from the following raw materials by weight: 2000 to 2500 parts of phthalic anhydride, 7500 to 8500 parts of maleic anhydride, 3500 to 4000 parts of diethylene glycol, 4500 to 5000 parts of 1,2-propylene glycol, 3 to 5 parts of an antioxidant, 8 to 12 parts of a polymerization inhibitor, 3 to 7 parts of methylhydroquinone, 8500 to 9000 parts of styrene and 1 to 2 parts of p-benzoquinone. Compared with the prior art, the unsaturated polyester resin for the bulk molding compound provided by the invention has the following advantages: cost is significantly reduced, and excellent mechanical property is maintained.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of Bulk Molding Compound unsaturated polyester resin and preparation method thereof.
Background technology
BMC (DMC) material is the abbreviation of Bulk (Dough) molding compounds, i.e. Bulk Molding Compound.Domesticly often be called unsaturated polyester Bulk Molding Compound.Its main raw material is by GF (short glass fiber), UP (unsaturated polyester), MD (filler) and the various additive material bulk prepreg through fully mixing.DMC material, is first applied twentieth century sixties in front West Germany and Britain, then obtains larger development in the U.S. and Japan respectively in the seventies and the eighties.Because BMC Bulk Molding Compound has excellent electric property, mechanical property, thermotolerance, chemical resistance, adapts to again various moulding process, can meet the requirement of various product to performance, therefore more and more be subject to liking of users.
Although current BMC product is through the development of decades and improvement, BMC product cost is high, also has research to attempt to reduce costs, but mechanical property can be caused not enough, seriously limits its industrial application.
Summary of the invention
The object of the invention is to overcome above-mentioned weak point, provide a kind of cost significantly to reduce and the Bulk Molding Compound unsaturated polyester resin of excellent mechanical property can be kept.
Another object of the present invention is to provide the preparation method of above-mentioned Bulk Molding Compound unsaturated polyester resin.
The object of the invention is to realize in the following manner:
A kind of Bulk Molding Compound unsaturated polyester resin, this resin is made primarily of the raw material of following weight part:
Phthalic anhydride 2000-2500 weight part, cis-butenedioic anhydride 7500-8500 weight part, Diethylene Glycol 3500-4000 weight part, 1,2-PD 4500-5000 weight part, oxidation inhibitor 3-5 weight part, stopper 8-12 weight part, toluhydroquinone 3-7 weight part, vinylbenzene 8500-9000 weight part, para benzoquinone 1-2 weight part.
This resin is preferably made primarily of the raw material of following weight part:
Phthalic anhydride 2200-2500 weight part, cis-butenedioic anhydride 7500-8000 weight part, Diethylene Glycol 3500-3700 weight part, 1,2-PD 4500-4800 weight part, oxidation inhibitor 3-4 weight part, stopper 8-10 weight part, toluhydroquinone 5-7 weight part, vinylbenzene 8500-8800 weight part, para benzoquinone 1-1.5 weight part.
This resin is most preferably made primarily of the raw material of following weight part:
Phthalic anhydride 2000 weight part, cis-butenedioic anhydride 7500 weight part, Diethylene Glycol 3700 weight part, 1,2-PD 4500 weight part, oxidation inhibitor 3 weight part, stopper 8 weight part, toluhydroquinone 7 weight part, vinylbenzene 8500 weight part, para benzoquinone 1 weight part.
Stopper of the present invention is preferably Resorcinol, and oxidation inhibitor is preferably triphenyl phosphite, and retarder is preferably copper naphthenate.
The preparation method of above-mentioned Bulk Molding Compound unsaturated polyester resin comprises the following steps:
A) be 1.5 ~ 1.8m at nitrogen flow
3under the condition of/h, by 1,2 propylene glycol, Diethylene Glycol, 3/5 stopper, phthalic anhydride, cis-butenedioic anhydride and oxidation inhibitor mixing after be warming up to 205 DEG C with the speed of 10-12 DEG C/h, insulation reaction 5-8h, reaction to middle control acid number reaches 39 ~ 45mgKOH/g, carries out decompression dehydration, until acid number reaches 31 ~ 37mgKOH/g, be cooled to 195 DEG C again, add the toluhydroquinone of remaining stopper and 2/7, then be cooled to 185 DEG C and obtain unsaturated polyester resin;
B) slowly added by the unsaturated polyester resin obtained in the mixture of vinylbenzene and para benzoquinone and remaining toluhydroquinone, be cooled to 70 ~ 80 DEG C while stirring, 2 ~ 3h adds the unsaturated polyester resin of full, then is cooled to 40 ~ 45 DEG C.
Stopper described in the method is preferably Resorcinol, and oxidation inhibitor is preferably triphenyl phosphite.
The Bulk Molding Compound unsaturated polyester resin that the present invention obtains also can be cured, and gel time controls at 30 ~ 40min.Add conventional promotor, solidifying agent etc. during solidification and make casting matrix according to the requirement of " making of sample " in GB/T8237-2005.
Beneficial effect of the present invention compared with the prior art:
The present invention adopts the para benzoquinone of specific consumption and toluhydroquinone as compound retarder, prevents product premature cure, can improve more than 72 days storage period than traditional product.Its specific feed postition can also prevent inappropriate polymerization and affect speed of response simultaneously.The present invention is combined 1,2-PD and Diethylene Glycol, substitutes conventional neopentyl glycol, methyl propanediol, the expensive raw material such as dipropylene glycol, and on the basis ensureing excellent mechanical property, cost significantly reduces.In preparation process, middle control acid number is preferably between 39 ~ 45mgKOH/g, if acid number is too high, free acid or sour more, easily runs off; If acid number is too low, then can greatly lose time.When the present invention reacts, adopt the nitrogen of specific flow velocity, be beneficial to and carry moisture content, contribute to the carrying out reacted.
The flexural strength of Bulk Molding Compound resin of the present invention can up to more than 110MPa, and tensile strength can up to more than 65MPa.
Embodiment
The present invention is further illustrated below by way of specific embodiment.But the detail of embodiment only for explaining the present invention, should not be construed as limited overall technical solution.
Embodiment 1
Formula: phthalic anhydride 2000 weight part, cis-butenedioic anhydride 7500 weight part, Diethylene Glycol 3700 weight part, 1,2-propylene glycol 4500 weight part, triphenyl phosphite 3 weight part, Resorcinol 8 weight part, toluhydroquinone 7 weight part, vinylbenzene 8500 weight part, para benzoquinone 1 weight part.
The preparation method of this Bulk Molding Compound unsaturated polyester resin is:
A) be 1.5 ~ 1.8m at nitrogen flow
3under the condition of/h, by 1,2 propylene glycol, Diethylene Glycol, 3/5 stopper, phthalic anhydride, cis-butenedioic anhydride and oxidation inhibitor mixing after be warming up to 205 DEG C with the speed of 10-12 DEG C/h, insulation reaction 5-8h, reaction to middle control acid number reaches 39 ~ 45mgKOH/g, carries out decompression dehydration, until acid number reaches 31 ~ 37mgKOH/g, be cooled to 195 DEG C again, add the toluhydroquinone of remaining stopper and 2/7, then be cooled to 185 DEG C and obtain unsaturated polyester resin;
B) slowly added by the unsaturated polyester resin obtained in the mixture of vinylbenzene and para benzoquinone and remaining toluhydroquinone, be cooled to 70 ~ 80 DEG C while stirring, 2 ~ 3h adds the unsaturated polyester resin of full, then is cooled to 40 ~ 45 DEG C.
The cobalt iso-octoate of resin 100g and 2g obtained and the cyclohexanone peroxide of 2g, solid is become after gel 40min, normal temperature places 24 hours, dry 3 hours at 60 DEG C, 110 DEG C of conditions dry 1 hour, normal temperature makes casting matrix after placing 24 hours, and the method makes casting matrix according to the custom requirements of " making of sample " in GB/T8237/2005.
Embodiment 2
Formula: phthalic anhydride 2200 weight part, cis-butenedioic anhydride 8000 weight part, Diethylene Glycol 3500 weight part,
1,2-PD 4800 weight part, triphenyl phosphite 3 weight part, Resorcinol 10 weight part, toluhydroquinone 5 weight part, vinylbenzene 8800 weight part, para benzoquinone 1 weight part.
The preparation method of this Bulk Molding Compound unsaturated polyester resin is:
A) be 1.5 ~ 1.8m at nitrogen flow
3under the condition of/h, by 1,2 propylene glycol, Diethylene Glycol, 3/5 stopper, phthalic anhydride, cis-butenedioic anhydride and oxidation inhibitor mixing after be warming up to 205 DEG C with the speed of 10-12 DEG C/h, insulation reaction 5-8h, reaction to middle control acid number reaches 39 ~ 45mgKOH/g, carries out decompression dehydration, until acid number reaches 31 ~ 37mgKOH/g, be cooled to 195 DEG C again, add the toluhydroquinone of remaining stopper and 2/7, then be cooled to 185 DEG C and obtain unsaturated polyester resin;
B) slowly added by the unsaturated polyester resin obtained in the mixture of vinylbenzene and para benzoquinone and remaining toluhydroquinone, be cooled to 70 ~ 80 DEG C while stirring, 2 ~ 3h adds the unsaturated polyester resin of full, then is cooled to 40 ~ 45 DEG C.
The cobalt iso-octoate of resin 100g and 2g obtained and the cyclohexanone peroxide of 2g, solid is become after gel 30min, normal temperature places 24 hours, dry 3 hours at 60 DEG C, 110 DEG C of conditions dry 1 hour, normal temperature makes casting matrix after placing 24 hours, and the method makes casting matrix according to the custom requirements of " making of sample " in GB/T8237/2005.
Embodiment 3
Formula: phthalic anhydride 2500 weight part, cis-butenedioic anhydride 7500 weight part, Diethylene Glycol 3700 weight part,
1,2-PD 4500 weight part, triphenyl phosphite 4 weight part, Resorcinol 8 weight part, toluhydroquinone 7 weight part, vinylbenzene 8500 weight part, para benzoquinone 1.5 weight part.
The preparation method of this Bulk Molding Compound unsaturated polyester resin is:
A) be 1.5 ~ 1.8m at nitrogen flow
3under the condition of/h, by 1,2 propylene glycol, Diethylene Glycol, 3/5 stopper, phthalic anhydride, cis-butenedioic anhydride and oxidation inhibitor mixing after be warming up to 205 DEG C with the speed of 10-12 DEG C/h, insulation reaction 5-8h, reaction to middle control acid number reaches 39 ~ 45mgKOH/g, carries out decompression dehydration, until acid number reaches 31 ~ 37mgKOH/g, be cooled to 195 DEG C again, add the toluhydroquinone of remaining stopper and 2/7, then be cooled to 185 DEG C and obtain unsaturated polyester resin;
B) slowly added by the unsaturated polyester resin obtained in the mixture of vinylbenzene and para benzoquinone and remaining toluhydroquinone, be cooled to 70 ~ 80 DEG C while stirring, 2 ~ 3h adds the unsaturated polyester resin of full, then is cooled to 40 ~ 45 DEG C.
The cobalt iso-octoate of resin 100g and 2g obtained and the cyclohexanone peroxide of 2g, solid is become after gel 30min, normal temperature places 24 hours, dry 3 hours at 60 DEG C, 110 DEG C of conditions dry 1 hour, normal temperature makes casting matrix after placing 24 hours, and the method makes casting matrix according to the custom requirements of " making of sample " in GB/T8237/2005.
Embodiment 4
Formula: phthalic anhydride 2500 weight part, cis-butenedioic anhydride 8500 weight part, Diethylene Glycol 4000 weight part,
1,2-PD 5000 weight part, oxidation inhibitor 5 weight part, stopper 12 weight part, toluhydroquinone 7 weight part, vinylbenzene 8500 weight part, para benzoquinone 2 weight part.
Preparation method is with embodiment 1.
Embodiment 5
Formula: phthalic anhydride 2000 weight part, cis-butenedioic anhydride 7500 weight part, Diethylene Glycol 3500 weight part,
1,2-PD 4500 weight part, oxidation inhibitor 3 weight part, stopper 8 weight part, toluhydroquinone 3 weight part, vinylbenzene 8500 weight part, para benzoquinone 1 weight part.
Preparation method is with embodiment 1.
Prepare material property according to embodiment 1 ~ 5 method and detect data as table 1:
Table 1
The present invention is not described in detail conventional production process and process, and detailed concrete grammar and process can be implemented in conjunction with aforementioned production method and ordinary method, and person of ordinary skill in the field can repeat to realize completely.
Claims (8)
1. a Bulk Molding Compound unsaturated polyester resin, is characterized in that this resin is made primarily of the raw material of following weight part:
Phthalic anhydride 2000-2500 weight part, cis-butenedioic anhydride 7500-8500 weight part, Diethylene Glycol 3500-4000 weight part, 1,2-PD 4500-5000 weight part, oxidation inhibitor 3-5 weight part, stopper 8-12 weight part, toluhydroquinone 3-7 weight part, vinylbenzene 8500-9000 weight part, para benzoquinone 1-2 weight part.
2. Bulk Molding Compound unsaturated polyester resin according to claim 1, is characterized in that this resin is made primarily of the raw material of following weight part:
Phthalic anhydride 2200-2500 weight part, cis-butenedioic anhydride 7500-8000 weight part, Diethylene Glycol 3500-3700 weight part, 1,2-PD 4500-4800 weight part, oxidation inhibitor 3-4 weight part, stopper 8-10 weight part, toluhydroquinone 5-7 weight part, vinylbenzene 8500-8800 weight part, para benzoquinone 1-1.5 weight part.
3. Bulk Molding Compound unsaturated polyester resin according to claim 2, is characterized in that this resin is made primarily of the raw material of following weight part:
Phthalic anhydride 2000 weight part, cis-butenedioic anhydride 7500 weight part, Diethylene Glycol 3700 weight part, 1,2-PD 4500 weight part, oxidation inhibitor 3 weight part, stopper 8 weight part, toluhydroquinone 7 weight part, vinylbenzene 8500 weight part, para benzoquinone 1 weight part.
4. the Bulk Molding Compound unsaturated polyester resin according to claim 1,2 or 3, is characterized in that described stopper is Resorcinol.
5. the Bulk Molding Compound unsaturated polyester resin according to claim 1,2 or 3, is characterized in that described oxidation inhibitor is triphenyl phosphite.
6. a preparation method for the Bulk Molding Compound unsaturated polyester resin described in claim 1,2 or 3, is characterized in that the method comprises the following steps:
A) be 1.5 ~ 1.8m at nitrogen flow
3under the condition of/h, by 1,2 propylene glycol, Diethylene Glycol, 3/5 stopper, phthalic anhydride, cis-butenedioic anhydride and oxidation inhibitor mixing after be warming up to 205 DEG C with the speed of 10-12 DEG C/h, insulation reaction 5-8h, reaction to middle control acid number reaches 39 ~ 45mgKOH/g, carries out decompression dehydration, until acid number reaches 31 ~ 37mgKOH/g, be cooled to 195 DEG C again, add the toluhydroquinone of remaining stopper and 2/7, then be cooled to 185 DEG C and obtain unsaturated polyester resin;
B) slowly added by the unsaturated polyester resin obtained in the mixture of vinylbenzene and para benzoquinone and remaining toluhydroquinone, be cooled to 70 ~ 80 DEG C while stirring, 2 ~ 3h adds the unsaturated polyester resin of full, then is cooled to 40 ~ 45 DEG C.
7. the preparation method of Bulk Molding Compound unsaturated polyester resin according to claim 6, is characterized in that described stopper is Resorcinol.
8. the preparation method of Bulk Molding Compound unsaturated polyester resin according to claim 6, is characterized in that described oxidation inhibitor is triphenyl phosphite.
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Cited By (4)
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CN109400857A (en) * | 2018-09-15 | 2019-03-01 | 福建省南安市华龙树脂有限公司 | A kind of soft unsaturated polyester resin and preparation method thereof for furniture industry |
CN109575256A (en) * | 2018-12-04 | 2019-04-05 | 镇江利德尔复合材料有限公司 | A kind of raising outdoor electric appliance insulation performance and the mold pressing resin of heat distortion temperature and preparation method thereof |
CN112321809A (en) * | 2020-12-05 | 2021-02-05 | 宜兴市兴合树脂有限公司 | Resin for chemical-resistant antistatic anti-ultraviolet molding compound |
CN114395218A (en) * | 2022-01-19 | 2022-04-26 | 杭州老板电器股份有限公司 | Edible oil-resistant bulk molding compound and preparation method and application thereof |
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CN109400857A (en) * | 2018-09-15 | 2019-03-01 | 福建省南安市华龙树脂有限公司 | A kind of soft unsaturated polyester resin and preparation method thereof for furniture industry |
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CN109575256A (en) * | 2018-12-04 | 2019-04-05 | 镇江利德尔复合材料有限公司 | A kind of raising outdoor electric appliance insulation performance and the mold pressing resin of heat distortion temperature and preparation method thereof |
CN112321809A (en) * | 2020-12-05 | 2021-02-05 | 宜兴市兴合树脂有限公司 | Resin for chemical-resistant antistatic anti-ultraviolet molding compound |
CN114395218A (en) * | 2022-01-19 | 2022-04-26 | 杭州老板电器股份有限公司 | Edible oil-resistant bulk molding compound and preparation method and application thereof |
CN114395218B (en) * | 2022-01-19 | 2024-02-06 | 杭州老板电器股份有限公司 | Edible oil-resistant bulk molding compound and preparation method and application thereof |
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