CN104926998B - A kind of tubular molding compound unsaturated polyester resin and preparation method thereof - Google Patents
A kind of tubular molding compound unsaturated polyester resin and preparation method thereof Download PDFInfo
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- CN104926998B CN104926998B CN201510052333.3A CN201510052333A CN104926998B CN 104926998 B CN104926998 B CN 104926998B CN 201510052333 A CN201510052333 A CN 201510052333A CN 104926998 B CN104926998 B CN 104926998B
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Abstract
The invention discloses a kind of tubular molding compound unsaturated polyester resin, which is mainly made of the raw material of following parts by weight：2,000 2500 parts by weight of phthalic anhydride, 7,500 8500 parts by weight of cis-butenedioic anhydride, 3,500 4000 parts by weight of diethylene glycol, 1,2 propylene glycol, 4,500 5000 parts by weight, 35 parts by weight of antioxidant, 8 12 parts by weight of polymerization inhibitor, 37 parts by weight of methylnaphthohydroquinone, 8,500 9000 parts by weight of styrene, 12 parts by weight of 1,4-benzoquinone.Compared with the prior art, tubular molding compound of the present invention is significantly reduced with unsaturated polyester resin cost and with the excellent mechanical property of holding.
Description
Technical field
The invention belongs to chemical fields, and in particular to a kind of tubular molding compound unsaturated polyester resin and its preparation side
Method.
Background technology
BMC (DMC) material is the abbreviation of Bulk (Dough) molding compounds, i.e. tubular molding compound.It is domestic normal
Referred to as unsaturated polyester (UP) tubular molding compound.Its primary raw material is by GF (short glass fiber), UP (unsaturated-resin), MD (filler)
And the dough shape prepreg that various additives are adequately mixed.DMC materials in the twentieth century sixties in preceding West Germany and
Britain is applied first, has then obtained larger development in the U.S. and Japan respectively in the seventies and the eighties.Because of BMC
Tubular molding compound has excellent electric property, mechanical performance, heat resistance, chemical resistance, and adapts to various moulding process,
Requirement of the various products to performance can be met, therefore increasingly liked by users.
For BMC products although by the continuous development and improvement of decades, BMC product costs are high, also there is research at present
Attempt to reduce cost, but mechanical property can be caused insufficient, seriously limit its commercial Application.
Invention content
It is an object of the present invention to overcome the above deficiencies, and providing a kind of cost significantly reduces and can keep excellent power
Learn the tubular molding compound unsaturated polyester resin of performance.
It is a further object of the present invention to provide the preparation methods of above-mentioned tubular molding compound unsaturated polyester resin.
The purpose of the present invention is what is be accomplished by the following way：
A kind of tubular molding compound unsaturated polyester resin, the resin are mainly made of the raw material of following parts by weight：
Phthalic anhydride 2000-2500 parts by weight, cis-butenedioic anhydride 7500-8500 parts by weight, diethylene glycol 3500-4000 parts by weight, 1,2-
Propylene glycol 4500-5000 parts by weight, antioxidant 3-5 parts by weight, polymerization inhibitor 8-12 parts by weight, methylnaphthohydroquinone 3-7 parts by weight, benzene second
Alkene 8500-9000 parts by weight, 1,4-benzoquinone 1-2 parts by weight.
The resin is preferably mainly made of the raw material of following parts by weight：
Phthalic anhydride 2200-2500 parts by weight, cis-butenedioic anhydride 7500-8000 parts by weight, diethylene glycol 3500-3700 parts by weight, 1,2-
Propylene glycol 4500-4800 parts by weight, antioxidant 3-4 parts by weight, polymerization inhibitor 8-10 parts by weight, methylnaphthohydroquinone 5-7 parts by weight, benzene second
Alkene 8500-8800 parts by weight, 1,4-benzoquinone 1-1.5 parts by weight.
The resin is most preferably mainly made of the raw material of following parts by weight：
2000 parts by weight of phthalic anhydride, 7500 parts by weight of cis-butenedioic anhydride, 3700 parts by weight of diethylene glycol, 4500 weight of 1,2-PD
Part, 3 parts by weight of antioxidant, 8 parts by weight of polymerization inhibitor, 7 parts by weight of methylnaphthohydroquinone, 8500 parts by weight of styrene, 1 weight of 1,4-benzoquinone
Part.
Polymerization inhibitor of the present invention is preferably hydroquinone, and antioxidant is preferably triphenyl phosphite, and retarder is preferred
For copper naphthenate.
The preparation method of above-mentioned tubular molding compound unsaturated polyester resin includes the following steps：
A) it is 1.5~1.8m in nitrogen flow3Under conditions of/h, by 1,2 propylene glycol, diethylene glycol, 3/5 polymerization inhibitor,
205 DEG C, insulation reaction 5-8h are warming up to the speed of 10-12 DEG C/h after phthalic anhydride, cis-butenedioic anhydride and antioxidant mixing, is reacted to middle control acid
Value carries out decompression dehydration, until acid value is cooled to 195 DEG C, adds in remaining up to 31~37mgKOH/g up to 39~45mgKOH/g
Polymerization inhibitor and 2/7 methylnaphthohydroquinone, be cooled to 185 DEG C and obtain unsaturated polyester resin；
B) unsaturated polyester resin of acquirement is slowly added into the mixed of styrene and 1,4-benzoquinone and remaining methylnaphthohydroquinone
It closes in object, is cooled to 70~80 DEG C while stirring, 2~3h adds whole unsaturated polyester resins, then is cooled to 40~45 DEG C.
Polymerization inhibitor described in this method is preferably hydroquinone, and antioxidant is preferably triphenyl phosphite.
The tubular molding compound that the present invention obtains can also be cured with unsaturated polyester resin, gel time control 30~
40min.Added in during curing conventional accelerating agent, curing agent etc. according in GB/T8237-2005 " making of sample " will
It asks and casting matrix is made.
Beneficial effects of the present invention compared with the prior art：
The present invention as compound retarder, prevents product premature cure using the 1,4-benzoquinone and methylnaphthohydroquinone of specific dosage,
72 days storage periods or more can be improved than traditional product.Simultaneously its specific feed postition can also prevent it is inappropriate polymerization and shadow
Ring reaction speed.Present invention combined use 1,2-PD and diethylene glycol, the conventional neopentyl glycol of replacement, methyl propanediol, two
The expensive raw material such as propylene glycol, cost significantly reduces on the basis of excellent mechanical property is ensured.In preparation process,
Middle control acid value is preferably between 39~45mgKOH/g, if acid value is excessively high, free acid or acid are more, are easily lost in；If acid value mistake
It is low, then it can waste time significantly.During present invention reaction, using the nitrogen of specific flow velocity, conducive to moisture content is carried, contribute to reaction
It carries out.
The bending strength of tubular molding compound of the present invention resin may be up to more than 110MPa, and tensile strength may be up to 65MPa
More than.
Specific embodiment
It is further illustrated the present invention below by way of specific embodiment.But the detail of embodiment is only used for explaining this hair
It is bright, it should not be construed as limited overall technical solution.
Embodiment 1
Formula：2000 parts by weight of phthalic anhydride, 7500 parts by weight of cis-butenedioic anhydride, 3700 parts by weight of diethylene glycol, 1,2-PD 4500
Parts by weight, 3 parts by weight of triphenyl phosphite, 8 parts by weight of hydroquinone, 7 parts by weight of methylnaphthohydroquinone, 8500 parts by weight of styrene,
1 parts by weight of 1,4-benzoquinone.
The preparation method of tubular molding compound unsaturated polyester resin is：
A) it is 1.5~1.8m in nitrogen flow3Under conditions of/h, by 1,2 propylene glycol, diethylene glycol, 3/5 polymerization inhibitor,
205 DEG C, insulation reaction 5-8h are warming up to the speed of 10-12 DEG C/h after phthalic anhydride, cis-butenedioic anhydride and antioxidant mixing, is reacted to middle control acid
Value carries out decompression dehydration, until acid value is cooled to 195 DEG C, adds in remaining up to 31~37mgKOH/g up to 39~45mgKOH/g
Polymerization inhibitor and 2/7 methylnaphthohydroquinone, be cooled to 185 DEG C and obtain unsaturated polyester resin；
B) unsaturated polyester resin of acquirement is slowly added into the mixed of styrene and 1,4-benzoquinone and remaining methylnaphthohydroquinone
It closes in object, is cooled to 70~80 DEG C while stirring, 2~3h adds whole unsaturated polyester resins, then is cooled to 40~45 DEG C.
The cobalt iso-octoate of resin 100g and 2g and the cyclohexanone peroxide of 2g obtained becomes after gel 40min solid
Body, room temperature 24 hours are dried 3 hours at 60 DEG C, and 110 DEG C of conditions are dried 1 hour, and casting is made in room temperature after 24 hours
Body, this method are that casting matrix is made according to the custom requirements of " making of sample " in GB/T8237/2005.
Embodiment 2
Formula：2200 parts by weight of phthalic anhydride, 8000 parts by weight of cis-butenedioic anhydride, 3500 parts by weight of diethylene glycol,
4800 parts by weight of 1,2-PD, 3 parts by weight of triphenyl phosphite, 10 parts by weight of hydroquinone, 5 weight of methylnaphthohydroquinone
Measure part, 8800 parts by weight of styrene, 1 parts by weight of 1,4-benzoquinone.
The preparation method of tubular molding compound unsaturated polyester resin is：
A) it is 1.5~1.8m in nitrogen flow3Under conditions of/h, by 1,2 propylene glycol, diethylene glycol, 3/5 polymerization inhibitor,
205 DEG C, insulation reaction 5-8h are warming up to the speed of 10-12 DEG C/h after phthalic anhydride, cis-butenedioic anhydride and antioxidant mixing, is reacted to middle control acid
Value carries out decompression dehydration, until acid value is cooled to 195 DEG C, adds in remaining up to 31~37mgKOH/g up to 39~45mgKOH/g
Polymerization inhibitor and 2/7 methylnaphthohydroquinone, be cooled to 185 DEG C and obtain unsaturated polyester resin；
B) unsaturated polyester resin of acquirement is slowly added into the mixed of styrene and 1,4-benzoquinone and remaining methylnaphthohydroquinone
It closes in object, is cooled to 70~80 DEG C while stirring, 2~3h adds whole unsaturated polyester resins, then is cooled to 40~45 DEG C.
The cobalt iso-octoate of resin 100g and 2g and the cyclohexanone peroxide of 2g obtained becomes after gel 30min solid
Body, room temperature 24 hours are dried 3 hours at 60 DEG C, and 110 DEG C of conditions are dried 1 hour, and casting is made in room temperature after 24 hours
Body, this method are that casting matrix is made according to the custom requirements of " making of sample " in GB/T8237/2005.
Embodiment 3
Formula：2500 parts by weight of phthalic anhydride, 7500 parts by weight of cis-butenedioic anhydride, 3700 parts by weight of diethylene glycol,
4500 parts by weight of 1,2-PD, 4 parts by weight of triphenyl phosphite, 8 parts by weight of hydroquinone, 7 weight of methylnaphthohydroquinone
Measure part, 8500 parts by weight of styrene, 1.5 parts by weight of 1,4-benzoquinone.
The preparation method of tubular molding compound unsaturated polyester resin is：
A) it is 1.5~1.8m in nitrogen flow3Under conditions of/h, by 1,2 propylene glycol, diethylene glycol, 3/5 polymerization inhibitor,
205 DEG C, insulation reaction 5-8h are warming up to the speed of 10-12 DEG C/h after phthalic anhydride, cis-butenedioic anhydride and antioxidant mixing, is reacted to middle control acid
Value carries out decompression dehydration, until acid value is cooled to 195 DEG C, adds in remaining up to 31~37mgKOH/g up to 39~45mgKOH/g
Polymerization inhibitor and 2/7 methylnaphthohydroquinone, be cooled to 185 DEG C and obtain unsaturated polyester resin；
B) unsaturated polyester resin of acquirement is slowly added into the mixed of styrene and 1,4-benzoquinone and remaining methylnaphthohydroquinone
It closes in object, is cooled to 70~80 DEG C while stirring, 2~3h adds whole unsaturated polyester resins, then is cooled to 40~45 DEG C.
The cobalt iso-octoate of resin 100g and 2g and the cyclohexanone peroxide of 2g obtained becomes after gel 30min solid
Body, room temperature 24 hours are dried 3 hours at 60 DEG C, and 110 DEG C of conditions are dried 1 hour, and casting is made in room temperature after 24 hours
Body, this method are that casting matrix is made according to the custom requirements of " making of sample " in GB/T8237/2005.
Embodiment 4
Formula：2500 parts by weight of phthalic anhydride, 8500 parts by weight of cis-butenedioic anhydride, 4000 parts by weight of diethylene glycol,
5000 parts by weight of 1,2-PD, 5 parts by weight of antioxidant, 12 parts by weight of polymerization inhibitor, 7 parts by weight of methylnaphthohydroquinone, benzene
8500 parts by weight of ethylene, 2 parts by weight of 1,4-benzoquinone.
The preparation method is the same as that of Example 1.
Embodiment 5
Formula：2000 parts by weight of phthalic anhydride, 7500 parts by weight of cis-butenedioic anhydride, 3500 parts by weight of diethylene glycol,
4500 parts by weight of 1,2-PD, 3 parts by weight of antioxidant, 8 parts by weight of polymerization inhibitor, 3 parts by weight of methylnaphthohydroquinone, benzene second
8500 parts by weight of alkene, 1 parts by weight of 1,4-benzoquinone.
The preparation method is the same as that of Example 1.
Material property detection data such as table 1 is prepared according to Examples 1 to 5 method：
Table 1
Conventional production process and process is not described in detail in the present invention, and detailed specific method and process can combine above-mentioned
Production method and conventional method are implemented, and person of ordinary skill in the field is fully able to repeat to realize.
Claims (8)
1. a kind of tubular molding compound unsaturated polyester resin, it is characterised in that the resin is mainly by the raw material system of following parts by weight
Into：
Phthalic anhydride 2000-2500 parts by weight, cis-butenedioic anhydride 7500-8500 parts by weight, diethylene glycol 3500-4000 parts by weight, 1,2- the third two
Alcohol 4500-5000 parts by weight, antioxidant 3-5 parts by weight, polymerization inhibitor 8-12 parts by weight, methylnaphthohydroquinone 3-7 parts by weight, styrene
8500-9000 parts by weight, 1,4-benzoquinone 1-2 parts by weight；
The tubular molding compound is as made from following preparation method with unsaturated polyester resin, and step is as follows：
A) it is 1.5~1.8m in nitrogen flow3Under conditions of/h, by 1,2- propylene glycol, diethylene glycol, 3/5 polymerization inhibitor, benzene
205 DEG C, insulation reaction 5-8h are warming up to the speed of 10-12 DEG C/h after acid anhydride, cis-butenedioic anhydride and antioxidant mixing, is reacted to middle control acid value
Up to 39~45mgKOH/g, decompression dehydration is carried out, until acid value is cooled to 195 DEG C, adds in remaining up to 31~37mgKOH/g
Polymerization inhibitor and 2/7 methylnaphthohydroquinone are cooled to 185 DEG C and obtain unsaturated polyester resin；
B) unsaturated polyester resin of acquirement is slowly added into the mixture of styrene and 1,4-benzoquinone and remaining methylnaphthohydroquinone
In, it is cooled to 70~80 DEG C while stirring, 2~3h adds whole unsaturated polyester resins, then is cooled to 40~45 DEG C.
2. tubular molding compound unsaturated polyester resin according to claim 1, it is characterised in that the resin mainly by with
The raw material of lower parts by weight is made：
Phthalic anhydride 2200-2500 parts by weight, cis-butenedioic anhydride 7500-8000 parts by weight, diethylene glycol 3500-3700 parts by weight, 1,2- the third two
Alcohol 4500-4800 parts by weight, antioxidant 3-4 parts by weight, polymerization inhibitor 8-10 parts by weight, methylnaphthohydroquinone 5-7 parts by weight, styrene
8500-8800 parts by weight, 1,4-benzoquinone 1-1.5 parts by weight.
3. tubular molding compound unsaturated polyester resin according to claim 1, it is characterised in that the resin mainly by with
The raw material of lower parts by weight is made：
2000 parts by weight of phthalic anhydride, 7500 parts by weight of cis-butenedioic anhydride, 3700 parts by weight of diethylene glycol, 4500 parts by weight of 1,2-PD resist
3 parts by weight of oxygen agent, 8 parts by weight of polymerization inhibitor, 7 parts by weight of methylnaphthohydroquinone, 8500 parts by weight of styrene, 1 parts by weight of 1,4-benzoquinone.
4. according to the tubular molding compound unsaturated polyester resin described in claim 1,2 or 3, it is characterised in that the inhibition
Agent is hydroquinone.
5. according to the tubular molding compound unsaturated polyester resin described in claim 1,2 or 3, it is characterised in that the antioxygen
Agent is triphenyl phosphite.
6. a kind of preparation method of the tubular molding compound unsaturated polyester resin described in claim 1,2 or 3, it is characterised in that
This method includes the following steps：
A) it is 1.5~1.8m in nitrogen flow3Under conditions of/h, by 1,2- propylene glycol, diethylene glycol, 3/5 polymerization inhibitor, benzene
205 DEG C, insulation reaction 5-8h are warming up to the speed of 10-12 DEG C/h after acid anhydride, cis-butenedioic anhydride and antioxidant mixing, is reacted to middle control acid value
Up to 39~45mgKOH/g, decompression dehydration is carried out, until acid value is cooled to 195 DEG C, adds in remaining up to 31~37mgKOH/g
Polymerization inhibitor and 2/7 methylnaphthohydroquinone are cooled to 185 DEG C and obtain unsaturated polyester resin；
B) unsaturated polyester resin of acquirement is slowly added into the mixture of styrene and 1,4-benzoquinone and remaining methylnaphthohydroquinone
In, it is cooled to 70~80 DEG C while stirring, 2~3h adds whole unsaturated polyester resins, then is cooled to 40~45 DEG C.
7. the preparation method of tubular molding compound unsaturated polyester resin according to claim 6, it is characterised in that described
Polymerization inhibitor be hydroquinone.
8. the preparation method of tubular molding compound unsaturated polyester resin according to claim 6, it is characterised in that described
Antioxidant be triphenyl phosphite.
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| CN109400857B (en) * | 2018-09-15 | 2021-01-01 | 福建省南安市华龙树脂有限公司 | Soft unsaturated polyester resin for furniture industry and preparation method thereof |
| 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 |
| 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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