CN116144154A - Heat-resistant yellowing-resistant unsaturated polyester molding compound and preparation method thereof - Google Patents
Heat-resistant yellowing-resistant unsaturated polyester molding compound and preparation method thereof Download PDFInfo
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- CN116144154A CN116144154A CN202111396527.7A CN202111396527A CN116144154A CN 116144154 A CN116144154 A CN 116144154A CN 202111396527 A CN202111396527 A CN 202111396527A CN 116144154 A CN116144154 A CN 116144154A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/06—Unsaturated polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a heat-resistant yellowing-resistant unsaturated polyester molding compound and a preparation method thereof, wherein the heat-resistant yellowing-resistant unsaturated polyester molding compound comprises m-benzene type unsaturated polyester resin, a low shrinkage agent, dicetyl peroxydicarbonate, bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, modified calcium carbonate, aluminum hydroxide and reinforcing fibers. The invention is designed by matching with the design and the forming process from the two angles of improving the heat resistance of the material and removing the yellowing factor, effectively improves the high temperature resistance of the unsaturated polyester molding compound, removes the yellowing factor, namely peroxide, fundamentally solves the problems of surface yellowing, oxidization and aging of the unsaturated polyester molding compound product under heating or long-term illumination, and is suitable for household appliances such as electric iron shells, electric oven shells and the like.
Description
Technical Field
The invention relates to the field of thermosetting molding materials, in particular to a heat-resistant yellowing-resistant unsaturated polyester molding compound and a preparation method thereof.
Background
The bulk unsaturated polyester molding compound BMC (BulkMolding Compound) is used as an excellent insulating material, and is widely used as an insulating material for electrical products such as switches, electric appliances and insulating parts of electric appliances since the bulk unsaturated polyester molding compound has the advantages of good dielectric property, stable size in a high-temperature environment, small shrinkage after curing and the like.
The electric iron, the electric oven and other articles for daily use have higher performance requirements on the materials of the electric iron and the electric oven because of higher working temperature. Chinese patent CN 102993660B discloses a preparation method of high-temperature-resistant flame-retardant unsaturated polyester molding compound, which takes p-benzene-type unsaturated polyester resin, a compound low-shrinkage additive, an initiator, a polymerization inhibitor, a thickener, a flame retardant, a mold release agent, ground glass fibers and reinforcing fibers as raw materials to prepare the high-temperature-resistant flame-retardant unsaturated polyester molding compound, but the applicant finds that the corresponding unsaturated polyester molding compound is obviously yellowing phenomenon of the surface of a product under heating or long-term illumination when the formula is used for preparing the corresponding unsaturated polyester molding compound and being used as an electric iron shell and an electric oven shell test, and can not meet the use requirements of beautifying the appearance and heat-resistant stability of household articles.
Disclosure of Invention
The invention provides a heat-resistant yellowing-resistant unsaturated polyester molding compound and a preparation method thereof, which solve the problem of yellowing when the unsaturated polyester molding compound is used as small household appliances such as an electric iron shell, an electric oven shell and the like in the prior art.
In order to solve the technical problems, the invention provides a heat-resistant yellowing-resistant unsaturated polyester molding compound which comprises the following components in percentage by weight:
14 to 15 percent of m-benzene type unsaturated polyester resin, 8 to 9 percent of low shrinkage agent, 0.3 to 0.35 percent of dicetyl peroxydicarbonate, 0.2 to 0.3 percent of bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, 30 to 40 percent of modified calcium carbonate, 30 to 40 percent of aluminum hydroxide and 1 to 16 percent of reinforcing fiber.
In a preferred embodiment of the present invention, the low shrinkage agent is polyvinyl acetate.
In a preferred embodiment of the invention, the reinforcing fibers are surface-coupled modified chopped glass fibers.
In a preferred embodiment of the invention, the length of the reinforcing fibers is 6 to 24mm.
In a preferred embodiment of the present invention, the modification method of the reinforcing fiber is as follows: adding the coupling agent, the high-hardness inorganic filler and the chopped glass fibers into a high-speed mixer according to a certain mass ratio, and mixing for 5-10 min to obtain the surface modified reinforced fibers.
In a preferred embodiment of the invention, the mass ratio of the coupling agent, the high-hardness inorganic filler and the chopped glass fibers is 1:10:90.
In a preferred embodiment of the present invention, the coupling agent is a silane coupling agent, and the high-hardness inorganic filler includes ultrafine aluminum hydroxide in a gibbsite type crystal form.
In order to solve the technical problems, the invention also provides a preparation method of the high heat-resistant yellowing-resistant unsaturated polyester molding compound, which comprises the following steps:
(1) And (3) preparing slurry: adding other components except the reinforced fibers into a mixer according to the formula proportion, mixing to obtain a mixed material a, and pumping into an automatic metering barrel for standby;
(2) Mixing by a double-roller open mill: adding the reinforced fibers and the mixed material a prepared in the step (1) to a double-roller open mill according to the formula proportion, and mixing by a wrapping roller to obtain a mixed material b;
(3) Molding and performance testing: and (3) after curing and forming the mixed material b, preparing a test sample, and performing performance test.
In a preferred embodiment of the present invention, in the step (3), the process conditions of the curing molding are: the molding temperature is 180 ℃ and the molding time is 30-60 s.
The beneficial effects of the invention are as follows: according to the heat-resistant yellowing-resistant unsaturated polyester molding compound and the preparation method thereof, from the two angles of improving the heat resistance of the material and removing yellowing factors, the formula design and the design of the molding process are carried out, and on one hand, the heat resistance of the molding compound is improved by selecting high-temperature-resistant m-benzene unsaturated polyester resin as matrix resin; on the other hand, the use of the bi (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite which has high curing temperature and low residue and can react with peroxide residue of the curing agent is adopted as the curing agent, so that the main substance peroxide which causes yellowing is eliminated, the problem of surface yellowing of an unsaturated polyester molding compound product under heating or long-term illumination is effectively solved, and the prepared unsaturated polyester molding compound has no yellowing phenomenon when used as household appliances such as an electric iron shell, an electric oven shell and the like, and has wide market prospect.
Drawings
FIG. 1 is a schematic process flow diagram of a method for preparing heat-resistant yellowing-resistant unsaturated polyester molding compound.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making clear and defining the scope of the present invention.
According to the invention, through the selection and use of the raw materials of the formula and the matching of the molding process, on one hand, the heat resistance of the molding compound is improved, the yellowing resistance of the molding compound is improved, and on the other hand, the factors causing yellowing caused by heating and long-term illumination in the molding compound are effectively removed. Through the comprehensive effect of the measures, the difficult problem that the unsaturated polyester molding compound is easy to yellow after being heated and illuminated for a long time is fundamentally solved.
The invention discloses a heat-resistant yellowing-resistant unsaturated polyester molding compound which comprises the following components in percentage by weight:
14-15% of m-benzene type unsaturated polyester resin; in the molecular formula of the m-benzene type unsaturated polyester resin, two ester groups on a main chain are far apart, the space effect is small, the m-benzene type unsaturated polyester resin has excellent physical and chemical properties, and the m-benzene type unsaturated polyester resin has excellent heat resistance, so that a molding compound product prepared by using the m-benzene type unsaturated polyester resin as a binder has good mechanical properties, toughness, heat resistance and corrosion resistance.
8-9% of low shrinkage agent, wherein the low shrinkage agent is polyvinyl acetate, and the polyvinyl acetate is excellent in performance, is heat-resistant, can effectively reduce the yield rate of preparation, and improves the surface finish.
And the dicetyl peroxydicarbonate is 0.3-0.35%, and is a safe and environment-friendly curing agent with higher reaction temperature, good tolerance and low residue after reaction. Residual curing agent (residual peroxide) after molding of the molding compound product can seriously affect heat resistance of the product, so that the product can yellow on the surface under long-term illumination or high-temperature conditions, and the product has poor heat stability and the surface is yellow. The selection of the dicetyl peroxydicarbonate with high curing temperature and low residue after curing can effectively improve the stability of the unsaturated polyester molding compound and effectively prevent yellowing.
The bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite accounts for 0.2 to 0.3 percent, and the bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite is an antioxidant, has an antioxidant effect on one hand, has a good protection effect on the color of a polymer, and can neutralize peroxide remained after curing on the other hand, thereby effectively preventing yellowing of a molding compound product.
30-40% of modified calcium carbonate, wherein the modified calcium carbonate can be well combined with m-benzene type unsaturated polyester resin, thereby having a toughening effect, and also having a certain flame-retardant effect, and having a synergistic flame-retardant effect with environment-friendly aluminum hydroxide; specifically, the modification method of the modified calcium carbonate comprises the following steps: dissolving stearic acid in an organic solvent (such as 2-propanol) in advance, adding the dissolved stearic acid solution into calcium carbonate according to the mass ratio of stearic acid to calcium carbonate of 1%, mixing in a high-speed mixer, and mixing at a high speed of 500r/min for 15min at 100 ℃ to obtain the calcium carbonate.
1-16% of reinforcing fiber, wherein the reinforcing fiber is surface coupling modified chopped glass fiber, the length of the reinforcing fiber is 6-24 mm, and the bonding force between the reinforcing fiber and m-benzene type unsaturated polyester resin can be improved through surface coupling treatment, so that the mechanical strength of a product is improved. Specifically, the surface treatment method of the reinforcing fiber comprises the following steps: taking a silane coupling agent and a high-hardness inorganic filler as surface modifiers, and mixing the silane coupling agent, the high-hardness inorganic filler and the chopped glass fibers according to the following ratio of 1:10:90 mass ratio is added into a high-speed mixer to be mixed for 5min, so that the coupling agent is fully dispersed, and certain scratches are formed on the surface of the glass fiber by utilizing the high-hardness inorganic filler, thereby increasing the friction resistance of the glass fiber and the affinity of the glass fiber to the resin, facilitating the infiltration of the resin to the glass fiber, and obtaining the modified reinforcing fiber. The high-hardness inorganic filler is superfine aluminum hydroxide in a gibbsite crystal form with low oil absorption, and specifically, the oil absorption of the superfine aluminum hydroxide to linseed oil is less than 22g/100g (15 ℃ C., 20 min) and the fineness is 1 mu m. Ultrafine aluminium hydroxide may also be able to enhance the flame retardant effect.
30-40% of aluminum hydroxide, wherein the aluminum hydroxide not only can resist flame, but also can prevent smoke generation after combustion, does not produce dripping substances and does not produce toxic gas;
1.2 to 1.8 percent of zinc stearate, which is used for lubricating materials and demolding finished products of molding compounds;
0.1 to 0.15 percent of active magnesium oxide, which is used for adjusting the viscosity of materials and is beneficial to the full combination of resin matrix and other fillers;
0.3 to 0.5 percent of inorganic colorant which can be added according to the color requirement of the product, such as carbon black, ferric oxide pigment and the like;
and the p-benzoquinone is 0.002-0.03%, which is beneficial to improving the storage stability of the unsaturated molding compound finished product.
Example 1
Calculated according to the weight percentage content,
(1) And (3) preparing slurry: adding 14% of m-phenylene unsaturated polyester resin, 8% of polyvinyl acetate, 0.3% of dicetyl peroxydicarbonate, 0.3% of bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, 35% of modified calcium carbonate, 40% of aluminum hydroxide, 1.8% of zinc stearate, 0.15% of active magnesium oxide, 0.44% of carbon black and 0.01% of p-benzoquinone into a high-speed mixer, stirring and mixing for 10min at a rotating speed of 1500r/min at 50-80 ℃ to obtain a mixed material a, and feeding the mixed material a into an automatic metering barrel for standby;
adding antioxidant bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, liquid unsaturated polyester resin, other various powder and coloring agent into a high-speed mixer for mixing for more than 10min, and fully dispersing to play a role in resisting oxidation and yellowing;
(2) Mixing by a double-roller open mill: adding 8% of reinforcing fibers and the mixed material a prepared in the step (1) to a double roller of a double-roller open mill according to the formula proportion, and mixing by a covered roller to obtain a mixed material b;
the liquid sizing agent and the modified reinforced glass fiber are added to a double-roller machine in proportion for extrusion and discharging, the structure of the glass fiber is not damaged, and the mechanical strength and the heat resistance of a molding compound product are improved;
(3) Molding and performance testing: the mixture b was cured at 180℃for 30s. And (3) after curing and molding, preparing a test sample, and performing performance test. Through high-temperature curing at 180 ℃, the curing agent is decomposed more thoroughly, so that the residual quantity is further reduced, and the high-temperature resistance of the product is improved.
Example 2
The difference from example 1 is that:
the formula proportion of the selected materials is as follows:
15% of m-phenylene unsaturated polyester resin, 9% of polyvinyl acetate, 0.35% of dicetyl peroxydicarbonate, 0.3% of bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, 36% of modified calcium carbonate, 37% of aluminum hydroxide, 1.8% of zinc stearate, 0.15% of active magnesium oxide, 0.37% of carbon black and 0.03% of p-benzoquinone;
the preparation method is the same as in example 1.
And performing performance test on the test sample prepared in the embodiment.
The test contents are as follows:
flexural strength, reference standard GB/T9341;
impact strength, reference standard GB/T1043.1;
shrinkage, reference standard ISO 2577;
insulation resistance, reference standard GB/T1410;
flame retardant UL94;
load deformation temperature (8.0 MPa) GB/T1634.2;
and (3) testing yellowing, wherein the temperature of the oven is 160 ℃/24 hours.
The test results are shown in the following table:
the test data show that the unsaturated polyester molding compound prepared by the method has excellent electrical insulation, lower dimensional shrinkage, high temperature resistance, yellowing resistance and excellent flame retardance, and meets the requirements of household appliances such as electric iron shells, electric oven shells and the like on heat stability and yellowing resistance.
The heat-resistant yellowing-resistant unsaturated polyester molding compound and the preparation method thereof fundamentally solve the problems of heat resistance and the like of the molding compound and ensure surface yellowing of products under heating or long-term illumination, and the prepared household appliances such as electric iron shells, electric oven shells and the like have no yellowing phenomenon, so that the special functional unsaturated polyester molding compound for household appliance shells is high in use safety. Has the following advantages:
1. by selecting high-temperature resistant m-benzene type unsaturated polyester resin as matrix resin, the heat resistance of the matrix is ensured, the heat resistance of the molding compound is fundamentally improved, and the yellowing resistance of the finished product is improved;
2. by selecting the setting of the curing agent with high curing temperature and low residue and the antioxidant capable of reacting with the peroxide remained in the curing agent, on one hand, the residual amount of the curing agent after curing is effectively reduced, and on the other hand, the antioxidant reacts with the residual peroxide, so that the problem of surface yellowing of the unsaturated molding compound product under heating or long-term illumination is fundamentally solved;
3. by improving the preparation process of pulping and mixing with the reinforcing fibers on a double-roller open mill, the mixing period is shortened, and the uniformity of material dispersion is improved, so that the prepared unsaturated polyester molding compound has more stable performance.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. The heat-resistant yellowing-resistant unsaturated polyester molding compound is characterized by comprising the following components in percentage by weight:
14 to 15 percent of m-benzene type unsaturated polyester resin, 8 to 9 percent of low shrinkage agent, 0.3 to 0.35 percent of dicetyl peroxydicarbonate, 0.2 to 0.3 percent of bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, 30 to 40 percent of modified calcium carbonate, 30 to 40 percent of aluminum hydroxide and 1 to 16 percent of reinforcing fiber.
2. The heat and yellowing resistant unsaturated polyester molding compound of claim 1, wherein the low shrinkage agent is polyvinyl acetate.
3. The heat and yellowing resistant unsaturated polyester molding compound of claim 2, wherein the reinforcing fibers are surface-coupled modified chopped glass fibers.
4. The heat-resistant yellowing-resistant unsaturated polyester molding compound according to claim 3, wherein the length of the reinforcing fibers is 6 to 24mm.
5. The heat-resistant yellowing-resistant unsaturated polyester molding compound according to claim 4, wherein the reinforcing fiber modification method comprises: adding the coupling agent, the high-hardness inorganic filler and the chopped glass fibers into a high-speed mixer according to a certain mass ratio, and mixing for 5-10 min to obtain the surface modified reinforced fibers.
6. The heat-resistant yellowing-resistant unsaturated polyester molding compound according to claim 5, wherein the mass ratio of the coupling agent, the high-hardness inorganic filler and the chopped glass fibers is 1:10:90.
7. The heat-resistant yellowing-resistant unsaturated polyester molding compound according to claim 6, wherein the coupling agent is a silane coupling agent; the high-hardness inorganic filler comprises superfine aluminum hydroxide in a gibbsite crystal form.
8. The heat-resistant yellowing-resistant unsaturated polyester molding compound according to claim 7, further comprising the following components in percentage by weight: 1.2 to 1.8 percent of zinc stearate, 0.1 to 0.15 percent of active magnesium oxide, 0.3 to 0.5 percent of inorganic colorant and 0.002 to 0.03 percent of p-benzoquinone.
9. A process for the preparation of the heat-resistant yellowing-resistant unsaturated polyester molding compound according to claim 1 or 8, comprising the steps of:
(1) And (3) preparing slurry: adding other components except the reinforced fibers into a mixer according to the formula proportion, mixing to obtain a mixed material a, and pumping into an automatic metering barrel for standby;
(2) Mixing by a double-roller open mill: adding the reinforced fibers and the mixed material a prepared in the step (1) to a double-roller open mill according to the formula proportion, and mixing by a wrapping roller to obtain a mixed material b;
(3) Molding and performance testing: and (3) after curing and forming the mixed material b, preparing a test sample, and performing performance test.
10. The method for preparing heat-resistant yellowing-resistant unsaturated polyester molding compound according to claim 9, wherein in the step (3), the process conditions of curing and molding are as follows: the molding temperature is 180 ℃ and the molding time is 30-60 s.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213797A (en) * | 2022-01-11 | 2022-03-22 | 陈小云 | Wear-resistant scratch-resistant SMC (sheet molding compound) molding compound and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114213797A (en) * | 2022-01-11 | 2022-03-22 | 陈小云 | Wear-resistant scratch-resistant SMC (sheet molding compound) molding compound and preparation method thereof |
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