CN113549178A - High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer and preparation method thereof - Google Patents
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
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- C08K7/00—Use of ingredients characterised by shape
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- C08K7/26—Silicon- containing compounds
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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Abstract
The invention discloses a high-strength BMC bulk molding compound prepared from PMMA powder and MMA monomers, and belongs to the technical field of bulk molding compounds. The bulk molding compound is prepared from the following raw materials in parts by weight: 1800-2200 parts of PMMA matrix resin, 550 parts of PMMA powder, 50-80 parts of initiator, 3-7 parts of polymerization inhibitor, 3400-3600 parts of filling material, 50-70 parts of internal release agent, 5-10 parts of BYK dispersing agent, 370 parts of thickening agent 330-100 parts of color paste, 80-120 parts of 10mm glass fiber and 20-30 parts of auxiliary agent. The invention relates to a high-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer, which is prepared from PMMA (polymethyl methacrylate) powder according to the mass ratio of 1: 1.2 dissolving in MMA monomer to prepare matrix resin, and assisting 1: MMA solution of 50HQ as polymerization inhibitor, 1: the MMA solution of 0.5TBPB is used as an initiator, and the fumed silica is used as a tackifier to prepare the kneaded BMC dough material, so that the required ATH filler is obviously reduced, and the obtained product has excellent strength performance.
Description
Technical Field
The invention belongs to the technical field of bulk molding compounds, and particularly relates to a high-strength BMC bulk molding compound prepared from PMMA powder and MMA monomers.
Background
Along with the development requirements of environmental protection and industrialization, the BMC molding composite material forming process and application are rapidly developing in recent years, the application range of products is continuously expanded, and the demand of home decoration, white household appliances and tableware is particularly promoted year by year. The new requirements on the material performance are put forward, and corresponding improvement and research are needed to be carried out so as to improve the physical property and the environmental protection level of the product.
The prior application CN111040353A of the applicant of the present invention discloses a bulk molding compound without styrene component, which is prepared by polymethyl methacrylate powder. The bulk molding compound is prepared from 1800-toughened 2300 parts of MMA resin, 260-toughened 320 parts of polymethyl methacrylate PMMA powder, 53-66 parts of initiator, 29700-toughened 32500 parts of filler, 80-120 parts of color paste, 380-toughened 435 parts of glass fiber and 23-29 parts of auxiliary agent, wherein the filler is used in a large amount.
Disclosure of Invention
The applicant of the present invention has conducted a series of studies on the reduction of the ATH content in the filler of the above prior application, and found that the raw material formula of the filler ATH can be reduced, and at the same time, part of the properties of the obtained BMC bulk molding compound are significantly superior to those of the prior application, and an unexpected technical effect is obtained.
The invention uses PMMA (polymethyl methacrylate) powder according to the mass ratio of 1: 1.2 dissolving in MMA monomer to prepare matrix resin, and assisting 1: MMA solution of 50HQ as polymerization inhibitor, 1: MMA solution of 0.5TBPB as initiator and fumed silica as tackifier to prepare kneaded BMC dough material.
The invention discloses a high-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer, which is prepared from the following raw materials in parts by weight:
1800-2200 parts of PMMA matrix resin, 550 parts of PMMA powder, 50-80 parts of initiator, 3-7 parts of polymerization inhibitor, 3400-3600 parts of filling material, 50-70 parts of internal release agent, 5-10 parts of BYK dispersing agent, 370 parts of thickening agent 330-100 parts of color paste, 80-120 parts of 10mm glass fiber and 20-30 parts of auxiliary agent.
In some preferred embodiments of the present invention, the composition is prepared from the following raw materials in parts by weight:
2000 parts of PMMA matrix resin, 500 parts of PMMA powder, 60 parts of initiator, 5 parts of polymerization inhibitor, 3500 parts of filling material ATH, 60 parts of internal release agent, 7 parts of BYK dispersing agent, 350 parts of thickening agent, 90 parts of color paste, 100 parts of 10mm glass fiber and 25 parts of auxiliary agent.
In some preferred embodiments of the present invention, the PMMA matrix resin is PMMA powder in a mass ratio of 1: (1-1.5) a matrix resin prepared by dissolving MMA monomer.
In some preferred embodiments of the present invention, the initiator is a mixture of 1: (0.3-0.8) of a mixed solution of TBPB and MMA.
In some preferred embodiments of the present invention, the polymerization inhibitor is a mixture of 1: (40-60) HQ MMA solution.
In some preferred embodiments of the present invention, the internal mold release agent is zinc stearate.
In some preferred embodiments of the present invention, the thickener is fumed silica powder.
The second aspect of the present invention is to disclose the method for preparing the bulk molding compound of the first aspect, wherein the raw materials are mixed and kneaded by a kneader, and the method comprises a step of forming at a medium-low temperature of 95-125 ℃.
In some preferred embodiments of the present invention, the method further comprises the step of determining the weight content of the thickener according to the following formula:
C＝K(a×C1+b×C2)；
wherein K is a correction coefficient, and takes a value of 0.7-0.9 when C1/C2 is more than or equal to 1.5, and takes a value of 1.1-1.3 when C1/C2 is less than 1.5; c1 is the weight content of PMMA in PMMA and MMA, C2 is the weight content of MMA in PMMA and MMA, a is a weight coefficient and takes the value of 0.8-1.2, and b is a weight coefficient and takes the value of 1.3-1.5.
In some preferred embodiments of the invention, the temperature during forming is controlled by the following PID algorithm:
wherein, the delta u (c) corresponds to the variation of the temperature in the time interval of two testing temperatures; kc is a constant, 8-9; f (C) is the deviation at the time of sampling C, f (C-1) is the deviation at the time of sampling C-1, and f (C-2) is the deviation at the time of sampling C-2; TS is sampling period, 1.0-1.1 s; TI is integration time, 1.5-2.0 min; TD is differential time, 1.0-1.5 min.
The invention has the beneficial effects that:
(1) the invention relates to a high-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer, which is prepared from PMMA (polymethyl methacrylate) powder according to the mass ratio of 1: 1.2 dissolving in MMA monomer to prepare matrix resin, and assisting 1: MMA solution of 50HQ as polymerization inhibitor, 1: the MMA solution of 0.5TBPB is used as an initiator, and the fumed silica is used as a tackifier to prepare the kneaded BMC dough material, so that the required ATH filler is obviously reduced, the strength performance of the obtained product is excellent, and the strength performance of the obtained product is not influenced.
(2) Because PMMA powder is dissolved in the matrix resin of MMA monomer and gas phase silicon dioxide, the PMMA powder is easier to disperse and uniform, and simultaneously, the process conditions required by product molding can realize thickening without adding magnesium oxide, so that the mass can obtain the viscosity required by molding without drying and heating, and the energy consumption is saved. PMMA powder is dissolved in MMA monomer, and the link is firmer during later stage molding and MMA monomer polymerization, so that the molded product has higher strength, stronger surface anti-fouling capability, higher hardness, corrosion resistance, higher aging resistance and the like. In addition, PMMA powder is dissolved in MMA monomer to be used as the BMC agglomerate molding temperature of the matrix resin, and is reduced to 95-125 ℃; the molding pressure is reduced to 8-12MPa, and the energy consumption is greatly reduced. Meanwhile, the BMC composite material without the styrene solvent can reach a food-grade material and is applied to production of white household appliances and tableware.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
In the present invention, all reagents are commercially available and conventional unless otherwise specified. The filler ATH is 800-1200 mesh ultrafine powder, and the fumed silica powder is hollow glass microspheres with the diameter of 7-40 nm. The auxiliary agent is a dispersing agent produced by BYK.
Unless otherwise specified, the examples and comparative examples are parallel tests with the same components, component contents, preparation steps, preparation parameters.
The invention is abbreviated: PMMA is polymethyl methacrylate, MMA is methyl methacrylate, TBPB is tert-butyl perbenzoate, HQ is hydroquinone, ATH is aluminum hydroxide, also known as alumina trihydrate.
Example 1
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The formula is as follows:
PMMA powder is prepared by mixing the following components in a mass ratio of 1: 1.2 preparing 1800 parts of matrix resin dissolved in MMA monomer, 450 parts of PMMA powder, and the volume ratio is 1: 50 parts of 0.5TBPB and MMA mixed solution (initiator) in a weight-volume ratio of 1: 3 parts of 50HQ MMA liquid (polymerization inhibitor), 3400 part of filling material ATH, 50 parts of zinc stearate (internal release agent), 5 parts of BYK dispersing agent, 330 parts of fumed silica powder (thickening agent), 80 parts of color paste, 80 parts of 10mm glass fiber and 20 parts of auxiliary agent.
The preparation method comprises the following steps:
after mixing the raw materials, the mixture was kneaded by a kneader.
Wherein, the method comprises a step of medium-low temperature molding at 95-125 ℃. The molding temperature is reduced to 95-125 ℃; the molding pressure is reduced to 8-12 MPa.
Example 2
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The formulation, which differs from example 1, is:
PMMA powder is prepared by mixing the following components in a mass ratio of 1: 1.2 preparing 2200 parts of matrix resin dissolved in MMA monomer, 550 parts of PMMA powder, and mixing the components in a volume ratio of 1: 80 parts of 0.5TBPB and MMA mixed solution (initiator) in a weight-volume ratio of 1: 7 parts of 50HQ MMA liquid (polymerization inhibitor), 3600 parts of filling material ATH, 70 parts of zinc stearate (internal release agent), 10 parts of BYK dispersing agent, 370 parts of fumed silica powder (thickening agent), 100 parts of color paste, 120 parts of 10mm glass fiber and 30 parts of auxiliary agent.
The preparation method is the same as example 1.
Example 3
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The formulation, which differs from example 1, is:
PMMA powder is prepared by mixing the following components in a mass ratio of 1: 1.2 dissolving 2000 parts of matrix resin prepared from MMA monomers, 500 parts of PMMA powder, and mixing the components in a volume ratio of 1: 60 parts of 0.5TBPB and MMA mixed solution (initiator) in a weight-volume ratio of 1: 5 parts of 50HQ MMA liquid (polymerization inhibitor), 3500 parts of filling material ATH, 60 parts of zinc stearate (internal release agent), 7 parts of BYK dispersing agent, 350 parts of fumed silica powder (thickening agent), 90 parts of color paste, 100 parts of 10mm glass fiber and 25 parts of auxiliary agent.
The preparation method is the same as example 1.
Example 4
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The formulation, which differs from example 1, is:
the method also comprises the step of determining the weight content of the thickening agent according to the following formula:
C＝K(a×C1+b×C2)；
wherein K is a correction coefficient, and takes a value of 0.7-0.9 when C1/C2 is more than or equal to 1.5, and takes a value of 1.1-1.3 when C1/C2 is less than 1.5; c1 is the weight content of PMMA in PMMA and MMA, C2 is the weight content of MMA in PMMA and MMA, a is a weight coefficient and takes the value of 0.8-1.2, and b is a weight coefficient and takes the value of 1.3-1.5.
The method for determining the weight content of the thickening agent in the embodiment can rapidly determine the content of the thickening agent according to the content and the proportion of PMMA and MMA. Within the range of thickener content determined by the method of this example, the bulk molding compound product has significantly better strength than products having thickener content outside the range.
Example 5
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The formulation, which differs from example 1, is:
the temperature during forming is controlled by the following PID algorithm:
wherein, the delta u (c) corresponds to the variation of the temperature in the time interval of two testing temperatures; kc is a constant, 8-9; f (C) is the deviation at the time of sampling C, f (C-1) is the deviation at the time of sampling C-1, and f (C-2) is the deviation at the time of sampling C-2; TS is sampling period, 1.0-1.1 s; TI is integration time, 1.5-2.0 min; TD is differential time, 1.0-1.5 min.
The temperature control method of the embodiment can reduce the temperature fluctuation in the molding process and reduce the performance products of the bulk molding compound in the same batch obtained by parallel processing.
Comparative example 1
A bulk molding compound without styrene component prepared from polymethyl methacrylate powder is prepared from 1800 parts of MMA resin, 260 parts of polymethyl methacrylate powder, 53 parts of initiator, 29700 parts of filler, 80 parts of color paste, 380 parts of glass fiber and 23 parts of auxiliary agent according to weight ratio.
The initiator is a mixed solution of MMA resin and TBPB, wherein the mass ratio of the MMA resin to the TBPB is 2: 1. The filler is aluminum hydroxide ATH. The length of the glass fiber is 8 mm. The auxiliary agent is HQ inhibitor.
The preparation method is the same as example 1.
Comparative example 2
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The formulation, which differs from example 1, is:
PMMA powder is prepared by mixing the following components in a mass ratio of 1: 1.2 preparing 1800 parts of matrix resin dissolved in MMA monomer, 450 parts of PMMA powder, and the volume ratio is 1: 50 parts of 0.5TBPB and MMA mixed solution (initiator) in a weight-volume ratio of 1: 3 parts of 50HQ MMA liquid (polymerization inhibitor), 3400 part of filling material ATH, 50 parts of zinc stearate (internal release agent), 5 parts of BYK dispersing agent, 130 parts of fumed silica powder (thickening agent), 80 parts of color paste, 80 parts of 10mm glass fiber and 20 parts of auxiliary agent.
The preparation method is the same as example 1.
Comparative example 3
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The formulation, which differs from example 1, is:
PMMA powder is prepared by mixing the following components in a mass ratio of 1: 1.2 preparing 1800 parts of matrix resin dissolved in MMA monomer, 450 parts of PMMA powder, and the volume ratio is 1: 50 parts of 0.5TBPB and MMA mixed solution (initiator) in a weight-volume ratio of 1: 3 parts of 50HQ MMA liquid (polymerization inhibitor), 2400 parts of filler ATH, 50 parts of zinc stearate (internal mold release agent), 5 parts of BYK dispersing agent, 330 parts of fumed silica powder (thickening agent), 80 parts of color paste, 80 parts of 10mm glass fiber and 20 parts of auxiliary agent.
The preparation method is the same as example 1.
Comparative example 4
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The difference from the examples is that 2000 parts of the base resin, PMMA powder and MMA, were not mixed to prepare a resin, but were directly mixed and kneaded together with other raw materials.
Comparative example 5
High-strength BMC bulk molding compound prepared from PMMA powder and MMA monomer
The formulation was the same as in example 1.
The preparation method is different from the example 1 in that the molding temperature is 180-200 ℃ and the molding pressure is 20-25 MPa.
Examples of the experiments
The bulk molding materials obtained in the examples and comparative examples of the present invention were tested for impact strength (cylinder holder, no notch) and flexural strength by the method of JB/T7770-1995 unsaturated polyester glass fiber reinforced Molding materials, and the results are shown in Table 1.
TABLE 1 Properties of the bulk Molding Compounds
| Impact strength/MPa | Flexural Strength/MPa | |
| Example 1 | 24 | 85 |
| Example 2 | 23 | 83 |
| Example 3 | 26 | 89 |
| Comparative example 1 | 22 | 82 |
| Comparative example 2 | 17 | 73 |
| Comparative example 3 | 21 | 80 |
| Comparative example 4 | 19 | 79 |
| Comparative example 5 | 21 | 81 |
The results show that examples 1-2 with reduced ATH content have slightly better impact and flexural strength than comparative example 1, indicating that this formulation reduces the amount of ATH used without affecting the product properties. In examples 1 to 3, example 3 is significantly superior to examples 1 and 2, and an unexpected technical effect is obtained. Comparative example 2, in which the content of fumed silica was reduced as compared to example 1, the impact strength and flexural strength were significantly reduced, illustrating the necessity and importance of fumed silica in the formulation; comparative example 3, in which the content of ATH as a filler is reduced, has significantly reduced impact strength and bending strength properties, indicating that a certain content of ATH needs to be ensured and cannot be reduced without limit; comparative example 4, in which the resin matrix was prepared without mixing PMMA powder and MMA, the impact strength and flexural strength properties were also significantly reduced, indicating that the matrix resin in which PMMA powder was dissolved in MMA monomer and fumed silica were more easily dispersed uniformly; the conventional comparative example 5 with higher temperature and higher pressure is adopted, the impact strength and the bending strength performance are also obviously reduced, which shows that the medium-temperature and low-pressure forming process aiming at the formula of the invention not only saves the capacity, but also does not influence or even improves the performance of the product, and obtains unexpected technical effects.
While the preferred embodiments and examples of the present invention have been described in detail, the present invention is not limited to the embodiments and examples, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (10)
1. The high-strength BMC bulk molding compound prepared from PMMA powder and MMA monomers is characterized by being prepared from the following raw materials in parts by weight:
1800-2200 parts of PMMA matrix resin, 550 parts of PMMA powder, 50-80 parts of initiator, 3-7 parts of polymerization inhibitor, 3400-3600 parts of filling material, 50-70 parts of internal release agent, 5-10 parts of BYK dispersing agent, 370 parts of thickening agent 330-100 parts of color paste, 80-120 parts of 10mm glass fiber and 20-30 parts of auxiliary agent.
2. A bulk molding compound as claimed in claim 1, characterized in that it is prepared from the following raw materials in parts by weight:
2000 parts of PMMA matrix resin, 500 parts of PMMA powder, 60 parts of initiator, 5 parts of polymerization inhibitor, 3500 parts of filling material ATH, 60 parts of internal release agent, 7 parts of BYK dispersing agent, 350 parts of thickening agent, 90 parts of color paste, 100 parts of 10mm glass fiber and 25 parts of auxiliary agent.
3. A bulk molding compound according to claim 1 or 2, wherein the PMMA matrix resin is PMMA powder in a mass ratio of 1: (1-1.5) a matrix resin prepared by dissolving MMA monomer.
4. A bulk moulding compound according to any one of claims 1 to 3, characterized in that said initiator is present in a volume ratio of 1: (0.3-0.8) of a mixed solution of TBPB and MMA.
5. A bulk moulding compound as claimed in any one of claims 1 to 4, wherein the polymerization inhibitor is present in a weight to volume ratio of 1: (40-60) HQ MMA solution.
6. A bulk moulding compound as claimed in any one of claims 1 to 5, characterized in that said internal mould release agent is zinc stearate.
7. A bulk moulding compound as claimed in any one of claims 1 to 6, characterized in that said thickener is fumed silica powder.
8. A method for producing a bulk molding compound as defined in any one of claims 1 to 7, wherein the raw materials are mixed and kneaded by a kneader, characterized by comprising a step of molding at a medium-low temperature of 95 to 125 ℃.
9. The method of claim 8, further comprising the step of determining the weight content of the thickener according to the following formula:
C＝K(a×C1+b×C2)；
wherein K is a correction coefficient, and takes a value of 0.7-0.9 when C1/C2 is more than or equal to 1.5, and takes a value of 1.1-1.3 when C1/C2 is less than 1.5; c1 is the weight content of PMMA in PMMA and MMA, C2 is the weight content of MMA in PMMA and MMA, a is a weight coefficient and takes the value of 0.8-1.2, and b is a weight coefficient and takes the value of 1.3-1.5.
10. The production method according to claim 8 or 9, wherein the temperature in the molding is controlled by the following PID algorithm:
wherein, the delta u (c) corresponds to the variation of the temperature in the time interval of two testing temperatures; kc is a constant, 8-9; f (C) is the deviation at the time of sampling C, f (C-1) is the deviation at the time of sampling C-1, and f (C-2) is the deviation at the time of sampling C-2; TS is sampling period, 1.0-1.1 s; TI is integration time, 1.5-2.0 min; TD is differential time, 1.0-1.5 min.
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| CN117069974A (en) * | 2023-07-18 | 2023-11-17 | 哈尔滨工业大学 | Methyl methacrylate resin system and method for forming fiber reinforced material by room-temperature in-situ dip transfer molding |
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