CN109435278B - Method for preparing large-size large-thickness polyester reinforced acrylate plate - Google Patents
Method for preparing large-size large-thickness polyester reinforced acrylate plate Download PDFInfo
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- CN109435278B CN109435278B CN201811547564.1A CN201811547564A CN109435278B CN 109435278 B CN109435278 B CN 109435278B CN 201811547564 A CN201811547564 A CN 201811547564A CN 109435278 B CN109435278 B CN 109435278B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/36—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and impregnating by casting, e.g. vacuum casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
- B29L2007/002—Panels; Plates; Sheets
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- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Polymerisation Methods In General (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The invention relates to a novel method for preparing a large-thickness polyester reinforced acrylate plate with uniform distribution, in particular to a method for preparing and polymerizing a large-thickness polyester reinforced acrylate plate by soaking polyester silk in a methyl methacrylate solution; the method is a method for preparing the acrylic ester board with large thickness and uniform distribution by uniformly and stably polymerizing polyester silk and methyl methacrylate solution through a uniform-speed overturning polymerization method of a 360-degree overturning machine, and is a novel method for preparing the composite material. The invention is prepared by casting and polymerizing 655 type polyester silk and methyl methacrylate, wherein the mass ratio of the polyester silk to the methyl methacrylate is 90 (+ -10): 100 (mass ratio). The invention can prepare the terylene enhanced acrylic ester plate with the thickness of 50mm and the uniformly distributed terylene silk in the internal structure of the plate.
Description
Technical Field
The invention relates to a novel method for preparing a large-thickness polyester reinforced acrylate plate with uniform distribution, in particular to a method for preparing and polymerizing a large-thickness polyester reinforced acrylate plate by soaking polyester silk in a methyl methacrylate solution; the method is a method for preparing the acrylic ester board with large thickness and uniform distribution by uniformly and stably polymerizing polyester silk and methyl methacrylate solution through a uniform-speed overturning polymerization method of a 360-degree overturning machine, and is a novel method for preparing the composite material.
Background
The terylene reinforced acrylic ester plate belongs to a composite material, is mainly applied to the connection of an organic glass product and an industrial equipment framework, and can transmit the external load born by an organic glass transparent part to the industrially prepared framework through a connecting piece made of the terylene reinforced acrylic ester plate. In recent years, organic glass has been widely used for an aircraft as a canopy, a windshield, and a quarter window due to its excellent physical and mechanical properties, and also as a windshield and a window of a jeep, a sunroof of a large building, a screen of a television and a radar, a shield of an instrument and a device, a housing of a telecommunication instrument, and the like. The organic glass hardware connection with the terylene reinforced acrylic ester plate as the reinforcing material is an excellent edge connection mode, and can effectively avoid stress concentration caused by edge drilling; the load on the organic glass transparent piece is uniformly transferred; the installation precision is high, and good air tightness can be ensured; meanwhile, the terylene reinforced acrylic ester plate material has similar physical and mechanical properties with the organic glass transparent member body material, and the linear expansion coefficient is similar, so that the stress caused by temperature change can be reduced. The aviation industry standard of D-1 polyester fabric reinforced acrylate plate manufacturing process published in 12 months of 1994 in China, the technology and the process can only produce small-size thin plates, and when the process is used for preparing plates with the thickness of 10mm or more, the polyester silk is unevenly distributed in the structure, so that the overall performance of the material is irregularly and disorderly dispersed, the bearing capacity of the frame edge connecting part of various types of industrial equipment is influenced, and potential safety hazards are brought, and the higher requirement of various types of industrial equipment on the edge connection of the organic glass transparent part cannot be met.
Disclosure of Invention
The invention adopts 655 type polyester silk and Methyl Methacrylate (MMA) to carry out bulk polymerization, fixes a certain amount of polyester silk in a special model, pours MMA serous fluid with certain viscosity, and prepares the terylene enhanced acrylic ester plate with the thickness of 50mm and the uniform distribution of the polyester silk in the internal structure of the plate through polymerization. And the terylene enhanced acrylic ester plates are uniformly distributed in the internal structure of the plate.
In the bulk polymerization process, the ratio of the initiator ABN to the methyl methacrylate is 0.005 (+ -0.001): 100 (mass ratio);
in the bulk polymerization process, the ratio of the light-resistant agent UVP to the methyl methacrylate is 0.05 (+ -0.01): 100 (mass ratio);
the content of resin (polymethyl methacrylate) in the polyester reinforced acrylate plate prepared by the method is 45-55 percent.
The invention solves the problem of internal uniformity of the large-thickness polyester reinforced acrylate plate material. Firstly, adding Methyl Methacrylate (MMA) qualified by inspection into a light-resistant agent UVP and an initiator ABN according to a mass ratio, pre-polymerizing at 75-80 ℃, cooling, stirring to room temperature, and performing vacuum treatment under (0.073-0.080) MPa to prepare MMA slurry with the viscosity of 12-20 s. Firstly, drying the required silk to be washed by a high-temperature pressing machine to improve the flatness, fixing the silk in a specific model, vertically placing the model into a water bath low-temperature overturning polymerization device after dust removal and impurity removal, filling prepared Methyl Methacrylate (MMA) slurry into the model, soaking for 12 hours, discharging bubbles between the silk cloth layers, carrying out vacuum degassing for 3 hours, and discharging gas between the silk cloth layers. The MMA and the polyester silk are uniformly distributed and the system reacts stably by utilizing the water bath low-temperature overturning tank to circularly overturn clockwise at 360 degrees at a certain rotating speed at 35 ℃. After the prepolymerization, the polyester reinforced acrylic ester board with large thickness is prepared by air bath high-temperature polymerization at 100-120 ℃. The terylene enhanced acrylic ester plate prepared in the way has the advantages that the terylene enhanced acrylic ester plate is uniformly distributed in the internal structure of the plate, the interlaminar shear strength, the tensile strength, the extrusion strength and other properties of the plate are greatly improved, the higher requirements of different users are met, the product quality of the terylene enhanced acrylic ester plate with large thickness is improved, the supply timeliness is ensured, the production process is easy to control, and the industrial production is easy to realize. The currently prepared sheet material with the thickness of 30mm passes the application examination of users and is approved.
The performance detection method of the large-thickness polyester reinforced acrylate plate comprises the following steps:
the interlaminar shear strength of the plate is detected according to the GJB 5872 test method for the interlaminar shear strength of oriented organic glass.
The linear expansion coefficient of the plate is detected according to the standard of GB 2572 test method for average linear expansion coefficient of fiber reinforced plastics.
Other performances of the plate are detected according to the standard of HB 5445 polyester reinforced acrylate plate specification.
Drawings
FIG. 1 is a sectional view of example 1.
FIG. 2 is a cross-sectional view of comparative example 1.
FIG. 3 is a cross-sectional view of comparative example 2.
Detailed Description
Example 1: adding 100 parts (by mass, hereinafter, referred to as mass parts) of refined qualified methyl methacrylate MMA, 0.05 part of light-resistant agent UVP and 0.005 part of initiator ABN into a polymerization kettle in proportion, stirring and heating to 75-80 ℃, cooling when the slurry viscosity reaches 12-20 s after reaction, preparing MMA slurry, and carrying out vacuum treatment for 30min at the normal temperature (0.073-0.080) MPa vacuum degree. Wash a certain amount silk and handle with high temperature pressing machine press, the silk is dry to the messenger, level and smooth no fold, will need wash the silk and fix and stack on clear lower bolster, on, the lower bolster coincidence, seal up with the soft plastic tubing of elasticity all around, when sealed on, feed inlet and gas vent are left to the lower extreme, the feed inlet is laid at the model lower extreme, the gas vent is at model upper end central connection exhaust apparatus, the model is tightened to requiring thickness with bow clamp all around, thickness in the middle of the large-scale anchor clamps control model for the model, the vertical type is placed in water bath low temperature upset polymerization groove. Injecting MMA slurry into a prepared model from a feed inlet at the lower end, soaking for 12 hours after grouting is completed, discharging bubbles between polyester silk fabrics, vacuumizing the model, wherein the vacuum pressure is more than or equal to 0.080MPa, sealing after 3 hours, maintaining in a water bath low-temperature overturning polymerization tank at 35 ℃, starting an overturning machine, circularly overturning the overturning machine clockwise by 360 degrees, and setting the overturning speed to be 20 +/-3/min. And maintaining the temperature of the elastomer, then carrying out air bath high-temperature polymerization at 100-120 ℃, maintaining the high-temperature polymerization for 3 hours, cooling and demolding to prepare the polyester reinforced acrylate plate. And (3) obtaining the terylene enhanced acrylate plate with uniformly distributed large-thickness materials after the surface inspection, the thickness inspection and the physical and mechanical property inspection of the plate. And preparing the terylene enhanced acrylic ester plate with the thickness of 30 mm. Through inspection, all the performances of the plate reach the requirements of HB 5445 polyester reinforced acrylate plate specification, and the shear strength of the plate is as high as 28MPa, which shows that the plate has a uniform internal structure; meanwhile, the linear expansion coefficient of the material is similar to that of organic glass, which shows the excellent matching property with the organic glass transparent piece.
Comparative example 1: (conventional water bath manufacturing 30mm thick plate)
MMA slurry was prepared as in the examples and used. Prepare to wash silk according to thickness needs and stack on clean lower bolster, upper and lower bolster coincidence is sealed with the flexible plastic tubing of elasticity all around, and feed inlet and gas vent are left to the upper end during sealed, and the gas vent connects exhaust apparatus at model upper end central authorities, and the model is tightened to required thickness with bow-shaped clamp all around, adopts vertical grout, pours MMA thick liquid from the feed inlet, and the air of getting rid of the model is inside until the model is filled with the thick liquid. The filled model was allowed to stand at room temperature for 24 hours with the bath polymerization parameters: and (3) raising the temperature to 35 +/-1 ℃, keeping the temperature for about 50-70 h, keeping the temperature for 31 +/-1 ℃, keeping the temperature for 24h, maintaining the temperature until the elastomer is polymerized at the high temperature of 110 ℃, maintaining the polymerization at the high temperature for 3h, cooling and demolding to prepare the polyester reinforced acrylate plate with the thickness of 30 mm.
Comparative example 2: (comparative example 1 analysis of the operation and grouting method, optimization of the process by combining the process conditions of the organic glass thick plate, polymerization in water bath, polymerization in air bath, and adjustment of polymerization temperature control conditions.)
MMA slurry was prepared as in the examples and used. Washing a certain amount of silk and fixedly stacking on a clean lower template, superposing the upper template and the lower template, sealing the periphery by using an elastic soft plastic pipe, reserving a feed inlet and an exhaust port at the upper end and the lower end during sealing, placing the feed inlet at the lower end of a model, connecting an exhaust device at the center of the upper end of the model by the exhaust port, tightening the periphery of the model by using an arch clamp to the required thickness, adopting vertical grouting, and naturally flowing MMA slurry into the model through the feed inlet at the lower part until the model is filled with the slurry. Standing the filled model at room temperature for 24h, horizontally placing a polymerization vehicle, putting the polymerization vehicle into a wind bath polymerization device, polymerizing at low temperature of 35 ℃ for about 120h, then heating to 110 ℃ for high-temperature polymerization, cooling and demolding after maintaining for 3h, and successfully preparing the 30 mm-thick polyester reinforced acrylate plate.
The product properties and technical indexes of the examples and comparative examples are compared in table 1:
table 1 comparison table of product performance and technical index
Observing the side surface after the plate is cut:
(1) example 1 the tangent plane is neat, washes silk evenly distributed, does not have fold, thickness is even.
(2) Comparative example 1 the polyester silk had wrinkles, and the surface of the plate had unevenness containing a large number of bubbles and had uneven thickness.
(3) Comparative example 2 polyester silk has no wrinkles, the matrix is layered, and the thickness is not uniform.
Claims (8)
1. A method for preparing a large-thickness terylene enhanced acrylate plate with uniformly distributed polyester silks is characterized by adding methyl methacrylate into a light resisting agent and an initiator for prepolymerization, then cooling to room temperature to prepare methyl methacrylate slurry with the viscosity of 12 s-20 s and the pressure of 0.073-0.080 MPa, carrying out vacuum treatment for 30 minutes, drying a certain amount of polyester silks by a high-temperature pressing machine to improve the flatness, fixing the polyester silks in a model, dedusting and removing impurities, vertically placing the model in a water bath polymerization turnover device, pouring the methyl methacrylate slurry, soaking for 12 hours, discharging bubbles among the polyester silk fabrics, carrying out vacuum pressure more than or equal to 0.080MPa, carrying out vacuum degassing for 3 hours to discharge gas among the polyester silks, carrying out cyclic turnover polymerization in a uniform speed turnover machine in a 360-degree clockwise direction at 30-40 ℃ in a water bath, and then carrying out high-temperature polymerization to prepare the large-thickness terylene enhanced acrylate plate, the mass ratio of the polyester silk added in the first polymerization to the methyl methacrylate is 90 +/-10: 100.
2. the method for preparing the polyester-silk uniformly distributed large-thickness polyester reinforced acrylate board as claimed in claim 1, wherein the initiator is ABN, and the mass ratio of the ABN to the methyl methacrylate is 0.005 +/-0.001: 100.
3. the method for preparing the polyester-silk uniformly distributed large-thickness polyester reinforced acrylate board as claimed in claim 1, wherein the light resistance agent is UVP, and the mass ratio of the UVP to the methyl methacrylate is 0.05 +/-0.01: 100.
4. the method for preparing the polyester-silk uniformly distributed large-thickness polyester-reinforced acrylate plate as claimed in claim 1, wherein the prepared polyester-reinforced acrylate plate has a polymethyl methacrylate content of 45-55%.
5. The method for preparing the polyester-silk uniformly distributed large-thickness polyester reinforced acrylate board as claimed in claim 1, wherein the pre-polymerization temperature is 75-80 ℃.
6. The method for preparing the large-thickness terylene enhanced acrylate sheet material with uniformly distributed polyester silk according to claim 1, wherein the high-temperature polymerization temperature is 100-120 ℃.
7. The method for preparing the large-thickness polyester reinforced acrylate board with uniformly distributed polyester silk according to claim 1, wherein the drying temperature of the high-temperature press is 100-120 ℃.
8. The method for preparing the polyester-silk uniformly distributed large-thickness polyester reinforced acrylate board as claimed in claim 1, wherein the overturning speed of the overturning device is 20 ± 3/min.
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| CN201811547564.1A CN109435278B (en) | 2018-12-18 | 2018-12-18 | Method for preparing large-size large-thickness polyester reinforced acrylate plate |
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| CN109435278B true CN109435278B (en) | 2021-01-15 |
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