Formula and synthesis method of large-thickness polymethyl methacrylate plate
阅读说明：本技术 大厚度聚甲基丙烯酸甲酯板材的配方及合成方法 (Formula and synthesis method of large-thickness polymethyl methacrylate plate ) 是由 吴贲华 陈云 高国忠 袁厚呈 申云飞 袁红柳 王健 于 2019-11-13 设计创作，主要内容包括：本发明涉及一种大厚度聚甲基丙烯酸甲酯板材的配方及合成方法,该合成方法包括以下步骤：取重量百分比为90.0％-98.0％的甲基丙烯酸甲酯、0.01％-0.5％的引发剂、1％-5％的抗紫外剂及0.01％-0.5％的调色剂混合在一起,并在真空条件下,加热搅拌,使其反应,形成反应液；冷却反应液,并于反应液中加入重量百分比为0.5％-5％的添加剂,形成预反应液；将预反应液浇注于模具内,加热模具,并保温,固化预反应液；重复上述步骤,直至模具中的固化的预反应液的高度达到所需制备的大厚度聚甲基丙烯酸甲酯板材的厚度；以及最终热处理,得到大厚度聚甲基丙烯酸甲酯板材。本发明具有透光率高、硬度高、抗压性能好等特点,非常适合用于潜水器观察窗,海底观光船。(The invention relates to a formula and a synthetic method of a large-thickness polymethyl methacrylate plate, wherein the synthetic method comprises the following steps: mixing 90.0-98.0 wt% of methyl methacrylate, 0.01-0.5 wt% of initiator, 1-5 wt% of anti-ultraviolet agent and 0.01-0.5 wt% of toner together, and heating and stirring under vacuum condition to react to form reaction liquid; cooling the reaction liquid, and adding 0.5-5 wt% of additive into the reaction liquid to form a pre-reaction liquid; pouring the pre-reaction liquid into a mold, heating the mold, preserving heat, and curing the pre-reaction liquid; repeating the steps until the height of the solidified pre-reaction liquid in the mould reaches the thickness of the prepared large-thickness polymethyl methacrylate plate; and finally carrying out heat treatment to obtain the polymethyl methacrylate plate with large thickness. The invention has the characteristics of high light transmittance, high hardness, good compression resistance and the like, and is very suitable for a submarine observation window and a submarine sightseeing boat.)
1. The formula of the large-thickness polymethyl methacrylate plate is characterized by comprising the following components in percentage by weight:
90.0% -98.0% of methyl methacrylate;
0.01% -0.5% of an initiator;
1% -5% of an anti-ultraviolet agent;
0.5% -5% of additive; and
0.01% -0.5% of toner.
2. The formulation of a high-thickness polymethylmethacrylate sheet according to claim 1, wherein the initiator is one or more of tert-butyl peroxyneodecanoate, dibenzoyl peroxide, dibutyl peroxydicarbonate, tert-butyl peroxy2-ethylhexanoate, and tert-butyl peroxyacetate.
3. The formulation of a large-thickness polymethylmethacrylate sheet according to claim 1, wherein the anti-ultraviolet agent is one or more of UV-P, UV-O, UV-9, UV-327 and Tinuvin P.
4. The formulation of a large-thickness polymethylmethacrylate sheet according to claim 1, wherein the additive is one or more of neopentyl glycol, neopentyl glycol dimethacrylate and sodium docusate.
5. The formulation of a high-thickness polymethylmethacrylate sheet according to claim 1, wherein the toner is one or both of solvent violet and solvent green.
6. A synthetic method of a large-thickness polymethyl methacrylate plate is used for synthesizing the large-thickness polymethyl methacrylate plate, and is characterized by comprising the following steps:
mixing 90.0-98.0 wt% of methyl methacrylate, 0.01-0.5 wt% of initiator, 1-5 wt% of anti-ultraviolet agent and 0.01-0.5 wt% of toner together, and heating and stirring under vacuum condition to react to form reaction liquid;
cooling the reaction liquid, and adding 0.5-5 wt% of additive into the reaction liquid to form a pre-reaction liquid;
pouring the pre-reaction liquid into a mold, heating the mold, preserving heat, and curing the pre-reaction liquid;
repeating the steps until the height of the solidified pre-reaction liquid in the mould reaches the thickness of the large-thickness polymethyl methacrylate plate to be prepared; and
and finally, carrying out heat treatment to obtain the large-thickness polymethyl methacrylate plate.
7. The method for synthesizing a large-thickness polymethyl methacrylate plate according to claim 6, wherein the initiator is one or more of tert-butyl peroxyneodecanoate, dibenzoyl peroxide, dibutyl peroxydicarbonate, tert-butyl peroxy2-ethylhexanoate and tert-butyl peroxyacetate; the uvioresistant agent is one or more of UV-P, UV-O, UV-9, UV-327 and Tinuvin P; the additive is one or more of neopentyl glycol, neopentyl glycol dimethacrylate and sodium docusate; the toner is one or two of solvent purple and solvent green.
8. The method for synthesizing the large-thickness polymethyl methacrylate plate according to claim 6, wherein the reaction solution is cooled by water cooling, and the temperature of the water cooling is 5-10 ℃.
9. The method for synthesizing the large-thickness polymethyl methacrylate plate according to claim 6, wherein the temperature of the mold is heated to 45 ℃, and the holding time is 24 hours.
10. The method for synthesizing a large-thickness polymethylmethacrylate sheet according to claim 6, wherein the final heat treatment method further comprises the steps of:
heating the mould to 60 ℃, and preserving heat for 4 hours;
heating the mould again to 80 ℃, and preserving the heat for 4 hours;
finally heating the mould to 120 ℃, and preserving the heat for 4 hours; and
and cooling to room temperature.
Technical Field
The invention relates to a polymethyl methacrylate plate, in particular to a formula and a synthetic method of a large-thickness polymethyl methacrylate plate.
Background
The sea is closely related to the life of human beings, and since the twenty-first century, the activities of exploring the sea and developing sea resources are developed in all countries in the world. The deep-sea submersible is an indispensable important carrying operation device entering deep sea, and the observation window is equivalent to the eyes of the deep-sea submersible and has the function of lifting the feet.
In the process of implementing the invention, the inventor finds that the prior art has at least the following problems:
Disclosure of Invention
In order to solve the technical problems in the prior art, the embodiment of the invention provides a formula and a synthetic method of a large-thickness polymethyl methacrylate plate. The specific technical scheme is as follows:
in a first aspect, a formula of a large-thickness polymethyl methacrylate plate is provided, and the formula of the large-thickness polymethyl methacrylate plate comprises the following components in percentage by weight:
90.0% -98.0% of methyl methacrylate;
0.01% -0.5% of an initiator;
1% -5% of an anti-ultraviolet agent;
0.5% -5% of additive; and
0.01% -0.5% of toner.
In a first possible implementation of the first aspect, the initiator is one or more of tert-butyl peroxyneodecanoate, dibenzoyl peroxide, dibutyl peroxydicarbonate, tert-butyl peroxy2-ethylhexanoate, tert-butyl peroxyacetate.
In a second possible implementation of the first aspect, the anti-ultraviolet agent is one or more of UV-P, UV-O, UV-9, UV-327, and Tinuvin P.
In a third possible implementation of the first aspect, the additive is one or more of neopentyl glycol, neopentyl glycol dimethacrylate and sodium docusate.
In a fourth possible implementation of the first aspect, the toner is one or both of solvent violet and solvent green.
In a second aspect, a method for synthesizing a large-thickness polymethyl methacrylate plate is provided, which is used for synthesizing the large-thickness polymethyl methacrylate plate, wherein the method for synthesizing the large-thickness polymethyl methacrylate plate comprises the following steps:
mixing 90.0-98.0 wt% of methyl methacrylate, 0.01-0.5 wt% of initiator, 1-5 wt% of anti-ultraviolet agent and 0.01-0.5 wt% of toner together, and heating and stirring under vacuum condition to react to form reaction liquid;
cooling the reaction liquid, and adding 0.5-5 wt% of additive into the reaction liquid to form a pre-reaction liquid;
pouring the pre-reaction liquid into a mold, heating the mold, preserving heat, and curing the pre-reaction liquid;
repeating the steps until the height of the solidified pre-reaction liquid in the mould reaches the thickness of the prepared large-thickness polymethyl methacrylate plate; and
finally, carrying out heat treatment to obtain the polymethyl methacrylate plate with large thickness.
In a first possible implementation of the second aspect, the initiator is one or more of tert-butyl peroxyneodecanoate, dibenzoyl peroxide, dibutyl peroxydicarbonate, tert-butyl peroxy2-ethylhexanoate, tert-butyl peroxyacetate; the uvioresistant agent is one or more of UV-P, UV-O, UV-9, UV-327 and TinuvinP; the additive is one or more of neopentyl glycol, neopentyl glycol dimethacrylate and sodium docusate; the toner is one or two of solvent purple and solvent green.
In a second possible implementation manner of the second aspect, the reaction solution is cooled by water cooling, and the temperature of the water cooling is 5-10 ℃.
In a third possible implementation of the second aspect, the temperature of the mold is heated to 45 degrees celsius for a period of 24 hours.
In a fourth possible implementation manner of the second aspect, the method of final heat treatment further comprises the following steps:
heating the mould to 60 ℃, and keeping the temperature for 4 hours;
heating the mold again to 80 ℃, and preserving the heat for 4 hours;
finally heating the mould to 120 ℃, and preserving the heat for 4 hours; and
and cooling to room temperature.
Compared with the prior art, the invention has the advantages that:
the large-thickness polymethyl methacrylate plate prepared by the formula and the synthesis method of the large-thickness polymethyl methacrylate plate has the characteristics of high light transmittance, high hardness, good compression resistance and the like, and is very suitable for observation windows of submersibles and submarine sightseeing ships.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart of the steps of a method for synthesizing a large-thickness polymethyl methacrylate sheet according to one, two or three embodiments of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
In one embodiment of the invention, the following components are weighed according to the weight percentage of the formula: 92% of methyl methacrylate, 0.03% of tert-butyl peroxyneodecanoate, 4% of UV-P, 3.96% of sodium docusate and 0.01% of solvent violet.
Referring to fig. 1, a schematic flow chart of steps of a
Specifically, methyl methacrylate, tert-butyl peroxyneodecanoate, an anti-ultraviolet agent UV-P and a solvent violet are added into a reaction kettle to form a mixed solution, and the mixed solution is vacuumized, wherein the vacuum degree is preferably-0.08-0.1 MPa, and can be, for example, 0.08, -0.05, -0.02 or 0.1MPa, but not limited thereto. The mixture is heated and stirred, preferably at 90 ℃ for 1 hour, to form a reaction solution by thorough mixing and reaction, but not limited thereto.
Specifically, since the chemical reaction generated in the process of forming the reaction solution generates heat and the temperature of the reaction solution is higher than the temperature of the reaction solution during heating and stirring, whether or not the reaction solution is sufficiently reacted can be determined by measuring the temperature of the reaction solution. In this embodiment, since the temperature of heating and stirring is 90 ℃, when the temperature of the reaction solution in the reaction kettle is close to 105 ℃, it can be judged that the reaction is sufficient, and then the reaction solution is transferred into another reaction kettle, which is jacketed with cooling water, preferably at 5-10 ℃, for example, 5, 7, 8 or 10 ℃, and then the additive sodium docusate is added to react with the reaction solution to form a pre-reaction solution, but not limited thereto.
And 103, pouring for the first time. Pouring the pre-reaction liquid into a mould, heating the mould, preserving heat and solidifying the pre-reaction liquid.
Specifically, after the pre-reaction solution is cooled to 40 ℃, the pre-reaction solution is poured into a mold, the mold is heated to 45 ℃, and the temperature is maintained, wherein the temperature maintaining time is preferably 24 hours, so as to solidify the pre-reaction solution, but not limited thereto.
And
Specifically, since the thickness of the polymethyl methacrylate plate with the large thickness to be prepared cannot be achieved by the conventional one-time casting, the above-mentioned step 101-104 is repeated to perform multiple times of casting until the thickness of the polymethyl methacrylate plate with the large thickness to be prepared is achieved, for example, the thickness of the polymethyl methacrylate plate with the large thickness to be prepared is 100mm, and the height of the pre-reaction liquid solidified by each casting is 20mm, and then the casting is performed for 5 times, so that the height of the pre-reaction liquid solidified in the mold is achieved to the thickness of the polymethyl methacrylate plate with the large thickness to be prepared, that is, 100mm, but not limited thereto.
And 105, finally carrying out heat treatment. Finally, carrying out heat treatment to obtain the polymethyl methacrylate plate with large thickness.
Specifically, heating the mold to 60 ℃, preserving heat for 4 hours, heating the mold again to 80 ℃, preserving heat for 4 hours, finally heating the mold to 120 ℃, preserving heat for 4 hours, and naturally cooling to room temperature to obtain the large-thickness polymethyl methacrylate plate.
In the second embodiment of the invention, the components are weighed according to the weight percentage of the formula: 92% of methyl methacrylate, 0.04% of dibenzoyl peroxide, 4% of an anti-ultraviolet agent UV-9, 1.94% of neopentyl glycol dimethacrylate and 0.02% of solvent violet.
Referring to fig. 1, a schematic flow chart of steps of a
Specifically, methyl methacrylate, dibenzoyl peroxide, UV-9 as an anti-ultraviolet agent and solvent violet are added into a reaction kettle to form a mixed solution, and the mixed solution is vacuumized, wherein the vacuum degree is preferably-0.08-0.1 MPa, and can be, for example, 0.08, -0.05, -0.02 or 0.1MPa, but not limited thereto. The mixture is heated and stirred at a temperature of preferably 80 ℃ for preferably 1.5 hours to allow sufficient mixing and reaction to form a reaction solution, but the temperature is not limited thereto.
Specifically, since the chemical reaction generated in the process of forming the reaction solution generates heat and the temperature of the reaction solution is higher than the temperature of the reaction solution during heating and stirring, whether or not the reaction solution is sufficiently reacted can be determined by measuring the temperature of the reaction solution. In this embodiment, since the temperature of heating and stirring is 80 ℃, when the temperature of the reaction solution in the reaction kettle is close to 100 ℃, it can be judged that the reaction is sufficient, and then the reaction solution is transferred into another reaction kettle, the other reaction kettle is jacketed with cooling water, the temperature is preferably 5-10 ℃, for example, 5, 7, 8 or 10 ℃, and the additive neopentyl glycol dimethacrylate is added to react with the reaction solution to form a pre-reaction solution, but not limited thereto.
And 103, pouring for the first time. Pouring the pre-reaction liquid into a mould, heating the mould, preserving heat and solidifying the pre-reaction liquid.
Specifically, after the pre-reaction solution is cooled to 35 ℃, the pre-reaction solution is poured into a mold, the mold is heated to 45 ℃, and the temperature is maintained, wherein the temperature maintaining time is preferably 24 hours, so as to solidify the pre-reaction solution, but not limited thereto.
And step 104, repeating pouring. And (4) repeating the step 101-104 until the height of the pre-reaction liquid solidified in the mold reaches the thickness of the large-thickness polymethyl methacrylate plate to be prepared.
Specifically, since the thickness of the polymethyl methacrylate plate with the large thickness to be prepared cannot be achieved by the conventional one-time casting, the above-mentioned step 101-104 is repeated to perform multiple times of casting until the thickness of the polymethyl methacrylate plate with the large thickness to be prepared is achieved, for example, the thickness of the polymethyl methacrylate plate with the large thickness to be prepared is 100mm, and the height of the pre-reaction liquid solidified by each casting is 20mm, and then the casting is performed for 5 times, so that the height of the pre-reaction liquid solidified in the mold is achieved to the thickness of the polymethyl methacrylate plate with the large thickness to be prepared, that is, 100mm, but not limited thereto.
And 105, finally carrying out heat treatment. Finally, carrying out heat treatment to obtain the polymethyl methacrylate plate with large thickness.
Specifically, heating the mold to 60 ℃, preserving heat for 4 hours, heating the mold again to 80 ℃, preserving heat for 4 hours, finally heating the mold to 120 ℃, preserving heat for 4 hours, and naturally cooling to room temperature to obtain the large-thickness polymethyl methacrylate plate.
In the three embodiments of the invention, the following components are weighed according to the weight percentage of the formula: 97% of methyl methacrylate, 0.06% of tert-butyl peroxy (2-ethylhexanoate), 2% of an anti-ultraviolet agent UV-327, 0.91% of neopentyl glycol dimethacrylate and 0.03% of solvent violet.
Referring to fig. 1, a schematic flow chart of steps of a
Specifically, methyl methacrylate, tert-butyl peroxy (2-ethylhexanoate), UV-327 anti-ultraviolet agent and purple solvent are added into a reaction kettle to form a mixed solution, and the mixed solution is vacuumized, wherein the vacuum degree is preferably-0.08-0.1 MPa, and can be, for example, 0.08, -0.05, -0.02 or 0.1MPa, but the vacuum degree is not limited to the above. The mixture is heated and stirred at a temperature of preferably 80 ℃ for preferably 1.5 hours to allow sufficient mixing and reaction to form a reaction solution, but the temperature is not limited thereto.
Specifically, since the chemical reaction generated in the process of forming the reaction solution generates heat and the temperature of the reaction solution is higher than the temperature of the reaction solution during heating and stirring, whether or not the reaction solution is sufficiently reacted can be determined by measuring the temperature of the reaction solution. In this embodiment, since the temperature of heating and stirring is 80 ℃, when the temperature of the reaction solution in the reaction kettle is close to 95 ℃, it can be judged that the reaction is sufficient, and then the reaction solution is transferred into another reaction kettle, the other reaction kettle is jacketed with cooling water, the temperature is preferably 5-10 ℃, for example, 5, 7, 8 or 10 ℃, and the additive neopentyl glycol dimethacrylate is added to react with the reaction solution to form a pre-reaction solution, but not limited thereto.
And 103, pouring for the first time. Pouring the pre-reaction liquid into a mould, heating the mould, preserving heat and solidifying the pre-reaction liquid.
Specifically, after the pre-reaction solution is cooled to 35 ℃, the pre-reaction solution is poured into a mold, the mold is heated to 45 ℃, and the temperature is maintained, wherein the temperature maintaining time is preferably 24 hours, so as to solidify the pre-reaction solution, but not limited thereto.
And step 104, repeating pouring. And (4) repeating the step 101-104 until the height of the pre-reaction liquid solidified in the mold reaches the thickness of the large-thickness polymethyl methacrylate plate to be prepared.
Specifically, since the thickness of the polymethyl methacrylate plate with the large thickness to be prepared cannot be achieved by the conventional one-time casting, the above-mentioned step 101-104 is repeated to perform multiple times of casting until the thickness of the polymethyl methacrylate plate with the large thickness to be prepared is achieved, for example, the thickness of the polymethyl methacrylate plate with the large thickness to be prepared is 100mm, and the height of the pre-reaction liquid solidified by each casting is 20mm, and then the casting is performed for 5 times, so that the height of the pre-reaction liquid solidified in the mold is achieved to the thickness of the polymethyl methacrylate plate with the large thickness to be prepared, that is, 100mm, but not limited thereto.
And 105, finally carrying out heat treatment. Finally, carrying out heat treatment to obtain the polymethyl methacrylate plate with large thickness.
Specifically, heating the mold to 60 ℃, preserving heat for 4 hours, heating the mold again to 80 ℃, preserving heat for 4 hours, finally heating the mold to 120 ℃, preserving heat for 4 hours, and naturally cooling to room temperature to obtain the large-thickness polymethyl methacrylate plate.
The large-thickness polymethyl methacrylate plate prepared in the above one to three examples was divided into three groups for testing, and each group of test items included tensile strength, tensile elongation at break, tensile modulus, flexural strength, water absorption, compressive yield strength, and compressive yield modulus.
A first group: the test object is a polymethyl methacrylate plate with large thickness prepared in one embodiment, and the test results are as follows:
second group: the test object is a large-thickness polymethyl methacrylate plate prepared in the two examples, and the test results are as follows:
third group: the test object is a large-thickness polymethyl methacrylate plate prepared in the three examples, and the test results are as follows:
the standard requirements of the plates of the observation window of the deep sea water vehicle in the prior art are as follows:
by combining the first to third groups of test data and the standard requirements of the prior art, the material performance of the large-thickness polymethyl methacrylate plate prepared by the
The foregoing description shows and describes several preferred embodiments of the invention, but as aforementioned, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
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