CN115838555B - Modified polymethyl methacrylate coating for organic glass and preparation and use methods thereof - Google Patents
Modified polymethyl methacrylate coating for organic glass and preparation and use methods thereof Download PDFInfo
- Publication number
- CN115838555B CN115838555B CN202211278457.XA CN202211278457A CN115838555B CN 115838555 B CN115838555 B CN 115838555B CN 202211278457 A CN202211278457 A CN 202211278457A CN 115838555 B CN115838555 B CN 115838555B
- Authority
- CN
- China
- Prior art keywords
- polymethyl methacrylate
- coating
- organic glass
- modified polymethyl
- butyl acetate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920003229 poly(methyl methacrylate) Polymers 0.000 title claims abstract description 62
- 239000004926 polymethyl methacrylate Substances 0.000 title claims abstract description 62
- 239000011248 coating agent Substances 0.000 title claims abstract description 46
- 238000000576 coating method Methods 0.000 title claims abstract description 46
- 239000011521 glass Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 41
- 229920005989 resin Polymers 0.000 claims abstract description 41
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 26
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 26
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 22
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 15
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004342 Benzoyl peroxide Substances 0.000 claims abstract description 12
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 12
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 11
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims description 25
- 238000001816 cooling Methods 0.000 claims description 16
- 238000001723 curing Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- LBTSNEJGMVFUEW-UHFFFAOYSA-N 2,2,3,3,4,4,5,5,6,8,8,8-dodecafluorooctoxy-dimethoxy-propylsilane Chemical compound FC(C(C(C(C(F)(F)CO[Si](OC)(OC)CCC)(F)F)(F)F)(F)F)CC(F)(F)F LBTSNEJGMVFUEW-UHFFFAOYSA-N 0.000 claims description 10
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 10
- 229910052731 fluorine Inorganic materials 0.000 claims description 10
- 239000011737 fluorine Substances 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- WNPVSRSMIAXYIZ-UHFFFAOYSA-N 8-fluorohenicosan-8-ol Chemical compound CCCCCCCCCCCCCC(O)(F)CCCCCCC WNPVSRSMIAXYIZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000013007 heat curing Methods 0.000 claims description 6
- 238000009423 ventilation Methods 0.000 claims description 6
- 238000007334 copolymerization reaction Methods 0.000 claims description 5
- 238000007766 curtain coating Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 15
- 230000001070 adhesive effect Effects 0.000 abstract description 15
- 239000006227 byproduct Substances 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 239000003973 paint Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 10
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 8
- 230000002194 synthesizing effect Effects 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920005372 Plexiglas® Polymers 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a modified polymethyl methacrylate coating for organic glass and a preparation and use method thereof, wherein the coating consists of modified polymethyl methacrylate resin, an N75 curing agent and butyl acetate, wherein the modified polymethyl methacrylate resin consists of a high-fluorine-content intermediate, methyl methacrylate, styrene, glycidyl methacrylate, methacrylic acid, butyl acrylate, butyl acetate, benzoyl peroxide and a molecular weight regulator DK-08; the polymethyl methacrylate coating with strong adhesive force, high hydrophobicity and high stain resistance for the organic glass prepared by the invention has stronger adhesive force, high hydrophobicity and high stain resistance when being coated on an organic glass substrate, greatly expands the application field of the polymethyl methacrylate coating, has simple preparation process and does not have toxic or side products.
Description
Technical Field
The invention relates to the field of protective coatings, in particular to a modified polymethyl methacrylate coating for organic glass and a preparation and application method thereof.
Background
Polymethyl methacrylate is widely used as coating resin in the industries of buildings, electric appliances, automobiles and the like, but the adhesion effect of the polymethyl methacrylate coating and the surface of organic glass is poor, a paint film is easy to fall off and is easy to be polluted by various stains, and the hydrophobicity is poor. There is therefore a need to develop a polymethyl methacrylate coating which can be applied to a plexiglass substrate with strong adhesion, hydrophobicity and stain resistance.
The main method for solving the problem at present is to try to increase the molecular weight of the resin, but the viscosity is higher due to the higher molecular weight, the resin is easy to gel at a rapid temperature in the preparation process, and the pigment and filler are difficult to uniformly disperse in a macromolecular resin skeleton structure, so that flocculation or gel formation is easy to occur in the storage and transportation processes. And adding surface auxiliary agents to the paint, but this method affects the overall performance of the paint.
Disclosure of Invention
The modified polymethyl methacrylate coating for the organic glass has strong adhesive force, hydrophobicity and stain resistance when being coated on an organic glass substrate, greatly expands the application field of the polymethyl methacrylate coating, and has the advantages of simple preparation process and no toxic or side product.
The invention provides a modified polymethyl methacrylate coating for organic glass, which comprises the following components in percentage by mass:
30 to 60 percent of modified polymethyl methacrylate resin
10 to 40 percent of N75 curing agent
Butyl acetate 20-40%
The modified polymethyl methacrylate resin comprises the following components in percentage by mass:
the preparation method of the modified polymethyl methacrylate resin comprises the following steps:
firstly, taking 20% of high-fluorine-content intermediate, 20% of methyl methacrylate, 20% of styrene, 20% of glycidyl methacrylate, 20% of methacrylic acid, 20% of butyl acrylate and 50% of butyl acetate, and adding the mixture into a kettle, heating and stirring until reflux; after the system is refluxed for 30min, a mixture composed of 80% of high-fluorine-content intermediate, 80% of methyl methacrylate, 80% of styrene, 80% of methacrylic acid, 80% of butyl acrylate, 25% of butyl acetate, 70% of glycidyl methacrylate, 70% of benzoyl peroxide and 70% of molecular weight regulator DK-08 is added dropwise, the dripping speed is uniform, the dripping time is 60-90 min, and the reflux is kept in the dripping process; after the dropwise addition is completed and the system is kept to reflux for 120min, 25% of butyl acetate, 10% of glycidyl methacrylate, 30% of benzoyl peroxide and 30% of molecular weight regulator DK-08 are fully and uniformly mixed and dropwise added, the dropwise addition time is within 30min, and the reflux is kept in the dropwise addition process; and after the dropwise adding is finished, introducing nitrogen into the system, continuously maintaining reflux copolymerization for 180-240 min, and then cooling and discharging to obtain colorless transparent clear resin and modified polymethyl methacrylate resin.
Further, the high fluorine content intermediate consists of the following components in percentage by mass:
the preparation method of the high-fluorine-content intermediate comprises the following steps: adding 20% of dodecafluoroheptyl propyl trimethoxysilane, 20% of tridecyl fluorooctanol and 20% of hydroxyethyl acrylate into the mixture, stirring and preserving the temperature at 55-65 ℃; after the system is kept warm for 30min, dropwise adding a mixed solution which is prepared by uniformly mixing 80% of dodecafluoroheptyl propyl trimethoxy silane, 80% of tridecyl fluorooctanol, 80% of hydroxyethyl acrylate and all concentrated sulfuric acid at the temperature of 55-65 ℃ within 30 min; and after the dripping is finished, preserving the heat for 60min, then cooling to below 10 ℃, starting heating, decompressing and pumping to the system of 60 ℃ by using a vacuum pump, stopping pumping, cooling and discharging to obtain the intermediate with high fluorine content.
The second aspect provides a preparation method of the modified polymethyl methacrylate coating for the organic glass, which comprises the following steps:
weighing the modified polymethyl methacrylate resin, the N75 curing agent and the butyl acetate according to the proportion, adding the modified polymethyl methacrylate resin, the N75 curing agent and the butyl acetate into a beaker, and stirring and mixing the materials uniformly under the environment of normal temperature and normal pressure to obtain the coating.
The third aspect provides a method for using the modified methyl methacrylate coating for the organic glass, which comprises the following steps: a proper amount of high-adhesion hydrophobic stain-resistant polymethyl methacrylate coating for organic glass is firstly uniformly sprayed or shower-coated on the surface of an organic glass substrate by using a spray gun, the coating amount is determined according to actual use conditions, then the object is placed under normal temperature and normal pressure ventilation conditions for standing for 1 hour until the surface is dry, and then the object is placed in a 70 ℃ environment for further heat curing, wherein the curing time is more than or equal to 1 hour, so that the optimal curing effect is achieved.
The beneficial effects of the invention are as follows:
compared with the traditional polymethyl methacrylate resin coating, the coating resin prepared by the invention has the advantages that the temperature change range is relatively fixed during synthesis, the reaction environment condition is not required to be high, the system is stable, and the explosion polymerization and the gelation are not easy to occur; the experimental instrument required by the synthesis process is simple and common, the resin in the system is fully reacted, and no obvious toxic or harmful byproducts are generated; the obtained resin is colorless and transparent, and the prepared paint is coated on an organic glass substrate, so that the paint has excellent adhesive force, hydrophobicity and stain resistance which are not possessed by the traditional polymethyl methacrylate resin paint, the defects of the adhesive force, hydrophobicity and stain resistance of the polymethyl methacrylate resin paint on the organic glass substrate are greatly overcome, the paint is suitable for more complex environmental conditions, and the application space of the polymethyl methacrylate resin paint on the substrate is expanded.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, based on the examples herein, which are within the scope of the invention, will be within the purview of one of ordinary skill in the art without the exercise of inventive faculty.
Embodiment one:
synthesizing an intermediate with high fluorine content: putting 14g of dodecafluoroheptyl propyl trimethoxysilane, 4g of trideoxyfluoro octanol and 1.6g of hydroxyethyl acrylate into a reaction kettle, stirring and controlling the temperature at 60 ℃; after the system is kept warm for 30min, a mixed solution which is prepared by uniformly mixing the rest 56g of dodecafluoroheptyl propyl trimethoxysilane, 16g of trideoxyfluoro octanol, 6.4g of hydroxyethyl acrylate and all 2g of concentrated sulfuric acid is dripped at 60 ℃ for 30min, and then the dripping is completed; and (3) after heat preservation for 60min, cooling to 8 ℃, then starting to heat, and reducing the pressure by using a vacuum pump to extract until the temperature of the system is 60 ℃, stopping extracting, cooling and discharging to obtain the intermediate 1 with high fluorine content.
Synthesizing modified polymethyl methacrylate resin: firstly, adding 0.4g of high-fluorine-content intermediate 1, 4g of methyl methacrylate, 4g of styrene, 0.4g of glycidyl methacrylate, 0.2g of methacrylic acid, 3g of butyl acrylate and 18g of butyl acetate into a kettle, heating and stirring until reflux; after the system is refluxed for 30min, a uniform mixture composed of 1.6g of intermediate with high fluorine content 1, 16g of methyl methacrylate, 16g of styrene, 0.8g of methacrylic acid, 12g of butyl acrylate, 9g of butyl acetate, 1.4g of glycidyl methacrylate, 1.4g of benzoyl peroxide and 1.4g of DK-08 is started to be dripped for 60min, and reflux is maintained during the dripping process; after the system is kept to reflux for 120min, the rest 9g of butyl acetate, 0.2g of glycidyl methacrylate, 0.6g of benzoyl peroxide and 0.6g of DK-08 are fully and uniformly mixed and dropwise added, after 30min of dropwise adding, the reflux is continuously kept, nitrogen is introduced into the system and the reflux copolymerization is continuously kept for 180min, and then the material is cooled and discharged, so that the colorless transparent clear modified polymethyl methacrylate resin 1 is obtained.
Preparing the polymethyl methacrylate coating with strong adhesive force, strong hydrophobicity and stain resistance for the organic glass: 30g of modified polymethyl methacrylate resin 1 and 5g of N75 curing agent are stirred and mixed uniformly under the environment of normal temperature and normal pressure, and the polymethyl methacrylate coating 1 with strong adhesive force, strong hydrophobicity and stain resistance for organic glass is obtained.
And (3) performing a curtain coating test on the organic glass plate by using the prepared polymethyl methacrylate coating with strong adhesive force, strong hydrophobicity and stain resistance. And (3) taking 50g of organic glass, coating the organic glass substrate surface with the high-adhesion high-hydrophobicity stain-resistant polymethyl methacrylate coating once, standing the sample plate for 1 hour under the normal temperature and normal pressure ventilation condition, putting the sample plate into a 70 ℃ oven for further heat curing for 2 hours, taking out the sample plate, cooling to room temperature, and then measuring.
Embodiment two:
synthesizing an intermediate with high fluorine content: 12g of dodecafluoroheptyl propyl trimethoxy silane, 4g of tridecyl fluorooctanol and 3.6g of hydroxyethyl acrylate are put into a reaction kettle to be stirred and controlled at 60 ℃; after the system is kept warm for 30min, the temperature is controlled at 60 ℃, and a mixed solution which is prepared by uniformly mixing 48g of dodecafluoroheptyl propyl trimethoxysilane, 16g of trideoxyfluoro octanol, 14.4g of hydroxyethyl acrylate and all 2g of concentrated sulfuric acid is started to be added dropwise, and after 30min, the dropwise addition is completed; and (3) after heat preservation for 60min, cooling to 6 ℃, then starting to heat, and reducing the pressure by using a vacuum pump to extract until the temperature of the system is 60 ℃, stopping extracting, cooling and discharging to obtain the intermediate 1 with high fluorine content.
Synthesizing modified polymethyl methacrylate resin: firstly, adding 0.6g of high-fluorine-content intermediate, 9g of methyl methacrylate, 3g of styrene, 0.6g of glycidyl methacrylate, 0.3g of methacrylic acid, 4.5g of butyl acrylate and 27g of butyl acetate into a kettle, heating and stirring until reflux; after the system is refluxed for 30min, a uniform mixture composed of 2.4g of high-fluorine-content intermediate, 36g of methyl methacrylate, 12g of styrene, 1.2g of methacrylic acid, 18g of butyl acrylate, 13.5g of butyl acetate, 2.1g of glycidyl methacrylate, 2.1g of benzoyl peroxide and 2.1g of DK-08 is started to be dripped for 90min, and the reflux is maintained during the dripping process; after the system is kept to reflux for 120min, the rest 13.5g of butyl acetate, 0.3g of glycidyl methacrylate, 0.9g of benzoyl peroxide and 0.9g of DK-08 are fully and uniformly mixed and dropwise added, after 30min of dropwise adding, the reflux is continuously kept, nitrogen is introduced into the system and the reflux copolymerization is continuously kept for 180min, and then the material is cooled and discharged, so that the colorless transparent clear modified polymethyl methacrylate resin 2 is obtained.
Preparing the polymethyl methacrylate coating with strong adhesive force, strong hydrophobicity and stain resistance for the organic glass: 25g of modified polymethyl methacrylate resin 3 and 15g of N75 curing agent and 10g of butyl acetate are stirred and mixed uniformly under the environment of normal temperature and normal pressure to obtain the high-adhesion high-hydrophobicity stain-resistant polymethyl methacrylate coating for the organic glass.
And spraying the prepared polymethyl methacrylate coating with strong adhesive force, high hydrophobicity and stain resistance for the organic glass to test the organic glass plate. And (3) spraying 60g of organic glass onto the surface of an organic glass substrate by using a high-adhesion high-hydrophobicity stain-resistant polymethyl methacrylate coating, standing the sample plate for 1 hour under normal temperature and normal pressure ventilation, putting the sample plate into a 70 ℃ oven for further heat curing for 3 hours, taking out the sample plate, cooling to room temperature, and then measuring. .
Embodiment III:
synthesizing an intermediate with high fluorine content: 12g of dodecafluoroheptyl propyl trimethoxy silane, 7.6g of tridecyl fluorooctanol and 0.4g of hydroxyethyl acrylate are taken to be put into a reaction kettle, and the stirring temperature is controlled to be 60 ℃; after the system is kept warm for 30min, the temperature is controlled at 60 ℃, and a mixed solution which is prepared by uniformly mixing 48g of dodecafluoroheptyl propyl trimethoxy silane, 30.4g of trideoxyfluoro octanol, 1.6g of hydroxyethyl acrylate and all 2g of concentrated sulfuric acid is started to be added dropwise, and after 30min, the dropwise addition is completed; and (3) after heat preservation for 60min, cooling to 4 ℃, then starting to heat and decompressing to extract to 60 ℃, stopping cooling and discharging to obtain the intermediate 3 with high fluorine content.
Synthesizing modified polymethyl methacrylate resin: firstly, adding 0.2g of high-fluorine-content intermediate, 4g of methyl methacrylate, 4g of styrene, 0.2g of glycidyl methacrylate, 0.2g of methacrylic acid, 3g of butyl acrylate and 20g of butyl acetate into a kettle, heating and stirring until reflux; after the system is refluxed for 30min, a uniform mixture composed of 0.8g of high-fluorine-content intermediate, 16g of methyl methacrylate, 16g of styrene, 0.8g of methacrylic acid, 12g of butyl acrylate, 10g of butyl acetate, 0.7g of glycidyl methacrylate, 0.7g of benzoyl peroxide and 0.7g of DK-08 is started to be dripped for 90min, and reflux is maintained during the dripping process; after the system is kept to reflux for 120min, the rest 10g of butyl acetate, 0.1g of glycidyl methacrylate, 0.3g of benzoyl peroxide and 0.3g of DK-08 are fully and uniformly mixed and dropwise added, after 30min of dropwise adding, the reflux is continuously kept, nitrogen is introduced into the system and the reflux copolymerization is continuously kept for 180min, and then the material is cooled and discharged, so that the colorless transparent clear modified polymethyl methacrylate resin 3 is obtained.
Preparing the polymethyl methacrylate coating with strong adhesive force, strong hydrophobicity and stain resistance for the organic glass: 30g of modified polymethyl methacrylate resin 3 and 30g of N75 curing agent, 40g of butyl acetate are stirred and mixed uniformly under the environment of normal temperature and normal pressure to obtain the high-adhesion high-hydrophobicity stain-resistant polymethyl methacrylate coating for the organic glass.
And (3) performing a curtain coating test on the organic glass plate by using the prepared polymethyl methacrylate coating with strong adhesive force, strong hydrophobicity and stain resistance. 100g of organic glass is coated on the surface of an organic glass substrate by using a high-adhesion high-hydrophobicity stain-resistant polymethyl methacrylate coating once, then a sample plate is placed under the normal temperature and normal pressure ventilation condition for 1 hour, and then the sample plate is placed into a 70 ℃ oven for further heat curing for 2 hours, and then the sample plate is taken out and cooled to the room temperature for testing.
Comparative example 1
Synthesizing polymethyl methacrylate resin: 100g of methyl methacrylate and 5g of benzoyl peroxide were weighed and then put into a conical flask with water bath at 90℃and heated and maintained at temperature. The whole reaction process must be monitored all the time to observe whether the initiator is completely decomposed, the system becomes viscous suddenly at an indefinite time, and coking is easily caused by uneven local heating. And cooling and discharging when the whole body is sticky.
Preparing a coating: and uniformly stirring and mixing 30g of resin, 10g of N75 curing agent and 20g of butyl acetate at normal temperature and normal pressure to obtain the coating.
And (3) performing a curtain coating test on the organic glass plate by using the prepared paint. And (3) taking 50g of paint, curtain coating the paint on the surface of the organic glass substrate, standing the sample plate for 3 hours under normal temperature and normal pressure ventilation, putting the sample plate into a T=70 ℃ oven for further heat curing for 3 hours, taking out the sample plate, cooling to room temperature, and then measuring.
Adhesion test reference standard for coating GB/T9286-1998, contact angle with water test reference standard GB/T30693-2014, stain resistance test reference standard GB/T9780-2013.
The test results are shown in Table 1 below:
table 1 test results table
Examples and comparative examples can be seen: the polymethyl methacrylate coating with strong adhesive force, high hydrophobicity and stain resistance for the organic glass prepared by the invention is colorless and transparent, has excellent adhesive force, hydrophobicity and stain resistance which are not possessed by the traditional polymethyl methacrylate resin coating when being coated on an organic glass substrate, and greatly overcomes the defects of adhesive force, hydrophobicity and stain resistance of the polymethyl methacrylate resin coating on the organic glass substrate so as to adapt to more complex environmental conditions and expand the application space of the polymethyl methacrylate resin coating on the substrate.
The present disclosure has been described with respect to the above-described embodiments, however, the above-described embodiments are merely examples of implementation of the present disclosure. It must be noted that the disclosed embodiments do not limit the scope of the present disclosure. Rather, the foregoing is considered to be illustrative, and it is to be understood that the invention is not limited to the specific details disclosed herein.
Claims (3)
1. A modified polymethyl methacrylate coating for organic glass is characterized in that: the weight percentage of the components is calculated according to the mass percentage,
consists of the following components:
30 to 60 percent of modified polymethyl methacrylate resin
10 to 40 percent of N75 curing agent
Butyl acetate 20-40%
The modified polymethyl methacrylate resin comprises the following components in percentage by mass:
the preparation method of the modified polymethyl methacrylate resin comprises the following steps:
firstly, taking 20% of high-fluorine-content intermediate, 20% of methyl methacrylate, 20% of styrene, 20% of glycidyl methacrylate, 20% of methacrylic acid, 20% of butyl acrylate and 50% of butyl acetate, and adding the mixture into a kettle, heating and stirring until reflux; after the system is refluxed for 30min, a mixture composed of 80% of high-fluorine-content intermediate, 80% of methyl methacrylate, 80% of styrene, 80% of methacrylic acid, 80% of butyl acrylate, 25% of butyl acetate, 70% of glycidyl methacrylate, 70% of benzoyl peroxide and 70% of molecular weight regulator DK-08 is added dropwise, the dripping speed is uniform, the dripping time is 60-90 min, and the reflux is kept in the dripping process; after the dropwise addition is completed and the system is kept to reflux for 120min, 25% of butyl acetate, 10% of glycidyl methacrylate, 30% of benzoyl peroxide and 30% of molecular weight regulator DK-08 are fully and uniformly mixed and dropwise added, the dropwise addition time is within 30min, and the reflux is kept in the dropwise addition process; after the dripping is finished, introducing nitrogen into the system, continuously maintaining reflux copolymerization for 180-240 min, and then cooling and discharging to obtain colorless transparent clear resin, namely modified polymethyl methacrylate resin;
the high-fluorine-content intermediate comprises the following components in percentage by mass:
the preparation method of the high-fluorine-content intermediate comprises the following steps: adding 20% of dodecafluoroheptyl propyl trimethoxy silane, 20% of tridecyl fluorooctanol and 20% of hydroxyethyl acrylate into a reaction kettle, stirring and preserving the temperature at 55-65 ℃; after the system is kept warm for 30min, dropwise adding a mixed solution which is prepared by uniformly mixing 80% of dodecafluoroheptyl propyl trimethoxy silane, 80% of tridecyl fluorooctanol, 80% of hydroxyethyl acrylate and all concentrated sulfuric acid at the temperature of 55-65 ℃ within 30 min; and after the dripping is finished, preserving the heat for 60min, then cooling to below 10 ℃, starting heating, decompressing and pumping to the system of 60 ℃ by using a vacuum pump, stopping pumping, cooling and discharging to obtain the intermediate with high fluorine content.
2. The method for preparing the modified polymethyl methacrylate coating for the organic glass of claim 1, which is characterized in that: weighing the modified polymethyl methacrylate resin, the N75 curing agent and the butyl acetate according to the proportion, adding the modified polymethyl methacrylate resin, the N75 curing agent and the butyl acetate into a beaker, and stirring and mixing the materials uniformly under the environment of normal temperature and normal pressure to obtain the coating.
3. The method for using the modified polymethyl methacrylate coating for organic glass of claim 1, which is characterized in that: and taking a proper amount of the modified polymethyl methacrylate coating for the organic glass, uniformly spraying or curtain coating the surface of the organic glass substrate by using a spray gun, wherein the coating amount is determined according to the actual use condition, then placing the object in a normal temperature and normal pressure ventilation condition for standing for 1 hour until the surface of the object is dry, and then placing the object in a 70 ℃ environment for further heat curing, wherein the curing time is more than or equal to 1 hour so as to achieve the optimal curing effect.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211278457.XA CN115838555B (en) | 2022-10-19 | 2022-10-19 | Modified polymethyl methacrylate coating for organic glass and preparation and use methods thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211278457.XA CN115838555B (en) | 2022-10-19 | 2022-10-19 | Modified polymethyl methacrylate coating for organic glass and preparation and use methods thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115838555A CN115838555A (en) | 2023-03-24 |
| CN115838555B true CN115838555B (en) | 2024-01-02 |
Family
ID=85576417
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211278457.XA Active CN115838555B (en) | 2022-10-19 | 2022-10-19 | Modified polymethyl methacrylate coating for organic glass and preparation and use methods thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115838555B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11181027A (en) * | 1997-12-24 | 1999-07-06 | Toagosei Co Ltd | Production of fluorine-containing copolymer |
| CN106280832A (en) * | 2016-08-22 | 2017-01-04 | 西北永新涂料有限公司 | Fluorinated silicone modified hydrophobic soil resistant acrylic resin and containing the varnish of this resin and preparation method |
| CN108485393A (en) * | 2018-04-10 | 2018-09-04 | 深圳市零度智控科技有限公司 | Hydrophobic oleophobic coating |
| CN110105493A (en) * | 2019-05-30 | 2019-08-09 | 江苏中新瑞光学材料有限公司 | The preparation process of the type of resistance to UV hydrophobic material |
| CN110256625A (en) * | 2019-06-13 | 2019-09-20 | 华南理工大学 | Highly filled fluorine-containing hydroxy polyacrylate aqueous dispersion and the preparation method and application thereof |
| CN114163560A (en) * | 2021-12-03 | 2022-03-11 | 中昊北方涂料工业研究设计院有限公司 | Strong-adhesion boiling-resistant coating for synthetic resin and organic glass |
-
2022
- 2022-10-19 CN CN202211278457.XA patent/CN115838555B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11181027A (en) * | 1997-12-24 | 1999-07-06 | Toagosei Co Ltd | Production of fluorine-containing copolymer |
| CN106280832A (en) * | 2016-08-22 | 2017-01-04 | 西北永新涂料有限公司 | Fluorinated silicone modified hydrophobic soil resistant acrylic resin and containing the varnish of this resin and preparation method |
| CN108485393A (en) * | 2018-04-10 | 2018-09-04 | 深圳市零度智控科技有限公司 | Hydrophobic oleophobic coating |
| CN110105493A (en) * | 2019-05-30 | 2019-08-09 | 江苏中新瑞光学材料有限公司 | The preparation process of the type of resistance to UV hydrophobic material |
| CN110256625A (en) * | 2019-06-13 | 2019-09-20 | 华南理工大学 | Highly filled fluorine-containing hydroxy polyacrylate aqueous dispersion and the preparation method and application thereof |
| CN114163560A (en) * | 2021-12-03 | 2022-03-11 | 中昊北方涂料工业研究设计院有限公司 | Strong-adhesion boiling-resistant coating for synthetic resin and organic glass |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115838555A (en) | 2023-03-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107434842B (en) | Core-shell structure hydroxyl acrylic resin emulsion and preparation method and application thereof | |
| CN102504733B (en) | Water-blush-resistant fluoride and siloxane modified waterborne pressure-sensitive adhesive and polyethylene protective film | |
| CN107141425A (en) | A kind of baking vanish aqueous epoxy resins and preparation method and application | |
| CN104341547A (en) | Polyacrylic ester sealing emulsion and preparation method thereof | |
| CN114316854A (en) | Acrylic acid adhesive with high solid content and low viscosity and preparation method thereof | |
| EP3652261A1 (en) | One-part thermal-curing acrylate adhesive precursor and preparation method thereof | |
| CN109180877A (en) | Plastic paint waterborne epoxy modified acrylic resin and preparation method thereof | |
| CN115838555B (en) | Modified polymethyl methacrylate coating for organic glass and preparation and use methods thereof | |
| CN109053952B (en) | Water-based acrylic resin and application thereof | |
| CN110408297A (en) | A kind of aqueous environment protection paint and preparation method thereof | |
| CN102432777B (en) | Method for modifying cellulose acetate butyrate (CAB) for electro-silvered simulating coating | |
| CN105462483B (en) | A kind of dual cure unsaturated polyester (UP) transparent priming | |
| CN112029030A (en) | Water-based acrylic resin for organic silicon modified glass paint and preparation method and application thereof | |
| CN112094369A (en) | Reactive acrylic resin and preparation method and application thereof | |
| CN109957322A (en) | A kind of double cross connection curing anti fogging film and preparation method thereof | |
| CN112011242A (en) | Water-based acrylic resin for coil coating and preparation method and application thereof | |
| CN111944404A (en) | Preparation method of special resin for water-based baking varnish with internal crosslinking function | |
| CN117003933B (en) | Soap-free polymeric cationic dispersion and preparation method thereof | |
| CN111334137B (en) | Waterproof spray, preparation method and application thereof | |
| CN117447887A (en) | Fluorine-silicon modified acrylic resin coating for organic glass and preparation and use methods thereof | |
| CN114085314B (en) | Aluminum baking varnish hydroxy acrylic resin and preparation method and application thereof | |
| CN114276486B (en) | Preparation method and application of fluorine-containing acrylate resin with super-hydrophobic cross-linked structure | |
| CN109321075A (en) | A kind of water-based anticorrosive paint and preparation method thereof | |
| CN109422855A (en) | A kind of line gravure UV gloss oil resin and its preparation method and application | |
| CN110204647B (en) | Tearable film thermoplastic acrylic resin and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |