Preparation method of butyl rubber for edge sealing of photovoltaic module

Abstract

The invention discloses a preparation method of butyl rubber for edge sealing of a photovoltaic module, and belongs to the technical field of adhesives. The preparation method comprises the following steps: putting liquid butyl rubber, polyisobutene and self-made resin into a kneading kettle, stirring and kneading for 1-2 hours at the temperature of 120-130 DEG C, raising the temperature to 160-170 DEG C, then adding a filler and a water absorbent, stirring for 1-2 hours, lowering the temperature to 100-110 DEG C, then adding a catalyst and an adhesive, stirring for 0.5-0.8 hour under the vacuum degree of-0.095-0.011 Mpa, discharging, and finally, cooling to the room temperature to obtain a finished product. The butyl rubber for edge sealing of the photovoltaic module is obtained. The butyl rubber for edge sealing of the photovoltaic module prepared by the invention has excellent flame retardant property and mechanical property.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of adhesives, and particularly relates to a preparation method of butyl glue for edge sealing of photovoltaic modules. BACKGROUND

[0002] Butyl adhesive tape has the advantages of convenient construction and wide temperature tolerance range, and is widely used in photovoltaic, building, automobile, instrument, and resin-based composite material vacuum infusion process caulking sealing and bonding. The butyl adhesive tape is composed of a butyl glue layer, a cover material and a release film, wherein the butyl glue layer is mainly composed of a composite material obtained by blending butyl rubber (IR) additives and fillers, and is prepared by calendering. IR is obtained by copolymerization of isobutene and a small amount of isoprene, and has good thermal stability, moisture resistance and chemical resistance. However, since the limiting oxygen index (LOI) of IR is only 18%, it belongs to flammable materials, which leads to a great safety hazard of butyl adhesive tape in use, thereby limiting the practical application of butyl adhesive tape, and therefore it is of great significance to study the flame-retardant modification of butyl adhesive tape. SUMMARY

[0003] The application aims to provide a preparation method of butyl glue for edge sealing of photovoltaic modules, so as to solve the problems in the prior art.

[0004] In order to solve the above technical problems, the application provides the following technical scheme: A butyl glue for edge sealing of photovoltaic modules comprises the following components by weight: liquid butyl glue 150-300 parts polyisobutene 30-100 parts self-made resin 150-300 parts filler 200-400 parts catalyst 20-50 parts water absorbent 0.5-5 parts adhesive 2-20 parts Preferably, the Mooney viscosity of the liquid butyl glue is controlled at 35-50 Pa·s, and the content of isoprene accounts for 3.5%-5.5% of the content of isobutene. As preferred, the preparation process of the self-made resin is as follows: taking 0.3-0.55 parts of hydroxyethyl methacrylate, 30-40 parts of acetonitrile, 3-5 parts of phenyl phosphonic dichloride, 3-5 parts of triethylamine, 0.01-0.03 parts of 4-dimethylaminopyridine and 3-5 parts of 1,3,5-tris (2-hydroxyethyl) isocyanurate by weight, the phenyl phosphonic dichloride and acetonitrile are added into a reactor, and they are stirred in an ice bath and under nitrogen condition at a rotating speed of 1200-2000 r / min for 30-40 min, then the hydroxyethyl methacrylate and triethylamine mixed solution is added dropwise into the reactor within 3-5 h under the condition of-2-0 ℃, the reaction is continued for 1-2 h under the condition of 0 ℃, then the 4-dimethylaminopyridine and 1,3,5-tris (2-hydroxyethyl) isocyanurate are slowly added into the reactor, the mixture is stirred in an ice bath for 2-3 h, then it is heated to 85-98 ℃ and refluxed for 12-15 h, after the solution is cooled to room temperature, the precipitated triethylamine hydrochloride is removed by filtration, then the filtrate is poured into deionized water with a volume of 5-10 times of the filtrate, and the crude product is obtained by dichloromethane extraction, then the crude product is further washed with deionized water for 5-8 times, then the crude extract is dissolved in dichloromethane and dried with anhydrous magnesium sulfate, finally the dichloromethane is removed by distillation, and the self-made resin is obtained; As preferred, the filler is any one of carbon black or silicon powder; As preferred, the water absorbing agent is vinyl trimethoxysilane; As preferred, the catalyst is any one of diisooctyl dimercaptousccinate dibutyl tin or butyl mercaptan tin; As preferred, the adhesive is any one of silane coupling agent containing epoxy group, silane coupling agent containing methoxy group, silane coupling agent containing amino group or silane oligomer; A preparation method of butyl glue for edge sealing of photovoltaic module, comprising the following steps: The liquid butyl glue, polyisobutylene and self-made resin are placed in a kneading kettle, after stirring and kneading at a temperature of 120-130 ℃ for 1-2 h, the temperature is raised to 160-170 ℃, then the filler and water absorbing agent are added and stirred for 1-2 h, then the temperature is reduced to 100-110 ℃, then the catalyst and adhesive are added, and after stirring under a vacuum degree of-0.095-0.011 Mpa for 0.5-0.8 h, the butyl glue for edge sealing of photovoltaic module is discharged.

[0005] Compared with the prior art, the present application has the following beneficial effects: The application adds self-made resin, in the re-burning process, the inert free radicals generated by pyrolysis of self-made flame retardant capture hydrogen free radicals, oxygen free radicals and hydroxyl radicals, then terminate the free radical chain reaction in the gas phase, the free radicals will also combine with active end groups, thereby avoiding further pyrolysis of chain segments in the condensed phase, and the generated non-combustible gas will dilute the concentration of combustible gas and oxygen in the gas phase, and take away the heat generated by combustion, then weaken the degree of combustion in the gas phase, and further improve the flame retardant performance of the system. DETAILED DESCRIPTION

[0006] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.

[0007] In order to more clearly illustrate the method provided by the application, the following embodiments are described in detail. In the following embodiments, the test methods of various indexes of the rubber-modified molded vinyl ester resin are as follows: Tear resistance: the edge of the photovoltaic module obtained in each example is taken in the same size and shape with the butyl glue and the material of the comparative example, and the tear resistance is determined according to the standard method of ASTM D624.

[0008] Flame retardant performance: the edge of the photovoltaic module obtained in each example is taken in the same size and shape with the butyl glue and the material of the comparative example, and the limiting oxygen index is determined according to the standard method of GB / T2406.

[0009] Example 1 The preparation process of the self-made resin is as follows: taking 0.55 parts of hydroxyethyl methacrylate, 40 parts of acetonitrile, 3 parts of phenyl dichlorophosphate, 5 parts of triethylamine, 0.03 parts of 4-dimethylaminopyridine and 5 parts of 1,3,5-tris(2-hydroxyethyl) isocyanurate by weight, phenyl dichlorophosphate and acetonitrile are added to the reactor, and under the condition of ice bath and nitrogen, the mixture is stirred at a speed of 1200 r / min for 40 min, then the mixture of hydroxyethyl methacrylate and triethylamine is added dropwise into the reactor at-2℃ within 5h, and the reaction is continued at 0℃ for 2h, then 4-dimethylaminopyridine and 1,3,5-tris(2-hydroxyethyl) isocyanurate are slowly added into the reactor, the mixture is stirred in an ice bath for 3h, then heated to 98℃ and refluxed for 12h, after the solution is cooled to room temperature, the precipitated triethylamine hydrochloride is removed by filtration, then the filtrate is poured into deionized water with a volume of 10 times the filtrate, and the crude product is obtained by dichloromethane extraction, then the crude product is further washed with deionized water for 5 times, then the crude extract is dissolved in dichloromethane and dried with anhydrous magnesium sulfate, finally the dichloromethane is removed by distillation, and the self-made resin is obtained; Taking 300 parts of liquid butyl rubber, 30 parts of polyisobutylene, 300 parts of self-made resin, 200 parts of filler, 20 parts of catalyst, 5 parts of water absorbing agent and 10 parts of adhesive by weight, the liquid butyl rubber, polyisobutylene and self-made resin are placed in a kneading kettle, stirred and kneaded at a temperature of 130℃ for 2h, then the temperature is raised to 160℃, then the filler and water absorbing agent are added and stirred for 2h, then the temperature is reduced to 100℃, then the catalyst and adhesive are added, and the material is discharged after stirring under a vacuum degree of 0.011 MPa for 0.5h, and the butyl rubber for photovoltaic module edge sealing is obtained; The Mooney viscosity of the liquid butyl rubber is controlled at 50 Pa·s, and the isoprene content accounts for 3.5% of the isobutene content; The filler is carbon black; The water absorbing agent is vinyltrimethoxysilane; The catalyst is di-n-octyltin dimercaptoacetate; The adhesive is a silane coupling agent containing epoxy groups.

[0010] Example 2 The preparation process of the self-made resin is as follows: taking 0.3 parts of hydroxyethyl methacrylate, 40 parts of acetonitrile, 3 parts of phenyl dichlorophosphate, 5 parts of triethylamine, 0.03 parts of 4-dimethylaminopyridine and 5 parts of 1,3,5-tris(2-hydroxyethyl) isocyanurate by weight fraction, phenyl dichlorophosphate and acetonitrile are added to the reactor, and under the condition of ice bath and nitrogen, the mixture is stirred at a rotating speed of 1600 r / min for 40 min, then the mixture of hydroxyethyl methacrylate and triethylamine is added dropwise into the reactor at 0℃ within 5h, and the reaction is continued at 0℃ for 2h, then 4-dimethylaminopyridine and 1,3,5-tris(2-hydroxyethyl) isocyanurate are slowly added into the reactor, the mixture is stirred in the ice bath for 3h, then it is heated to 85℃ and refluxed for 15h, after the solution is cooled to room temperature, the precipitated triethylamine hydrochloride is removed by filtration, then the filtrate is poured into deionized water with a volume of 5 times that of the filtrate, and the crude product is obtained by dichloromethane extraction, then the crude product is further washed with deionized water for 8 times, then the crude extract is dissolved in dichloromethane and dried with anhydrous magnesium sulfate, finally the dichloromethane is removed by distillation, and the self-made resin is obtained; Taking 300 parts of liquid butyl rubber, 30 parts of polyisobutylene, 300 parts of self-made resin, 200 parts of filler, 20 parts of catalyst, 5 parts of water absorbing agent and 10 parts of adhesive by weight fraction, the liquid butyl rubber, polyisobutylene and self-made resin are placed in a kneading kettle, stirred and kneaded at a temperature of 120℃ for 1h, then the temperature is raised to 170℃, then the filler and water absorbing agent are added and stirred for 2h, then the temperature is reduced to 100℃, then the catalyst and adhesive are added, and the material is discharged after stirring under a vacuum degree of-0.095Mpa for 0.8h, and the butyl rubber for photovoltaic module edge sealing is obtained; The Mooney viscosity of the liquid butyl rubber is controlled at 35Pa·s, and the isoprene content accounts for 5.5% of the isobutene content; The filler is carbon black; The water absorbing agent is vinyltrimethoxysilane; The catalyst is isooctyl dimercaptousccinate dibutyl tin; The adhesive is a silane coupling agent containing epoxy group.

[0011] Example 3 The preparation process of the self-made resin is as follows: taking 0.3 parts of hydroxyethyl methacrylate, 40 parts of acetonitrile, 5 parts of phenyl dichlorophosphate, 5 parts of triethylamine, 0.03 parts of 4-dimethylaminopyridine and 5 parts of 1,3,5-tris(2-hydroxyethyl) isocyanurate by weight, phenyl dichlorophosphate and acetonitrile are added to the reactor, and they are stirred in an ice bath and nitrogen atmosphere at a rotation speed of 2000 r / min for 40 min, then a mixed solution of hydroxyethyl methacrylate and triethylamine is added dropwise into the reactor at 0°C within 5 h, and the reaction is continued at 0°C for 1 h, then 4-dimethylaminopyridine and 1,3,5-tris(2-hydroxyethyl) isocyanurate are slowly added to the reactor, the mixture is stirred in an ice bath for 3 h, then it is heated to 98°C and refluxed for 15 h, after the solution is cooled to room temperature, the precipitated triethylamine hydrochloride is removed by filtration, then the filtrate is poured into 9 times the volume of deionized water, and the crude product is obtained by dichloromethane extraction, then the crude product is further washed with deionized water for 8 times, then the crude extract is dissolved in dichloromethane and dried with anhydrous magnesium sulfate, and finally the dichloromethane is removed by distillation to obtain the self-made resin; Taking 300 parts of liquid butyl rubber, 30 parts of polyisobutylene, 300 parts of self-made resin, 200 parts of filler, 20 parts of catalyst, 5 parts of water absorbing agent and 10 parts of adhesive by weight, the liquid butyl rubber, polyisobutylene and self-made resin are placed in a kneading kettle, stirred and kneaded at a temperature of 130°C for 1 h, then the temperature is raised to 170°C, then the filler and water absorbing agent are added and stirred for 1 h, then the temperature is lowered to 100°C, then the catalyst and adhesive are added, and after stirring for 0.8 h under a vacuum degree of-0.095 Mpa, the product is discharged, which is a butyl rubber for photovoltaic module edge sealing; The Mooney viscosity of the liquid butyl rubber is controlled at 40 Pa·s, and the isoprene content accounts for 5.5% of the isobutene content; The filler is any one of silicon micropowder; The water absorbing agent is vinyltrimethoxysilane; The catalyst is butyltin mercaptide; The adhesive is a silane coupling agent containing an epoxy group.

[0012] Comparative Example 1 Taking 300 parts of liquid butyl rubber, 30 parts of polyisobutylene, 300 parts of self-made resin, 200 parts of filler, 20 parts of catalyst, 5 parts of water absorbing agent and 10 parts of adhesive by weight, the liquid butyl rubber, polyisobutylene and self-made resin are placed in a kneading kettle, stirred and kneaded at a temperature of 130°C for 1 h, then the temperature is raised to 170°C, then the filler and water absorbing agent are added and stirred for 1 h, then the temperature is lowered to 100°C, then the catalyst and adhesive are added, and after stirring for 0.8 h under a vacuum degree of-0.095 Mpa, the product is discharged, which is a butyl rubber for photovoltaic module edge sealing; The liquid butyl rubber has a Mooney viscosity of 40 Pa-s, and the isoprene content is 5.5% of the isobutylene content; The filler is any one of silicon micropowder; The water absorbing agent is vinyl trimethoxysilane; The catalyst is butyl tin mercaptide; The adhesive is an epoxy group-containing silane coupling agent.

[0013] Table 1 Tear resistance Limiting oxygen index Tear resistance Limiting oxygen index Example 1 124 N / mm 40.6% Comparative Example 1 88 N / mm 21.7% Example 2 127 N / mm 41.8% Example 3 126 N / mm 41.9% From the data comparison of Examples 1-3 and Comparative Example 1 in Table 1, it can be seen that, in the present application, by adding the self-made resin, in the combustion process, the inert free radicals generated by the pyrolysis of the self-made flame retardant will capture hydrogen free radicals, oxygen free radicals and hydroxyl free radicals, then terminate the free radical chain reaction in the gas phase, and the free radicals will also combine with the active end groups, thereby avoiding further pyrolysis of the chain segments in the condensed phase, and the non-combustible gas generated will dilute the concentration of combustible gas and oxygen in the gas phase, and carry away the heat generated by combustion, thereby reducing the degree of combustion in the gas phase, and further improving the flame retardant performance of the system.

[0014] It is apparent for those skilled in the art that the present application is not limited to the details of the foregoing exemplary embodiments, and that the present application can be implemented in other particular forms without departing from the spirit or essential characteristics of the present application. Therefore, the embodiments should be considered in all respects as illustrative and not restrictive, and the scope of the present application should be defined by the appended claims rather than the above description, and it is intended to include all changes falling within the meaning and scope of equivalents of the claims. Any mark in the claims should not be considered as limiting the involved claims.

Claims

1. A butyl adhesive for sealing the edges of photovoltaic modules, characterized in that, Includes the following components by weight: 150-300 parts liquid butyl rubber 30-100 parts of polyisobutylene Homemade resin 150-300 parts 200-400 parts of filler 20-50 parts of catalyst 3-5 parts absorbent 2-20 parts adhesive.

2. The butyl sealant for sealing the edges of photovoltaic modules according to claim 1, characterized in that, The liquid butyl rubber has a Mooney viscosity of 35-50 Pa·s, and isoprene accounts for 3.5%-5.5% of the isobutylene content.

3. The butyl sealant for sealing the edges of photovoltaic modules according to claim 1, characterized in that, The preparation process of the self-made resin is as follows: Take 0.3-0.55 parts by weight of hydroxyethyl methacrylate, 30-40 parts by weight of acetonitrile, 3-5 parts by weight of phenyl phosphate dichloride, 3-5 parts by weight of triethylamine, 0.01-0.03 parts by weight of 4-dimethylaminopyridine, and 3-5 parts by weight of 1,3,5-tris(2-hydroxyethyl)isocyanurate. Add phenyl phosphate dichloride and acetonitrile to a reactor and stir for 30-40 minutes under ice bath and nitrogen conditions at a speed of 1200-2000 r / min. Then, add the mixed solution of hydroxyethyl methacrylate and triethylamine dropwise to the reactor over 3-5 hours at -2 to 0°C. The reaction was continued at ℃ for 1-2 hours. Then, 4-dimethylaminopyridine and 1,3,5-tris(2-hydroxyethyl)isocyanurate were slowly added to the reactor. The mixture was stirred in an ice bath for 2-3 hours, then heated to 85-98℃ and refluxed for 12-15 hours. After the solution cooled to room temperature, the precipitated triethylamine hydrochloride was removed by filtration. The filtrate was then poured into 5-10 times its volume of deionized water and extracted with dichloromethane to obtain the crude product. The crude product was then washed with deionized water 5-8 times. The crude extract was then dissolved in dichloromethane and dried with anhydrous magnesium sulfate. Finally, the dichloromethane was removed by distillation to obtain the self-made resin.

4. The butyl sealant for sealing the edges of photovoltaic modules according to claim 1, characterized in that, The filler is either carbon black or silica powder.

5. The butyl sealant for sealing the edges of photovoltaic modules according to claim 1, characterized in that, The absorbent is vinyltrimethoxysilane.

6. The butyl sealant for sealing the edges of photovoltaic modules according to claim 1, characterized in that, The catalyst is either dibutyltin dithiocarbamate or butyltin thiolate.

7. The butyl sealant for sealing the edges of photovoltaic modules according to claim 1, characterized in that, The adhesive is any one of epoxy-containing silane coupling agents, methoxy-containing silane coupling agents, amino-containing silane coupling agents, or silane oligomers.

8. A method for preparing butyl sealant for sealing photovoltaic modules as described in any one of claims 1-7, characterized in that, Includes the following steps: Liquid butyl rubber, polyisobutylene, and homemade resin are placed in a kneading kettle and kneaded for 1-2 hours at 120-130℃. The temperature is then increased to 160-170℃, followed by the addition of filler and water absorbent and stirring for 1-2 hours. The temperature is then lowered to 100-110℃, and finally, catalyst and adhesive are added. The mixture is stirred for 0.5-0.8 hours under a vacuum of -0.095-0.011 MPa before being discharged to obtain butyl rubber for sealing photovoltaic modules.