CN117186453A - Method for improving compatibility of plasticizer in polyvinyl acetal intermediate film - Google Patents
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- CN117186453A CN117186453A CN202310157288.2A CN202310157288A CN117186453A CN 117186453 A CN117186453 A CN 117186453A CN 202310157288 A CN202310157288 A CN 202310157288A CN 117186453 A CN117186453 A CN 117186453A
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- polyvinyl acetal
- plasticizer
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- interlayer film
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- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 81
- 239000004014 plasticizer Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 42
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 title 1
- 150000001241 acetals Chemical class 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000011354 acetal resin Substances 0.000 claims abstract description 26
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 26
- 239000011229 interlayer Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003377 acid catalyst Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims 3
- 230000008569 process Effects 0.000 abstract description 7
- 230000001105 regulatory effect Effects 0.000 abstract description 7
- 230000001276 controlling effect Effects 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000004220 aggregation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 125000004036 acetal group Chemical group 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 239000003995 emulsifying agent Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 4
- 238000005481 NMR spectroscopy Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000006359 acetalization reaction Methods 0.000 description 3
- 150000001299 aldehydes Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000005340 laminated glass Substances 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 2
- MUGSTXRSLGJVOB-UHFFFAOYSA-N 2-[2-[2-(6-methylheptanoyloxy)ethoxy]ethoxy]ethyl 6-methylheptanoate Chemical compound C(CCCCC(C)C)(=O)OCCOCCOCCOC(CCCCC(C)C)=O MUGSTXRSLGJVOB-UHFFFAOYSA-N 0.000 description 1
- FRQDZJMEHSJOPU-UHFFFAOYSA-N Triethylene glycol bis(2-ethylhexanoate) Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CCCC FRQDZJMEHSJOPU-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a method for improving the compatibility of a plasticizer in a polyvinyl acetal intermediate film, which starts from a temperature process according to the acetal reaction kinetics of polyvinyl acetal resin, and improves the compatibility of the polyvinyl acetal resin and the plasticizer by regulating and controlling the aggregation structure of the polyvinyl acetal. The method of the invention not only improves the fluidity and the processability of the polyvinyl acetal film, but also improves the compatibility and the performance stability of the plasticizer, has the characteristics and advantages of simple operation and no need of newly adding other process equipment, and has good market competitiveness.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a method for improving the compatibility of plasticizers in a polyvinyl acetal intermediate film, and the polyvinyl acetal resin and the polyvinyl acetal intermediate film prepared by the method.
Background
The polyvinyl acetal intermediate film is a key component material for manufacturing laminated glass, is prepared by melt extrusion of polyvinyl acetal resin and a certain proportion of plasticizer, and is widely applied to the fields of automobiles, buildings, photovoltaics and the like. The processability of the polyvinyl acetal intermediate film is one of the key evaluation parameters, and the performance quality and the production processing efficiency of the polyvinyl acetal intermediate film are directly determined. Because the polyvinyl acetal intermediate film is produced and processed by mixing a certain proportion of plasticizer, how to maintain the compatibility and stability of the body and the plasticizer is the key for improving the stability and quality of the application performance of the polyvinyl acetal intermediate film.
In the production and processing of the polyvinyl acetal intermediate film, the polyvinyl acetal resin and the plasticizer are gradually heated and plasticized after entering an extruder, and the mixture effect is achieved through shearing of a screw, and then the mixture is extruded through a die head and then cooled and molded. The obtained polyvinyl acetal interlayer film was then bonded to glass at high temperature and high pressure to produce laminated glass. However, when the compatibility of the polyvinyl acetal resin and the plasticizer is insufficient, a problem of precipitation of the plasticizer and maldistribution of the plasticizer in the intermediate film product are extremely liable to occur at the time of cooling molding. Taking an automobile windshield as an example, it is required to have extremely high adhesion, impact resistance and weather resistance at the same time. Under these performance requirements, the adjustable window of the plasticizer content and the acetalization degree of the polyvinyl acetal are very narrow, and the quality of the final product of the polyvinyl acetal intermediate film can only be improved from the improvement of the compatibility of the polyvinyl acetal resin with the plasticizer and the uniformity in the processing process.
In order to improve the compatibility of the polyvinyl acetal and the plasticizer, other means such as adding other compatibility-assisting formulas are adopted in the prior published document, and although the precipitation rate of the plasticizer of the polyvinyl acetal interlayer can be reduced to a certain extent, the problems of durability and stability of the plasticizer cannot be guaranteed, and the cost of processing raw materials is increased. In practice, polyvinyl acetals contain predominantly hydrophobic acetal groups and hydrophilic hydroxyl groups, while plasticizers tend to be hydrophobic esters. Improving the compatibility of the polyvinyl acetal with the plasticizer can be achieved by increasing the acetal group content and dispersibility. As described above, the regulation range of the acetal group content is limited based on the performance requirement of the polyvinyl acetal interlayer film, and only by regulating the dispersibility thereof can be achieved.
In terms of regulating the dispersibility of groups, it has been reported in the known documents that the compatibility with plasticizers is regulated by mixing polyvinyl acetals with different acetal group ratios so as to achieve the uniform average acetal group content, but this method is liable to cause instability of impact resistance under high-temperature and low-temperature conditions. There are also well known documents that the sequence distribution of polyvinyl acetals can be regulated by different kinds of emulsifiers or surfactants. However, the emulsifier is often difficult to be effectively and completely removed in the polyvinyl acetal product, so that the problem of yellowing of the polyvinyl acetal intermediate film and the like is caused. In addition, the residual emulsifier also causes a decrease in fluidity of the polyvinyl acetal and a decrease in heat resistance.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, a main object of the present invention is to provide a method for improving the compatibility of plasticizers in a polyvinyl acetal interlayer, and a polyvinyl acetal resin and a polyvinyl acetal interlayer prepared by the method.
The regulation of the sequence distribution of the polyvinyl acetal can be carried out both kinetically and thermodynamically. Since thermodynamic methods generally involve changes in the reaction system, there is a higher demand for raw materials, equipment; the sequence distribution is simpler and the operability is realized by dynamically controlling the sequence distribution. The industrial production of polyvinyl acetals is usually a precipitation process, in which the reaction proceeds from homogeneous to heterogeneous phase as the acetalization degree increases and the product gradually precipitates due to the decrease in solubility. The heterogeneous reaction is extremely easy to generate the phenomenon of non-uniform reaction, and the reaction rate can be greatly influenced due to the limited contact area of materials. By regulating and controlling the temperature rising rate and the gradient temperature rising process, the acetalization in the molecule can be compensated by utilizing the temperature from the acetal reaction dynamics angle, and the acetal rate and uniformity in the heterogeneous phase can be improved. By utilizing the self-acceleration effect of the acetal reaction, the reaction is carried out towards the high sequence dispersibility direction with lower energy barrier and more stable chemical structure, more continuous hydroxyl phase areas are obtained, and the compatibility between the continuous acetal groups and the ester plasticizer is better realized. In the polyvinyl acetal intermediate film, the improvement of the compatibility of the plasticizer can improve the flow property and the processability of materials, and has positive promotion effect on improving the processing efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for improving the compatibility of plasticizers in polyvinyl acetal interlayer films. The method is characterized by comprising the following steps:
(1) At the temperature of 5-30 ℃, the acid catalyst and aldehyde are added into the polyvinyl alcohol aqueous solution within 5-60 min. Wherein, the acid catalyst and aldehyde are added by fully stirring and uniformly mixing one component with the polyvinyl alcohol aqueous solution, and then adding the other component;
(2) The temperature of the reaction system is raised to 60-80 ℃ in a gradient way. Specifically, firstly heating the system to 30-50 ℃ at a speed of not lower than 20 ℃/h, preserving heat and curing for 5-90 min, and then heating the system to 60-80 ℃ at a speed of not lower than 20 ℃/h, preserving heat and curing for 5-240 min;
(3) Cooling the cured reaction system to below 60 ℃, then adding alkali liquor into the system, keeping stirring for 5-30 min, and filtering to obtain a solid resin product;
(4) Washing the solid resin product with pure water for 1-10 times, and filtering to obtain a washing product;
(5) Drying the cleaning product at 40-60 ℃ to obtain polyvinyl acetal resin;
(6) The polyvinyl acetal resin obtained above was mixed with a plasticizer, and extrusion casting was performed to obtain a polyvinyl acetal interlayer film.
Wherein: the polyvinyl acetal prepared by the method has a hydroxyl value of 17-20wt% and a c/i ratio of VA structural units of more than 0.75; the melt index of the polyvinyl acetal resin at 120 ℃ and 27.5 percent of plasticizer addition is more than or equal to 1.5g/10min; under the compatibility test, the polyvinyl acetal intermediate film is placed on supersaturated CuSO 4 Plasticization after 72h of solutionThe precipitation area of the agent is less than or equal to 1.5cm 2 。
Further, step (2) is preferably: heating the reaction system to 35-50 ℃ at a speed of not less than 20 ℃/h, preserving heat and curing for 5-60 min, and heating the reaction system to 65-80 ℃ at a speed of not less than 20 ℃/h, preserving heat and curing for 60-240 min.
Further, the temperature rising rate in the step (2) is more preferably not less than 30 ℃/h, thereby achieving the purpose of accelerating the kinetics of the acetal reaction.
Further, in the step (1), no emulsifier is added during the reaction.
Further, the temperature range of 5 to 30℃in the step (1) is preferably 5 to 20 ℃.
Further, in the step (3), the temperature of the reaction system is reduced to below 60 ℃, so that a large amount of heat is mainly prevented from being released in the acid-base neutralization reaction at the moment of adding alkali liquor, and PVB resin is locally heated unevenly to cause coarsening or agglomeration of particles.
Further, in the step (1), the mass of the aldehyde accounts for 50-60% of the mass of the polyvinyl alcohol.
Further, in step (1), the acidic catalyst includes at least one of hydrochloric acid, sulfuric acid, nitric acid, and p-toluenesulfonic acid.
In the step (6), the intermediate film is prepared by single-screw or double-screw extrusion casting, and the addition amount of the plasticizer accounts for 27.5% of the mass of the polyvinyl acetal intermediate film.
Further, in the step (6), no other auxiliary capacity formulation system is required to be added in the manufacturing process of the intermediate film.
The c/i of the polyvinyl acetal resin obtained above was obtained by hydrogen nuclear magnetic resonance spectroscopy 1 H NMR) was measured. In characterizing c/i of the polyvinyl acetal resin by nuclear magnetic resonance hydrogen spectrometry, 5mg of the polyvinyl acetal resin was sufficiently dissolved in 0.5mL of DMSO-d6, and scanned at least 16 times on a 600MHz nuclear magnetic resonance spectrometer. The resulting nuclear magnetic patterns were integrated using the MestReNova software, and the ratio of the mole fractions of H element in the interval of 4.35 to 4.25ppm (c-VA) to 4.25 to 4.15ppm (i-VA) was calculated and referred to as the c/i value.
The hydroxyl value of the polyvinyl acetal resin prepared above was tested by a chemical titration method. The hydroxyl groups in the polyvinyl acetal resin are esterified with acetic anhydride in pyridine solution, and the excess acetic anhydride is hydrolyzed. And taking phenolphthalein as an indicator, titrating and neutralizing with a NaOH standard solution, and calculating the hydroxyl content in the polyvinyl acetal resin.
The test method of the prepared polyvinyl acetal resin melt finger comprises the following steps: 27.5wt% of triethylene glycol di-isooctanoate is added, and the mixture is passed through a melt index apparatus at 120 ℃ under a load of 21.6kg, and the outflow mass at 10min is recorded as the melt index in g/10min.
The method for testing the compatibility of the plasticizer in the prepared polyvinyl acetal intermediate film comprises the following steps: placing the polyvinyl acetal intermediate film at a constant temperature and humidity for 24h under the conditions that the humidity is 30% and the temperature is 25 ℃ and placing the polyvinyl acetal intermediate film at the bottom to contain oversaturated CuSO under the environment temperature of 25 DEG C 4 The deposition area after 72 hours was calculated in the desiccator of the solution.
Compared with the prior art, the invention has the beneficial effects that:
compared with the existing production process, the reaction process of the invention does not need to add additives such as emulsifying agent which can influence the product performance. According to the acetal reaction kinetics of the polyvinyl acetal resin, the compatibility of the polyvinyl acetal resin and the plasticizer is improved by regulating and controlling the sequence distribution of the polyvinyl acetal from the temperature process. The method improves the fluidity and the processability of the polyvinyl acetal film, and improves the compatibility and the performance stability of the plasticizer. The invention also has the characteristics and advantages of simple operation and no need of newly adding other process equipment, and has good market competitiveness.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) 100g of polyvinyl alcohol having an average polymerization degree of 1700 was dissolved in 1000mL of pure water and stirred at 90℃for 1 hour to be sufficiently dissolved, and then cooled to 15 ℃. Adding 35g of hydrochloric acid with the mass concentration of 36-38% into the system, and fully and uniformly mixing. 57g of butyraldehyde were then added dropwise to the system at a constant rate over 30 minutes.
(2) After butyraldehyde is added, stirring and reacting for 20min at the temperature; then, heating the reaction system to 40 ℃ at a speed of 30 ℃/h, and stirring and reacting for 30min at the temperature; finally, the reaction system was heated from 40℃to 70℃at 30℃per hour, and reacted at this temperature with stirring for 2 hours.
(3) The temperature of the reaction system is reduced to 50 ℃, 40mL of 15wt% sodium hydroxide is added into the reaction liquid, and the mixture is stirred for 15min and centrifugally dehydrated to obtain a solid product.
(4) And (3) repeatedly washing and filtering the solid product for 5 times at 50 ℃, and carrying out suction filtration to obtain a cleaning product.
(5) And (3) placing the cleaning product in a forced air drying box, and drying for 4 hours at 50 ℃ to obtain the polyvinyl acetal resin product.
(6) The polyvinyl acetal resin obtained above was mixed with 27.5% of triethylene glycol di-2-ethylhexanoate as a plasticizer, and a polyvinyl acetal intermediate film was produced by a single screw extruder.
Example 2
The procedure and conditions were the same as in example 1, except that the temperature gradient increasing rate of both steps in the reaction system in step (2) was changed to 20℃per hour.
Example 3
The procedure and conditions were the same as in example 1, except that the temperature gradient increasing rate of both steps in the reaction system in step (2) was changed to 60℃per hour.
Example 4
The procedure and conditions were the same as in example 1, except that the reaction system was stirred at 40℃for 60 minutes in step (2).
Example 5
The procedure and conditions were the same as in example 1, except that the reaction system was stirred at 40℃for 90 minutes in step (2).
Example 6
The procedure and conditions were the same as in example 1, except that the temperature was lowered to 10℃in step (1).
Example 7
The procedure and conditions were the same as in example 1, except that the temperature was lowered to 20℃in step (1).
Comparative example 1
The procedure and conditions were the same as in example 1 except that sodium dodecylbenzenesulfonate was added to the system in an amount of 0.1wt% relative to the total amount of PVA after the temperature was lowered to 15℃in step (1).
Comparative example 2
The procedure and conditions were the same as in example 1, except that in step (2), the reaction system was directly warmed to 70℃at 30℃per hour.
Comparative example 3
The procedure and conditions were the same as in example 1, except that the gradient heating rate in the reaction system in step (2) was changed to 10℃per hour.
Comparative example 4
The procedure and conditions were the same as in example 1 except that the cooling treatment was not performed on the reaction system before the addition of the alkali liquor in step (3).
Table 1 evaluation results of polyvinyl acetals
The foregoing description of the exemplary embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (10)
1. A method for improving plasticizer compatibility in a polyvinyl acetal interlayer film, comprising the steps of:
(1) Adding an acid catalyst and aldehyde into the polyvinyl alcohol aqueous solution within 5-60 min at the temperature of 5-30 ℃;
(2) Heating the reaction system to 30-50 ℃ at a speed of not less than 20 ℃/h, preserving heat and curing for 5-90 min, and heating the reaction system to 60-80 ℃ at a speed of not less than 20 ℃/h, preserving heat and curing for 5-240 min;
(3) Cooling the cured reaction system to below 60 ℃, then adding alkali liquor into the system, keeping stirring for 5-30 min, and filtering to obtain a solid resin product;
(4) Washing the solid resin product with pure water for 1-10 times, and filtering to obtain a washing product;
(5) Drying the cleaning product at 40-60 ℃ to obtain polyvinyl acetal resin;
(6) And mixing the polyvinyl acetal resin with a plasticizer, and performing extrusion casting to obtain the polyvinyl acetal intermediate film.
2. The method of improving plasticizer compatibility in a polyvinyl acetal interlayer film according to claim 1, wherein: in the step (1), the acid catalyst and the aldehyde are added by fully stirring and uniformly mixing one component with the polyvinyl alcohol aqueous solution, and then adding the other component.
3. The method for improving the compatibility of plasticizers in a polyvinyl acetal interlayer film according to claim 1, wherein the step (2) is: heating the reaction system to 35-50 ℃ at a speed of not less than 20 ℃/h, preserving heat and curing for 5-60 min, and heating the reaction system to 65-80 ℃ at a speed of not less than 20 ℃/h, preserving heat and curing for 60-240 min.
4. The method for improving compatibility of plasticizers in a polyvinyl acetal interlayer film according to claim 1, wherein a temperature rising rate in the step (2) is not less than 30 ℃/h.
5. The method of improving plasticizer compatibility in a polyvinyl acetal interlayer film according to claim 1, wherein: the temperature in the step (1) is 5-20 ℃.
6. The method of improving plasticizer compatibility in a polyvinyl acetal interlayer film according to claim 1, wherein: the mass of the aldehyde in the step (1) accounts for 50-60% of the mass of the polyvinyl alcohol.
7. The method of improving plasticizer compatibility in a polyvinyl acetal interlayer film according to claim 1, wherein: in step (1), the acidic catalyst comprises at least one of hydrochloric acid, sulfuric acid, nitric acid and p-toluenesulfonic acid.
8. The method of improving plasticizer compatibility in a polyvinyl acetal interlayer film according to claim 1, wherein: in the step (6), no other auxiliary capacity formulation system is needed to be added in the manufacturing process of the intermediate film.
9. The method of improving plasticizer compatibility in a polyvinyl acetal interlayer film according to claim 1, wherein: in the step (5), the hydroxyl value of the polyvinyl acetal resin is 17-20wt%, the c/i ratio of the VA structural unit is more than 0.75, and the melt index of the polyvinyl acetal resin at 120 ℃ and 27.5% of plasticizer addition amount is more than or equal to 1.5g/10min.
10. The method of improving plasticizer compatibility in a polyvinyl acetal interlayer film according to claim 1, wherein: in step (6), the polyvinyl acetal interlayer film is placed in supersaturated CuSO 4 The precipitation area of the plasticizer after 72 hours of the solution is less than or equal to 1.5cm 2 。
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310157288.2A CN117186453A (en) | 2023-02-23 | 2023-02-23 | Method for improving compatibility of plasticizer in polyvinyl acetal intermediate film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310157288.2A CN117186453A (en) | 2023-02-23 | 2023-02-23 | Method for improving compatibility of plasticizer in polyvinyl acetal intermediate film |
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| CN202310157288.2A Pending CN117186453A (en) | 2023-02-23 | 2023-02-23 | Method for improving compatibility of plasticizer in polyvinyl acetal intermediate film |
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- 2023-02-23 CN CN202310157288.2A patent/CN117186453A/en active Pending
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