CN108032579B - Internally plasticized sound-insulation PVB film and preparation method thereof - Google Patents
Internally plasticized sound-insulation PVB film and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/42—Layered products comprising a layer of synthetic resin comprising condensation resins of aldehydes, e.g. with phenols, ureas or melamines
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1515—Three-membered rings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/24—All layers being polymeric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/10—Properties of the layers or laminate having particular acoustical properties
- B32B2307/102—Insulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2419/00—Buildings or parts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/12—Photovoltaic modules
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
- B32B2605/08—Cars
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
- B32B2605/12—Ships
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
- B32B2605/18—Aircraft
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Joining Of Glass To Other Materials (AREA)
- Laminated Bodies (AREA)
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Abstract
The invention relates to an internally plasticized sound-insulating PVB film and a preparation method thereof, wherein the internally plasticized sound-insulating PVB film comprises the following components: the PVB film at least comprises a three-layer structure and at least comprises two types of PVB films, wherein one type of PVB film is a conventional PVB film, and the other type of PVB film is a conventional PVB film, and 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester is used as an internal plasticizer and reacts with hydroxyl on PVB, and finally the internal plasticizer is grafted in a PVB molecular chain in a side group mode to play a self-lubricating role, so that the fluidity is high, and the processability is good. The finally obtained internally plasticized sound-insulating PVB multilayer film has excellent safety and processability and also has better sound-insulating property.
Description
Technical Field
The invention belongs to the field of application of safety glass laminated films, and particularly relates to an internally plasticized sound-insulation PVB film and a preparation method thereof.
Background
Polyvinyl butyral (hereinafter referred to as PVB) resin is a main raw material for producing PVB films, and belongs to the field of thermoplastic polymer materials. Through development of more than half a century, the PVB membrane becomes a necessary raw material for producing various safety glasses due to excellent optical performance, high temperature resistance, low temperature resistance, mechanical performance and good bonding performance to inorganic glass. When the PVB membrane is strongly impacted by the outside, the PVB membrane can absorb impact energy, does not generate broken sheets, has safety characteristics, and develops functions of sound insulation, light control, heat insulation, color change, fog prevention, privacy, theft prevention and the like in recent years, is an ideal safe glass processing material, and is widely applied to the industries of automobiles and buildings.
Along with the development of world economy, the improvement of the economic level of people continuously improves the requirement on the comfort of the environment, and the sound insulation performance is more and more emphasized. Methods of blocking sound transmission typically utilize materials to isolate or block the transmission of sound energy. On one hand, when sound waves are incident to the material, a part of the sound waves are reflected by the interface, and on the other hand, for the damping material, when a part of the sound waves are transmitted in the material, the mechanical energy of vibration can cause viscous flow loss and relative motion among material molecules to cause internal friction, and sound energy is converted into heat energy to be dissipated, so that the aim of sound insulation is fulfilled.
With the increasing serious problem of noise pollution, the PVB laminated glass industry is actively exploring how to improve the sound insulation performance of the material and maximize the sound insulation amount. A single-layer interlayer having particularly good sound absorption properties has insufficient mechanical stability and adhesive properties. Researchers have generally achieved improved sound insulation performance using multi-layer systems. CN 105172289 a states that an interlayer film for laminated glass composed of at least two sub-films, wherein the first sub-film comprises PVB having a proportion of polyvinyl acetate groups of 0.1-11 mol% and the second sub-film comprises PVB having a proportion of polyvinyl acetate groups of 5-8 mol%, has an improved sound-insulating effect. Patent CN 104884247 a also proposes at least two sub-films, wherein the first sub-film is composed of PVB containing plasticizer with a polyvinyl alcohol content of 17 to 22 wt%, and the second sub-film is composed of PVB containing plasticizer with a polyvinyl alcohol content of 11 to 14 wt%, while ensuring the safety performance, the sound-insulating property is improved. At present, in the proposed means for increasing the sound insulation effect, the amount of the plasticizer in the middle layer is increased to different degrees to increase the difference between layers, so that the energy loss in the sound energy transmission process between different damping layers is increased, the sound insulation performance is increased, certain influence is more or less caused on the safety and the processing performance of the film, and in addition, the migration can be generated to two sides due to the higher plasticizer content in the middle layer, so that the sound insulation effect is reduced. How to increase the sound insulation capability as much as possible on the basis of ensuring the processing performance and the safety performance is still a research hotspot.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an internally plasticized sound-insulating PVB film and a preparation method thereof.
The invention adopts the following technical scheme: an internally plasticized sound-insulating PVB film is composed of at least three PVB films, at least two PVB films are included, the outer layer is a conventional PVB film, and the middle layer is a high-fluidity film containing an internal plasticizer of 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester.
The middle layer of the internally plasticized sound-insulating PVB film takes 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester as an internal plasticizer, as shown in a structural formula (I),
the oxygen heterocyclic ring on the molecular chain reacts with the hydroxyl (structural formula II) in the PVB,
the C-O bond on the 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester is broken to produce new hydroxyl, meanwhile, a molecular chain is grafted to a PVB molecular chain, the obtained structural formula is shown as a formula (III),
in the preparation method of the internally plasticized sound-insulating PVB film, in the processing process, part of 4, 5-epoxy dioctyl (2-ethylhexyl) phthalate added in the middle layer reacts with hydroxyl in PVB in a molten state and is grafted to a PVB molecular chain in a side chain form, so that the hydrogen bond interaction between hydroxyl functional groups is reduced, the fluidity of the PVB film is improved, and the PVB film has a self-lubricating effect; another portion is present in the PVB as a blend to act as an external plasticizer or compatibilizer, which can facilitate the compatibility of other plasticizers with the PVB and reduce the bleeding of other plasticizers.
As a preferable technical proposal, the addition amount of the 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester is 0.01 to 30 percent.
As a preferred technical scheme, the PVB used has the hydroxyl content of 10-30 percent and the ester group content of 0.1-6 percent.
As a preferred solution, one or more compounds selected from the following are used as co-plasticizers: di-2-ethylhexyl sebacate (DOS), di-2-ethylhexyl adipate (DOA), di-2-ethylhexyl phthalate (DOP), di-2-butoxyethyl adipate (DBEA), dihexyl adipate (DHA), dibutyl sebacate (DBS), di-2-butoxyethyl sebacate (DBES), diisononyl 1, 2-cyclohexanedicarboxylate (DINCH), di-isononyl phthalate (DINP) and triethylene glycol-bis-2-ethylhexanoate (3G 8).
As a preferred technical scheme, the total plasticizer content in the internally plasticized sound-insulating PVB film is 26-28 wt%, so that the safety and the processing performance of the internally plasticized sound-insulating PVB film are ensured.
As a preferable technical scheme, in order to promote the reaction of the 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester and the polyvinyl acetal, a ring-opening initiator is added to promote the reaction, and the initiator is selected from one or more of triethylene diamine, dimethylaniline, methyl tetrahydrophthalic anhydride, tris- (dimethylaminomethyl) phenol, tris-2-ethylhexanoate and succinic anhydride.
As a preferred technical scheme, the intermediate layer contains metal ions of less than 150 ppm.
The plasticized acoustic PVB film of the present invention includes other additives known to those skilled in the art such as UV-absorbers, antioxidants, adhesion modifiers, surface tension modifiers, organic or inorganic nanoparticles, stabilizers.
As a preferred technical scheme, the processing process of the sound insulation PVB film can be performed in a co-extrusion manner.
The invention also protects the internally plasticized sound-insulating PVB film for use in automobiles, aircraft, architectural glazings, watercraft or in photovoltaic modules.
Compared with the prior art, the invention has the following beneficial effects.
In the sound insulation PVB film produced by the invention, the 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester is used as an internal plasticizer in the interlayer, and reacts with hydroxyl in the PVB, so that the self-lubricating effect is achieved, the fluidity of the film is increased, the dispersion of other additives is facilitated, and the precipitation of a co-plasticizer is reduced; in addition, the reaction generates the same amount of hydroxyl groups, so that the adhesive property between the glass and different types of PVB is not adversely affected.
The sound insulation PVB film produced by the invention increases the flow property of the interlayer under the condition of not increasing the content of the plasticizer, thereby increasing the capability range of viscous flow loss caused by the mechanical energy of vibration when sound is transmitted and internal friction caused by the relative motion between material molecules, namely increasing the capability of converting sound energy into heat energy. The sound insulation effect is obviously improved, and the safety and the processing performance of the sound insulation material are not sacrificed.
The sound insulation PVB film produced by the invention reduces the dosage of the external plasticizer due to the addition of the plasticizer in the interlayer, thereby not only improving the overall mechanical property of the film, but also reducing the migration of the plasticizer in the interlayer.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail and completely with reference to the following embodiments. It should be understood that the described embodiments are only a few embodiments of the present invention, not all embodiments, and are not to be construed as limiting the present invention. Based on the embodiments of the present invention, any person skilled in the art can make no creative effort or substantial adjustment according to the present invention, and the protection scope of the present invention is still covered.
The test method comprises the following steps:
the method for testing tensile strength and elongation at break comprises the following steps: the sample preparation and measurement are carried out according to the national standard GB/T32020-.
(II) an anti-penetration test method: the sample preparation and determination are carried out according to the national standard GB/T9656-.
(III) a fused finger test method:
1. the instrument comprises the following steps: XNR-400GM type melt flow Rate determination apparatus, Changzhou DemTure precision Instrument Co.
2. The method comprises the following steps: the test is carried out according to the national standard GB/T3682-2000, about 6g of samples are weighed and cut into small particles of 2mm multiplied by 2 mm. And (3) waiting for the charging barrel of the XNR-400GM type melt flow rate tester to be heated to the set value of 140 ℃, stabilizing for 10min, pulling out the piston rod, and adding a sample to be tested. The piston rod was reinserted and compacted, the temperature was maintained for 10min, then a 21.6kg weight was added, the test was started when the rod was lowered until the lower marker ring was level with the barrel, and the weight of the strip flowing out of the melt finger tester port was weighed as m1, m2 for 1 min.
3. And (3) calculating: melt index (m1+ m2) × 5 (unit: g/10min)
(IV) a sound insulation quantity test method: according to the measurement of the enterprise standard Q/DSTGF 001-.
The starting materials used in the following examples were all commercially available.
Example 1
200kg of PVB resin powder and various auxiliaries (an antioxidant, a surface tension control agent and a binding power control agent) are added into a powder mixer, and the mixture is stirred at a high speed of 1000RPM for 20 minutes, wherein the temperature of the material is controlled between 40 ℃ and 50 ℃. Wherein 100kg of resin powder is added with 28.5kg of 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester and 9.5kg of 3G8 as plasticizers at the rotating speed of 20RPM, stirred at low speed for 5-10 minutes, passes through a 52-type double-screw extruder, the processing temperature is set between 160 ℃ and 190 ℃, the resin is melted and plasticized at the rotating speed of 80RPM, and the plasticized resin is introduced into a middle module of a three-layer die; and adding 38kg of 3G8 into 100kg of resin powder at the rotating speed of 20RPM, stirring at low speed for 5-10 minutes, passing through a 95-type twin-screw extruder, setting the processing temperature between 160 ℃ and 190 ℃, melting and plasticizing under the condition of the rotating speed of a screw of 80RPM, and introducing into the outer layer of the three-layer die after plasticizing. And forming sound insulation PVB films with uniform thickness, cooling, shaping and coiling to obtain the finished product.
Example 2
200kg of PVB resin powder, 25.3kg of 4, 5-epoxytetrahydrodioctyl phthalate (2-ethylhexyl) ester and 12.7kg of 3G8 were mixed by the same procedure as in example 1 to obtain a sound-insulating PVB multilayer film.
Example 3
200kg of PVB resin powder, 19kg of 4, 5-epoxytetrahydrodioctyl phthalate (2-ethylhexyl) ester and 19kg of 3G8 were mixed by the same procedure as in example 1 to obtain a sound-insulating PVB multilayer film.
Example 4
200kg of PVB resin powder, 12.7kg of 4, 5-epoxytetrahydrodioctyl phthalate (2-ethylhexyl) ester and 25.3kg of 3G8 were mixed by the same procedure as in example 1 to obtain a sound-insulating PVB multilayer film.
Example 5
200kg of PVB resin powder, 9.5kg of 4, 5-epoxytetrahydrodioctyl phthalate (2-ethylhexyl) ester and 28.5kg of 3G8 were mixed by the same procedure as in example 1 to obtain a sound-insulating PVB multilayer film.
Comparative example 1
200kg of PVB resin powder and various auxiliaries (an antioxidant, a surface tension control agent and a binding power control agent) are added into a powder mixer, and the mixture is stirred at a high speed of 1000RPM for 20 minutes, wherein the temperature of the material is controlled between 40 ℃ and 50 ℃. Wherein 100kg of resin powder is added with 38kg of 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester of plasticizer at the rotating speed of 20RPM, stirred at low speed for 5-10 minutes, passes through a 52-type double-screw extruder, the processing temperature is set between 160 ℃ and 190 ℃, the resin is melted and plasticized at the rotating speed of the screw of 80RPM, and the plasticized resin is introduced into a middle module of a three-layer die; and adding 38kg of 3G8 into 100kg of resin powder at the rotating speed of 20RPM, stirring at low speed for 5-10 minutes, passing through a 95-type twin-screw extruder, setting the processing temperature between 160 ℃ and 190 ℃, melting and plasticizing under the condition of the rotating speed of a screw of 80RPM, and introducing into the outer layer of the three-layer die after plasticizing. And forming sound insulation PVB films with uniform thickness, cooling, shaping and coiling to obtain the finished product.
Comparative example 2
100kg of PVB resin powder and various auxiliaries (an antioxidant, a surface tension control agent and a binding power control agent) are added into a powder mixer, and the mixture is stirred at a high speed of 1000RPM for 20 minutes, wherein the temperature of the material is controlled between 40 ℃ and 50 ℃. Finally, 3G8 containing 38kg of plasticizer was added at 20RPM and stirred at low speed for 5-10 minutes. Then the mixture is put into a double-screw extruder in a metering mode, the processing temperature is set between 160 ℃ and 190 ℃, the mixture is melted and plasticized under the condition of the rotating speed of a screw rod being 80RPM, a PVB film with uniform thickness is formed through a T-shaped die with an opening being 0.5mm-0.8mm, and the PVB film is cooled, shaped and coiled into a finished product.
The PVB intermediate film test results are shown in Table 1.
TABLE 1
Examples 1-5 were sheets prepared with the plasticizer and 3G8 added in different ratios in the middle layer, and comparative examples 1 and 2 were cases where only one plasticizer was added to the middle layer. As seen from Table I, the addition of dioctyl (2-ethylhexyl) 4, 5-epoxytetrahydrophthalate as an internal plasticizer to the middle layer of the acoustical product significantly increases the melt index of the product and improves flowability. A certain amount of 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester is added, the tensile strength and the elongation at break are qualified, when only one internal plasticizer is added into the middle layer, the fluidity is too large, the whole safety performance of the product is affected, the penetration resistance is unqualified, and therefore, the addition amount needs to be optimized; the addition of an internal plasticized membrane provides an increase in sound insulation over conventional PVB membranes.
The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, improvements, equivalents and the like that fall within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. An internal plasticized sound insulation PVB film is characterized by comprising at least three layers of PVB films, at least two PVB films are included, the outer layer is a conventional PVB film, and the middle layer is a high-fluidity film containing an internal plasticizer of 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester; the middle layer takes 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester as an internal plasticizer, the structure is shown as formula (I),
the oxygen heterocyclic ring on the molecular chain reacts with the hydroxyl in the PVB, the hydroxyl is shown as a structural formula (II),
the C-O bond on the 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) is broken to produce new hydroxyl, and meanwhile, the molecular chain is grafted to the PVB molecular chain to obtain the structural formula shown in the formula (III),
the addition amount of the 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester is 0.01-30%; the hydroxyl content of the PVB is 10-30%, and the ester group content is 0.1-6%; di-isononyl phthalate (DINP) and triethylene glycol-bis-2-ethylhexanoate (3G8) were used as co-plasticizers and no other plasticizers, and the total plasticizer content of the sound-damping PVB film was 26-28% by weight.
2. The sound-insulating PVB film according to claim 1, wherein during processing, a part of 4, 5-epoxy tetrahydro dioctyl phthalate (2-ethylhexyl) ester added in the interlayer reacts with hydroxyl groups in PVB in a molten state, and is grafted to PVB molecular chains in a side chain manner, and another part of the 4, 5-epoxy tetrahydro dioctyl phthalate exists in the PVB film in a blended manner and serves as an external plasticizer or a compatilizer.
3. An acoustic PVB film according to claim 1, wherein said interlayer comprises less than 150ppm of metal ions.
4. The sound-insulating PVB film according to claim 1, wherein the sound-insulating PVB film is processed by co-extrusion.
5. An internally plasticized acoustic PVB film according to any of claims 1-4 for use in an automobile, aircraft, architectural glazing, watercraft or in a photovoltaic module.
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| DE102004043907A1 (en) * | 2004-09-10 | 2006-03-16 | Kuraray Specialities Europe Gmbh | Plasticizer-containing PVB films with ether bonds containing carboxylic acid esters as co-plasticizer |
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Denomination of invention: An inner plasticized sound insulation PVB film and its preparation method Effective date of registration: 20200909 Granted publication date: 20200512 Pledgee: Zheshang Bank Limited by Share Ltd. Taizhou branch Pledgor: ZHEJIANG DECENT NEW MATERIAL Co.,Ltd. Registration number: Y2020330000682 |