CN102029704B - Method for preparing thick polyvinyl butyral (PVB) film by direct water cooling process - Google Patents

Method for preparing thick polyvinyl butyral (PVB) film by direct water cooling process Download PDF

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Publication number
CN102029704B
CN102029704B CN2010105259832A CN201010525983A CN102029704B CN 102029704 B CN102029704 B CN 102029704B CN 2010105259832 A CN2010105259832 A CN 2010105259832A CN 201010525983 A CN201010525983 A CN 201010525983A CN 102029704 B CN102029704 B CN 102029704B
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water
temperature
film
pvb
tank
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CN102029704A (en
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陈庚
林卫平
汤君武
朱立疆
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Zhejiang Deste new materials Limited by Share Ltd
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ZHEJIANG DECENT PLASTIC CO Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07Flat, e.g. panels
    • B29C48/08Flat, e.g. panels flexible, e.g. films
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92609Dimensions
    • B29C2948/92647Thickness
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92904Die; Nozzle zone
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/88Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/919Thermal treatment of the stream of extruded material, e.g. cooling using a bath, e.g. extruding into an open bath to coagulate or cool the material

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

The invention belongs to the technical field of plastic molding and processing, in particular to a method for preparing a thick polyvinyl butyral (PVB) film by a direct water cooling process. The method comprises the following specific steps: (1) mixing materials; (2) extruding and plasticizing; (3) shaping by the direct water cooling process; (4) removing surface water; (5) performing online thickness measurement; and (6) drying, splitting and winding. In the invention, the PVB film with the thickness of more than 1mm is produced by combining the direct water cooling process with a drying treatment method, which can greatly reduce the time that a fused mixture of the PVB and a plasticizer is exposed to air, realize rapid cooling, high cooling efficiency and even thickness, and avoid the defects such as material aging and yellowing, reduced mechanical properties, shortened service life, high production cost and the like.

Description

A kind of water that utilizes directly cools off the method for preparing thick polyethylene butyral film
Technical field:
The invention belongs to the plastic molding processing technology field, be specifically related to a kind of water that utilizes and directly cool off the method for preparing thick polyethylene butyral film.
Background technology:
Water directly cooling be used in plastic granulating, sheet material, and the processing of profile shapes in very common; But it is the direct water-cooling process application is rarely found in sheet material or plastic sheeting; Disclosed only have patent: CN101177040A that the direct process for cooling of water is used for blown film, is used to solve the problem that film flake thickness degree is inhomogeneous and cooling is not enough.
Polyvinyl butyral resin (PVB) has the extraordinary transparency, mechanical strength, cold resistance, UV resistant performance, and the bonding force good to glass is to use the most a kind of intermediate layer material in the laminated glass field.The polyvinyl butyral resin of molten state and the mixture of plasticizer are exposed to and are prone in the air oxidation, chain rupture behavior take place, and material variable color jaundice, mechanical properties decrease, service life are shortened.
At present; The production technology of PVB film be polyvinyl butyral resin and plasticizer through extruder mixing after; Through the die moulding; Through embossing rod and the indirect cooling and shaping of chill roll, there is following weak point in this technology again: the one, and the time that under the condition of high temperature, is exposed to air owing to film is long, and material is prone to aging yellowing; The 2nd, owing to be indirect cooling, cooling effectiveness is not high, is difficult to produce the film of thickness greater than 1mm; The 3rd, the equipment investment of embossing rod and chill roll is bigger, has increased production cost.
Adopt the mode of the direct process for cooling of water to cooperate the method for oven dry processing to produce the PVB film, can greatly reduce the polyvinyl butyral resin of molten state and the mixture of plasticizer and be exposed to the airborne time, realize cooling fast, avoid above-mentioned problem.
Summary of the invention:
The purpose of this invention is to provide a kind of production method that can produce one-tenth-value thickness 1/10 greater than the polyvinyl butyral film of 1mm.
The present invention is achieved in that
A kind of water that utilizes directly cools off the method for preparing thick polyethylene butyral film, and concrete steps are as follows:
(1) batch mixing: with residual hydroxyl content at the PVB of 17-23% resin-oatmeal and diester class plasticizer and auxiliary agent; On homogenizer, mix; The rotating speed of homogenizer is 400-800rpm, and mixing time is 8-12min, is that benchmark calculates with PVB resin-oatmeal dry weight in the mixture; Plasticizer-containing 25-40%, auxiliary agent be 10-5000PPM.
(2) extrusion plasticizing: pour the mixture of step () gained into hopper, extrude, remove impurity through fondant filter, through the Melt Pump voltage stabilizing in the extruder plasticizing that has exhaust section; From the extrusion molding of T die, wherein, screw speed 20-50rpm, measuring pump rotating speed 20-40rpm; 80-100 ℃ of feeding section temperature, 140-160 ℃ of fluxing zone temperature, 150-165 ℃ of homogenizing zone temperature; Mold temperature is at 150-170 ℃, and the low both sides of the medium temperature of mould are slightly high, in order to guarantee the pressure of mould; Pressure sensor is set before Melt Pump the rotating speed of main frame is done closed-loop control, pressure is 2-5Mpa before the pump, and pressure is 10-18Mpa behind the pump.
(3) the direct cooling and shaping of water: the sheet material that comes out from the T type die directly gets into the tank cooling under the effect of traction, cooling water adopts deionized water, and a 2-5m is set outside tank 3Water tank cooperate cooling tower that water temperature is controlled between 20-40 ℃; Make water and the water in the water tank in the tank form a circulation through water pump; The temperature of water progressively raises on the water surface from the bottom in the tank, and water surface temperature is controlled less than 60 ℃, and the water temperature of the downward 10cm distance of the water surface is at 25-30 ℃; When water surface temperature is too high, increase the internal circulating load of water, the water internal circulating load is 5-10m 3, the distance of deflector roll is at 20-50cm in the water surface and the water.
(4) remove surface water: film through scraping damping roller, is removed lip-deep ponding after leaving the water surface, and the damping roller of scraping below film is arranged with drip; With importing on the delivery port after the water access of dripping, avoid the fluctuation of the water surface, after the traction of first road; Get into the first road baking oven; Temperature of oven is set in 70-90 ℃ and carry out air blast, and film no longer includes water from the baking oven surface, back of coming out, and is convenient to online measurement.
(5) thickness measurement online: the film that comes out from baking oven carries out in length and breadth the monitoring to thickness through the thickness measurement online system; And guide operating personnel on hauling speed, mould bolt, mold temperature, to finely tune to produce the satisfactory product of the uniformity, the x-ray detection system of selecting for use penetration capacity to be adjusted at the scope of 0.5-3mm detects.
(6) oven dry, splitting winding: the film that has anhydrated in the surface is done further to dry to handle to be adsorbed on the moisture in the film with removal through the second road baking oven; Bake out temperature is at 90-120 ℃; Go out behind the second road baking oven and observe testing product outward appearance situation through one lamp box again, cut that to batch promptly be finished product.
Above-mentioned diester class plasticizer is 3GO (triethylene glycol two tricaprylates), 4G7 (four contract three second, two heptanoates), DBS (dibutyl sebacate).
Above-mentioned auxiliary agent is: one of heat stabilizer, light stabilizer, bonding force conditioning agent or its combination.
The present invention compares the outstanding advantage of prior art:
1, the present invention can produce the polyvinyl butyral film of thickness greater than 1mm;
2, the present invention adopts the method production PVB film that the mode of the direct process for cooling of water cooperates oven dry to handle; Can greatly reduce the polyvinyl butyral resin of molten state and the mixture of plasticizer and be exposed to the airborne time; Realize cooling fast; Cooling effectiveness is high, and thickness is even, can avoid defectives such as material aging flavescence, mechanical properties decrease, shortening in service life, production cost height.
Description of drawings:
Fig. 1 is a production line sketch map of the present invention;
Fig. 2 is a tank sketch map of the present invention.
The specific embodiment:
With specific embodiment the present invention is further described below, referring to Fig. 1-2:
A kind of water that utilizes directly cools off the method for preparing thick polyethylene butyral film, and concrete steps are as follows:
(1) batch mixing: with residual hydroxyl content at the PVB of 17-23% resin-oatmeal and diester class plasticizer and auxiliary agent; On homogenizer, mix; The rotating speed of homogenizer is 400-800rpm, and mixing time is 8-12min, is that benchmark calculates with PVB resin-oatmeal dry weight in the mixture; Plasticizer-containing 25-40%, auxiliary agent be 10-5000PPM.
(2) extrusion plasticizing: pour the mixture of step () gained into hopper 1, extrude, remove impurity through fondant filter 3, through Melt Pump 4 voltage stabilizings in the extruder that has exhaust section 2 plasticizings; From 5 extrusion moldings of T die, wherein, screw speed 20-50rpm, measuring pump rotating speed 20-40rpm; 80-100 ℃ of feeding section temperature, 140-160 ℃ of fluxing zone temperature, 150-165 ℃ of homogenizing zone temperature; Mold temperature is at 150-170 ℃, and the low both sides of the medium temperature of mould are slightly high, in order to guarantee the pressure of mould; Pressure sensor is set before Melt Pump the rotating speed of main frame is done closed-loop control, pressure is 2-5Mpa before the pump, and pressure is 10-18Mpa behind the pump.
(3) the direct cooling and shaping of water: the sheet material that comes out from the T type die directly gets into tank 6 coolings under the effect of traction, cooling water adopts deionized water, and a 2-5m is set outside tank 6 3Water tank cooperate cooling tower that water temperature is controlled between 20-40 ℃; Make water and the water in the water tank in the tank 6 form a circulation through water pump; The temperature of water progressively raises on the water surface from the bottom in the tank 6, and water surface temperature is controlled less than 60 ℃, and the water temperature of the downward 10cm distance of the water surface is at 25-30 ℃; When water surface temperature is too high, increase the internal circulating load of water, the water internal circulating load is 5-10m 3, the distance of deflector roll 7 is at 20-50cm in the water surface and the water.
(4) remove surface water: film through scraping damping roller 8, is removed lip-deep ponding after leaving the water surface, and the damping roller 8 of scraping below film is arranged with drip; With importing on the delivery port 601 after the water access of dripping, avoid the fluctuation of the water surface, after first road traction 9; Get into the first road baking oven 10; The temperature of baking oven 10 is set in 70-90 ℃ and carry out air blast, and film no longer includes water from baking oven 10 surface, back of coming out, and is convenient to online measurement.
(5) thickness measurement online: the film that comes out from baking oven 10 carries out in length and breadth the monitoring to thickness through the thickness measurement online system; And guide operating personnel on hauling speed, mould bolt, mold temperature, to finely tune; To produce the satisfactory product of the uniformity, the x-ray detection system 11,12 of selecting for use penetration capacity to be adjusted at the scope of 0.5-3mm detects.
(6) oven dry, splitting winding: the film that has anhydrated in the surface is done further to dry to handle to be adsorbed on the moisture in the film with removal through the second road baking oven 13; Bake out temperature is at 90-120 ℃; Go out behind the second road baking oven 13 and observe testing product outward appearance situation through one lamp box 14 again, cut that to batch promptly be finished product.
Above-mentioned diester class plasticizer is 3GO (triethylene glycol two tricaprylates), 4G7 (four contract three second, two heptanoates), DBS (dibutyl sebacate).
Above-mentioned auxiliary agent is: one of heat stabilizer, light stabilizer, bonding force conditioning agent or its combination.
With preparation thickness 1.52mm, the PVB intermediate coat of width 1850mm is an example:
With 100 parts of PVB resins, 30 parts of plasticizer 3GO (triethylene glycol two tricaprylates) and 0.03 part of antioxidant 1010,0.02 part of ultra-violet absorber UV326; 0.005 part bonding force conditioning agent; Under the rotating speed of 600RPM, mixed 10 minutes, put into to plastify in the double screw extruder and extrude.
Concrete process conditions are:
The temperature in twin-screw eight districts is respectively: 80 ℃, and 120 ℃, 140 ℃, 145 ℃, 145 ℃, 150 ℃; 155 ℃, 155 ℃, 150 ℃ of melt filtration actuator temperatures, 155 ℃ of Melt Pump temperature, T type die 13 district's temperature are respectively: 165 ℃, 160 ℃; 158 ℃, 156 ℃, 156 ℃, 155 ℃, 155 ℃, 155 ℃; 156 ℃, 156 ℃, 158 ℃, 160 ℃, 165 ℃.
The mould mouth is a dried up height 2cm, 50 ℃ of flume surface coolant-temperature gages, deflector roll water clearance 35cm under water, draught line speed 1.2m/min.80 ℃ of the first road oven temperatures, 110 ℃ of the second road oven temperatures.
Through detecting the PVB the key technical indexes be:
Yellowness index 8.9, thickness 1.52 ± 3mm, moisture 0.42% is to the bonding force 52N/cm of glass, light transmittance 87.6%, mist degree 0.5%.
The foregoing description is merely one of preferred embodiment of the present invention, is not to limit practical range of the present invention with this, so: all equivalences of doing according to shape of the present invention, structure, principle change, and all should be covered by within protection scope of the present invention.

Claims (3)

1. one kind is utilized water directly to cool off the method for preparing thick polyethylene butyral film, it is characterized in that having following steps:
(1) batch mixing: with residual hydroxyl content at the PVB of 17-23% resin-oatmeal and diester class plasticizer and auxiliary agent; On homogenizer, mix; The rotating speed of homogenizer is 400-800rpm, and mixing time is 8-12min, is that benchmark calculates with PVB resin-oatmeal dry weight in the mixture; Plasticizer-containing 25-40%, auxiliary agent are 10-5000PPM;
(2) extrusion plasticizing: pour the mixture of step () gained into hopper, extrude, remove impurity through fondant filter, through the Melt Pump voltage stabilizing in the extruder plasticizing that has exhaust section; From the extrusion molding of T die, wherein, screw speed 20-50rpm; Measuring pump rotating speed 20-40rpm, 80-100 ℃ of feeding section temperature, 140-160 ℃ of fluxing zone temperature; 150-165 ℃ of homogenizing zone temperature, mold temperature are at 150-170 ℃, and the low both sides of the medium temperature of mould are slightly high; Pressure sensor is set before Melt Pump the rotating speed of main frame is done closed-loop control, pressure is 2-5Mpa before the pump, and pressure is 10-18Mpa behind the pump;
(3) the direct cooling and shaping of water: the sheet material that comes out from the T type die directly gets into the tank cooling under the effect of traction, cooling water adopts deionized water, and a 2-5m is set outside tank 3Water tank cooperate cooling tower that water temperature is controlled between 20-40 ℃; Make water and the water in the water tank in the tank form a circulation through water pump; The temperature of water progressively raises on the water surface from the bottom in the tank, and water surface temperature is controlled less than 60 ℃, and the water temperature of the downward 10cm distance of the water surface is at 25-30 ℃; When water surface temperature is too high, increase the internal circulating load of water, the water internal circulating load is 5-10m 3, the distance of deflector roll is at 20-50cm in the water surface and the water;
(4) remove surface water: film after leaving the water surface through scraping damping roller; Remove lip-deep ponding; The damping roller of scraping below film is arranged with drip, imports on the delivery port after the water that drips is inserted, after the traction of first road; Get into the first road baking oven, temperature of oven is set in 70-90 ℃ and carry out air blast;
(5) thickness measurement online: the film that comes out from baking oven carries out in length and breadth to the monitoring of thickness through the thickness measurement online system, and to produce the satisfactory product of the uniformity, the x-ray detection system of selecting for use penetration capacity to be adjusted at the scope of 0.5-3mm detects;
(6) oven dry, splitting winding: the film that has anhydrated in the surface is done further to dry to handle to be adsorbed on the moisture in the film with removal through the second road baking oven; Bake out temperature is at 90-120 ℃; Go out behind the second road baking oven and observe testing product outward appearance situation through one lamp box again, cut that to batch promptly be finished product.
2. a kind of water that utilizes according to claim 1 directly cools off the method for preparing thick polyethylene butyral film, it is characterized in that: described diester class plasticizer is 3GO, 4G7, DBS.
3. a kind of water that utilizes according to claim 1 directly cools off the method for preparing thick polyethylene butyral film, and it is characterized in that: described auxiliary agent is: one of heat stabilizer, light stabilizer, bonding force conditioning agent or its combination.
CN2010105259832A 2010-10-30 2010-10-30 Method for preparing thick polyvinyl butyral (PVB) film by direct water cooling process Active CN102029704B (en)

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CN102504456A (en) * 2011-10-31 2012-06-20 陈庆江 Production process and production system of durable PVB (polyvinyl butyral) intermediate films
CN102514173B (en) 2011-12-07 2014-05-21 浙江大学 Dynamic microchannel plastic extrusion-molding device and method
CN103171121B (en) * 2011-12-26 2016-01-20 上海晶棠安全玻璃技术应用研究中心 A kind of solar energy power generating PVB doubling film manufacturing method
CN103029927B (en) * 2012-12-10 2015-07-01 上海宝钢磁业有限公司 Novel powder polyvinyl alcohol grain feeder and feeding process
CN103660249A (en) * 2013-11-28 2014-03-26 南宁市日建塑料包装有限责任公司 Sheet thickness adjusting device of plastic sheet machine
CN103728677B (en) * 2013-12-26 2016-02-03 石平辉 Plastics convex lens array film goods of biodegradable environmental protection and preparation method thereof
CN104441566B (en) * 2014-11-11 2017-01-11 界首市鑫豪塑胶有限公司 PVC (polyvinyl chloride) plastic flooring cooling and setting method
CN104844739A (en) * 2015-05-15 2015-08-19 亿帆鑫富药业股份有限公司 Crosslinkable PVB (polyvinyl butyral), production method of crosslinkable PVB, and method utilizing crosslinkable PVB to produce crosslinkable PVB film
CN108099083A (en) * 2017-12-25 2018-06-01 福州福启橡塑有限公司 A kind of sheet rubber extrusion molding production line
CN109176997A (en) * 2018-07-27 2019-01-11 芜湖凯兴汽车电子有限公司 A kind of plastic products processing rapid cooling shaping equipment
CN109702979A (en) * 2018-12-17 2019-05-03 嘉兴彩虹光学膜片科技有限公司 A kind of plastic film extrusion cooling device
CN111347647A (en) * 2020-03-27 2020-06-30 江苏奥天利新材料有限公司 Preparation method of temperature-control color-changing PVB intermediate film
CN116967036B (en) * 2023-08-01 2024-07-19 肇庆理士电源技术有限公司 Electrostatic spraying production line for dry electrode production

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Address after: 317200 Chicheng City, Zhejiang province Tiantai County Street workers East Road, No. 801

Patentee after: Zhejiang Deste new materials Limited by Share Ltd

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Denomination of invention: A method of preparing thick polyvinyl butyral film by direct cooling with water

Effective date of registration: 20200909

Granted publication date: 20121128

Pledgee: Zheshang Bank Limited by Share Ltd. Taizhou branch

Pledgor: ZHEJIANG DECENT NEW MATERIAL Co.,Ltd.

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