Improved glue and PET base material co-granulation type protective film and manufacturing method thereof

A production method and improved technology, applied in the direction of adhesives, adhesive types, pressure-sensitive films/sheets, etc., can solve the problem of harsh storage and transportation conditions, high organic solvent prices, and difficult recycling of protective films/adhesive tapes, etc. The problem is to achieve a win-win situation of economic and social environmental benefits, the preparation method is simple and feasible, and the effect of resisting the influence of environmental humidity is achieved.

Pending Publication Date: 2020-05-08

TECH SUN INT KUNSHAN

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AI-Extracted Technical Summary

Problems solved by technology

[0009] 2. As solid hazardous waste, it should be handled by a qualified professional institution: the cost of this kind of treatment is high, and the price of treatment fee per ton ranges from 4,000 yuan to 5,000 yuan, and the storage and transportation conditions are harsh, which is difficult for ordinary enterprises to bear;

The disadvantages of this treatment method are: due to the use of organic solvents, there are hidden fire safety and occupational health safety hazards; the high price of organic solvents leads to unreasonable economics, and the organic solvents after use also have problems to be treated

However, in view of the huge differences between PET and various pressure-sensitive adhesives in chemical composition, molecular structure, molecular weight, modulus, melt index, surface free energy, and solubility parameters, various protective materials based on PET It is difficult to recycle the film/adhesive tape through co-extrusion granulation, so how to solve the compatibility of PET and the pressure-sensitive adhesive coating coated on it during extrusion granulation It is the key to solve the production and research and development of PET substrate co-granulation protective film

[0015] The use of polyester pressure-sensitive polymer materials can effec...

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Abstract

The invention discloses an improved glue and PET base material co-granulation type protective film and a manufacturing method thereof. The protective film comprises a PET base material, the surface ofthe PET base material subjected to corona treatment is coated with a moderately cross-linked improved saturated polyester pressure-sensitive adhesive coating subjected to solubilization and graft modification treatment, a release film can be attached to the moderately cross-linked improved saturated polyester pressure-sensitive adhesive coating subjected to solubilization and graft modification treatment, and the improved saturated polyester pressure-sensitive adhesive subjected to solubilization and graft modification treatment in the moderately cross-linked improved saturated polyester pressure-sensitive adhesive coating subjected to solubilization and graft modification treatment comprises graft-modified saturated polyester macromolecules, polycaprolactone and polyacrylate components.The prepared pressure-sensitive adhesive is excellent in adhesive property and good in edge bearing property compared with a traditional protective film preparation process, and after the pressure-sensitive adhesive is used, the waste protective film can be directly extruded and granulated to obtain reusable novel plastic particles, so subsequent reutilization is convenient.

Application Domain

Pressure sensitive film/foil adhesivesFilm/foil adhesive release liners +1

Technology Topic

PelletizingPolyester +9

Image

Examples

Experimental program(3)

Example Embodiment

[0088] Example 1

[0089] A method for making a protective film that can be co-granulated with improved glue and PET substrate:

[0090] A. Chemical synthesis of improved saturated polyester pressure-sensitive adhesives treated with solubilization and grafting:

[0091] 1. Polymerization of compatibilizer:

[0092] 1) Mix accurately measured 90Kg of caprolactone monomer, 3.0Kg of acrylic acid, 3.0Kg of hydroxyethyl acrylate and 60Kg of xylene in the reaction kettle and heat up to 140°C-150°C to stabilize the reflux for 10 minutes above;

[0093] 2) Dissolve 0.50Kg stannous octoate with 10Kg xylene and add it dropwise to the reaction kettle within 10 minutes; the preparation container and dropping tank of stannous octoate are rinsed twice with 10Kg xylene respectively, and the flushing solution is collected in In the reactor;

[0094] 3) Continue to keep the temperature at 140°C-150°C to stabilize the reflux for more than 15 minutes;

[0095] 4) The polymerization time is not less than 240 minutes; a solubilizing agent solution is obtained;

[0096] 2. Synthesis of improved saturated polyester pressure-sensitive adhesive with solubilization and grafting treatment:

[0097] 1) take by weighing 70Kg, 15Kg, 10Kg, 50Kg, 10Kg, 10Kg, 10Kg, 10Kg respectively the total 185Kg of toluene for use;

[0098] 2) Add 300Kg of accurately metered ETERKYD5016-TS-52 type thermoplastic saturated copolymerized high molecular weight polyester resin solution and 70Kg of toluene with a solid content of 52 ± 2% into the reactor and stir and dissolve the solubilizer solution evenly, then heat up to Between 88-95°C, keep the reflux stable for 15 minutes or more;

[0099] 3) Get 1000g of 20% water-containing BPO and stir and dissolve it in 15Kg of toluene, and let it stand for more than 60 minutes. % BPO was stirred and dissolved in 10Kg of toluene, and left to stand for more than 60 minutes. After the solution became clear and transparent, the water precipitated at the bottom of the liquid was removed to obtain a monomer initiator solution. Take 800g of BPO containing 20% water and stirred and dissolved in 10Kg In the toluene of the solution, leave it still for more than 60 minutes, after the solution becomes clear and transparent, remove the moisture precipitated at the bottom of the liquid to obtain an additional solution for the initiator;

[0100] 4) Mix accurately measured 21.6Kg of isooctyl acrylate, 2.7Kg of acrylic acid, and 2.7Kg of hydroxyethyl acrylate in a stainless steel container, and then add the monomer initiator solution to obtain the monomer drip solution;

[0101] 5) Add the initiator drip solution to the reactor within 10 minutes, then control the reaction temperature at 88-95°C and react for 20-30 minutes;

[0102] 6) Evenly add the monomer dropwise liquid into the reactor, and the dropwise time is 180 minutes;

[0103] 7) After the dropwise addition is completed, add the initiator supplement solution dropwise within 10 minutes when the reaction is 60 minutes, and continue the reaction at 88°C-95°C for more than 60 minutes;

[0104] 8) 0.68Kg of the grafted catalyst stannous octoate is dissolved in 10Kg of toluene to obtain a catalyst solution; the catalyst solution is added to the reactor, and the toluene of 10Kg is used to rinse the dropping tank and related pipelines for 2 times. Put it into the reaction kettle evenly in 5-10 minutes;

[0105] 9) Keep the temperature between 88-95°C and continue the reaction for 60 minutes or more to complete the grafting reaction;

[0106] 10) Cool the reactor to 35-45°C, turn off the nitrogen protection, and stop stirring;

[0107] 11) filter and discharge the material into the barrel, and store in a sealed manner to obtain a solubilized graft-modified saturated polyester pressure-sensitive adhesive with a solid content of 40%;

[0108] B. Preparation of improved saturated polyester pressure-sensitive adhesive coating solution for solubilization and grafting:

[0109] 1) 5Kg Cymel303 type methyl etherified melamine resin was stirred and dissolved with 10Kg of ethyl acetate to obtain a crosslinking agent dilution;

[0110] 2) Slowly add 50Kg of the improved saturated polyester pressure-sensitive adhesive treated with solubilizer grafting to 25Kg of ethyl acetate under stirring, and continue stirring for more than 30 minutes to obtain the glue dilution;

[0111] 3) Add the crosslinking agent diluent and 875g of tributyl citrate to the glue diluent under stirring, and continue to stir for more than 30 minutes to obtain the improved saturated polyester pressure-sensitive adhesive with solubilization and grafting treatment. agent coating liquid;

[0112] C. Coating of modified saturated polyester pressure-sensitive adhesive coating:

[0113] Apply the prepared solubilized and grafted modified saturated polyester pressure-sensitive adhesive coating solution to the corona surface of PET substrate 1 with a multi-functional coater, and the corona value is not less than 52mN/ m, the thickness of the coated dry glue is controlled to be 10 microns, the time for the protective film to pass through the drying section of the 135°C oven is not less than 1 minute, and the anti-adhesive release film 3 is pasted at the winding station to obtain a PET-based Solubilized and grafted improved co-granulated protective film for materials. The coated protective film needs to be post-cured at 55°C for no less than 48 hours before it can achieve stable viscosity and meet customer requirements.

[0114] D. Regranulation test of protective film that can be co-granulated with improved glue and PET substrate:

[0115] 1) Simple sorting of the used improved glue to be re-granulated and recycled and the co-granulated protective film of the PET substrate to remove other types of materials;

[0116] 2) According to the feeding size of the screw extrusion granulator, the protective film to be recycled and granulated is cut into specifications of appropriate size;

[0117] 3) Set the parameters such as the screw speed and the temperature of the extruder to carry out granulation recovery;

[0118] 4) After water-cooling and air-cooling, the extruded molten strips are cut into plastic particles of specifications, and the particles are light yellow;

[0119] The new plastic particles recovered can be used for further processing or sold.

[0120] The basic properties of the improved adhesive and PET substrate co-granulation protective film prepared in Example 1 are shown in Table 1. Table 1 The basic properties of a co-granulation protective film of the improved adhesive and PET substrate

[0121]

[0122] The basic properties of the improved glue and PET base material co-granulation protective film in Example 1 can meet the requirements for the use of the protective film. The produced particles are light yellow, with smooth surface and high mechanical strength. Polyester and adhesive It has good compatibility with solvents and can meet the requirements of injection molding, extrusion molding, blow molding and other processing techniques. It can be used as a new PET compound, fiber, etc., and meets the requirements of reuse.

Example Embodiment

[0123] Example 2

[0124] A method for making a protective film that can be co-granulated with improved glue and PET substrate:

[0125]A. Preparation of improved saturated polyester pressure-sensitive adhesive coating solution for solubilization and grafting:

[0126] 1) 6Kg Cymel303 type methyl etherified melamine resin was stirred and dissolved with 10Kg of ethyl acetate to obtain a crosslinking agent dilution;

[0127] 2) Slowly add 40Kg of the solubilized and graft-modified modified saturated polyester pressure-sensitive adhesive into 24Kg of ethyl acetate under stirring, and continue stirring for more than 30 minutes to obtain the glue dilution;

[0128] 3) Add the crosslinking agent diluent and 700g of tributyl citrate to the glue diluent under stirring, and continue to stir for more than 30 minutes to obtain the improved saturated polyester pressure-sensitive adhesive with solubilization and grafting treatment. agent coating liquid;

[0129] B. Coating of modified saturated polyester pressure-sensitive adhesive coating:

[0130] Apply the prepared solubilized and grafted improved saturated polyester pressure-sensitive adhesive coating solution to the corona surface of PET substrate 1 with a multi-functional coater, and the corona value is not less than 52mN/m, Control the thickness of the coated dry glue to 10 microns, control the time for the protective film to pass through the drying section of a 135°C oven for not less than 1 minute, and attach the anti-adhesive release film 3 at the winding station to produce a PET-based Co-granulation protective film, the coated protective film needs to be post-cured at 55°C for no less than 48 hours before it can achieve stable viscosity and meet customer requirements;

[0131] C. Regranulation test of protective film that can be co-granulated with improved glue and PET substrate:

[0132] 1) Simple sorting of the used PET base material co-granulation protective film to be re-granulated and recycled to remove other types of materials;

[0133] 2) According to the feeding size of the screw extrusion granulator, the protective film to be recycled and granulated is cut into specifications of appropriate size;

[0134] 3) Set the parameters such as the screw speed and the temperature of the extruder to carry out granulation recovery;

[0135] 4) After water-cooling and air-cooling, the extruded molten material strips are cut into plastic particles of specifications, and the particles are light yellow; the recovered new plastic particles can be used for further processing or sale;

[0136] The basic properties of the improved glue prepared in Example 2 and the PET base material co-granulation protective film are shown in Table 2

[0137] Table 2 Basic properties of a co-granulation protective film with improved glue and PET substrate

[0138]

[0139]

[0140] It can be seen that the basic properties of the improved glue and PET base material co-granulation protective film in Example 2 can meet the requirements for the use of the protective film. The particles produced are light yellow, with smooth surface and high mechanical strength. Polyester and The adhesive has good compatibility and can meet the processing techniques of injection molding, extrusion molding, blow molding, etc. It can be used as a new PET compound, fiber, etc., and meets the requirements of reuse.

Example Embodiment

[0141] Example 3

[0142] A method for making a double-sided protective film that can be co-granulated with improved glue and PET substrate:

[0143] A. Preparation of improved saturated polyester pressure-sensitive adhesive coating solution for solubilization and grafting:

[0144] 1) Stir and dissolve 10Kg of Cymel303 type methyl etherified melamine resin with 10Kg of ethyl acetate to obtain a crosslinking agent dilution;

[0145] 2) Slowly add 50Kg of the solubilized and grafted saturated polyester pressure-sensitive adhesive to 40Kg of ethyl acetate under stirring, and continue stirring for more than 30 minutes to obtain the glue dilution;

[0146] 3) Add the crosslinking agent diluent and 875g of tributyl citrate to the glue diluent under stirring, and continue to stir for more than 30 minutes to obtain the improved saturated polyester pressure-sensitive adhesive with solubilization and grafting treatment. agent coating liquid;

[0147] B. Coating of modified saturated polyester pressure-sensitive adhesive coating:

[0148] Apply the prepared solubilized and grafted modified saturated polyester pressure-sensitive adhesive coating solution to the corona surface of PET substrate 1 with a multi-functional coater, and the corona value is not less than 52mN/ m, control the thickness of the coated dry glue to 10 microns, control the time for the protective film to pass through the drying section of the 135°C oven for not less than 1 minute, and attach the anti-adhesive release film 3 at the winding station, and then repeatedly coat the PET base On the other side of material 1, an improved co-granulation double-sided protective film with PET as the base material was prepared. The coated protective film can only be achieved after post-curing at 55°C for no less than 48 hours. The viscosity is stable and meets the requirements of customers;

[0149] C. Regranulation test of double-sided protective film that can be co-granulated with improved glue and PET substrate:

[0150] 1) Simply sort the used PET base material co-granulation double-sided protective film to be re-granulated to remove other types of materials;

[0151] 2) According to the feeding size of the screw extrusion granulator, cut the double-sided protective film to be recycled and granulated into specifications of appropriate size;

[0152] 3) Set the parameters such as the screw speed and the temperature of the extruder to carry out granulation recovery;

[0153] 4) The extruded molten strip is water-cooled and air-cooled, and then cut into plastic particles of the specification, which are yellowish; the recycled new plastic particles can be used for further processing or sale.

[0154] The basic properties of the improved glue and PET base material co-granulation double-sided protective film prepared in Example 3 are shown in Table 3. Table 3 An improved glue and PET base material co-granulation double-sided protective film is basically performance

[0155]

[0156] It can be seen that the basic properties of the double-sided protective film that can be co-granulated with the improved glue and PET substrate in Example 3 can meet the requirements for the use of the protective film. The particles produced are light yellow, with smooth surfaces and high mechanical strength. Polyester It has good compatibility with adhesives and can meet the requirements of injection molding, extrusion molding, blow molding, etc. It can be used as a new PET compound, fiber, etc., and meets the requirements of reuse.

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the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

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