CN109536115B - Preparation method of solvent type PU flocking adhesive - Google Patents

Preparation method of solvent type PU flocking adhesive Download PDF

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CN109536115B
CN109536115B CN201811462504.XA CN201811462504A CN109536115B CN 109536115 B CN109536115 B CN 109536115B CN 201811462504 A CN201811462504 A CN 201811462504A CN 109536115 B CN109536115 B CN 109536115B
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polyester
flocking
preparation
solvent
mixture
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CN109536115A (en
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陆建明
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Suzhou Lushi New Material Co ltd
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Suzhou Lushi New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • C09J175/06Polyurethanes from polyesters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/42Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4202Two or more polyesters of different physical or chemical nature
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/42Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4236Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
    • C08G18/4238Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C08G18/7671Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to a preparation method of a solvent type PU flocking adhesive, which comprises the following steps: (a) dissolving polyester dihydric alcohol, polyester trihydric alcohol and thermoplastic TPU in a mixed solvent, and dehydrating to obtain a first mixture; the mass ratio of the polyester diol to the polyester triol to the thermoplastic TPU is 100: 40-60: 15-25; (b) and adding liquefied MDI into the first mixture, sealing, continuously mixing for 10-15 hours by using a shaking machine, sealing, standing for 3 days, and adjusting to 38-43% of solid content and 200-400 cps of viscosity. Therefore, the method can be directly used for the flocking process of the PVC sealing strip, on-site preparation is not needed, the curing condition meets the requirements of the on-line flocking process (120 ℃, 3-5 min), and the flocking wear-resistant requirement is met.

Description

Preparation method of solvent type PU flocking adhesive
Technical Field
The invention belongs to the field of adhesives, relates to a flocking adhesive, and particularly relates to a preparation method of a solvent type PU flocking adhesive.
Background
The automobile flocking sealing strip mainly comprises a window side sealing strip (water cutting) and a window glass guide groove, and has the functions of sealing external wind and rain, preventing dust from entering, reducing noise, enabling glass to slide more easily and the like. The flocking adhesive applied to the PVC sealing strip at present is mainly a bi-component system (namely bi-component polyurethane solvent adhesive), the usable time of the A component and the B component after mixing is generally 1-2 hours, and the existing technology is generally adopted for a small amount of times and is prepared on site; if field management is disordered, and the viscosity of the A component and the B component is continuously increased after the A component and the B component are mixed, the flocking quality is difficult to effectively control.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a solvent type PU flocking adhesive.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a solvent type PU flocking adhesive comprises the following steps:
(a) dissolving polyester dihydric alcohol, polyester trihydric alcohol and thermoplastic TPU in a mixed solvent, and dehydrating to obtain a first mixture; the mass ratio of the polyester diol to the polyester triol to the thermoplastic TPU is 100: 40-60: 15-25;
(b) adding liquefied MDI into the first mixture, sealing, continuously shaking up and mixing for 10-15 hours by a shaking up machine, sealing and standing for a plurality of days, and adjusting the solid content to 38-43% and the viscosity to 200-400 cps; the NCO/OH value (molar ratio) of the materials is 1.4-1.8.
Optimally, the mass ratio of the polyester diol to the polyester triol to the thermoplastic TPU is 100: 50: 20.
preferably, the mixed solvent is a mixture of cyclohexanone, butanone, toluene, xylene, ethyl acetate and butyl acetate.
Optimally, in step (b), the standing time is 3 days.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: according to the preparation method of the solvent type PU flocking adhesive, the first mixture of specific components and liquefied MDI are subjected to mixing reaction, and the solid content and viscosity of the product are adjusted, so that the solvent type PU flocking adhesive can be directly used for a flocking process of PVC sealing strips, on-site preparation is not needed, the curing condition meets the requirement of an on-line flocking process (120 ℃ @ 3-5 min), and the flocking abrasion-resistant requirement is met.
Detailed Description
The invention relates to a preparation method of a solvent type PU flocking adhesive, which comprises the following steps: (a) dissolving polyester dihydric alcohol, polyester trihydric alcohol and thermoplastic TPU in a mixed solvent, and dehydrating to obtain a first mixture; the mass ratio of the polyester diol to the polyester triol to the thermoplastic TPU is 100: 40-60: 15-25; (b) adding liquefied MDI into the first mixture, uniformly mixing, sealing and standing for a plurality of days, and adjusting the solid content to 38-43% and the viscosity to 200-400 cps; the NCO/OH value (molar ratio) of the materials is 1.4-1.8. The first mixture of the specific components and the liquefied MDI are subjected to mixing reaction, and the solid content and viscosity of the product are adjusted, so that the method can be directly used for the flocking process of the PVC sealing strip without field preparation, and the curing condition meets the requirements of an online flocking process (120 ℃ @ 3-5 min) (namely high-temperature rapid curing) and meets the requirements of flocking and abrasion resistance.
The mass ratio of the polyester diol, the polyester triol and the thermoplastic TPU is preferably 100: 50: 20; the PU flocking adhesive has optimal performance. The mixed solvent is a mixture consisting of a plurality of cyclohexanone, butanone, toluene, xylene, ethyl acetate and butyl acetate; in the step (b), the standing time is 3 days
The present invention will be further illustrated with reference to the following examples.
Example 1
The embodiment provides a preparation method of a solvent type PU flocking adhesive, which comprises the following steps:
(a) dissolving 100 parts of polyester diol (usually polybutylene adipate with molecular weight of about 2000), 50 parts of polyester triol (with molecular weight of about 400) and 20 parts of thermoplastic TPU (with activation temperature of 55-65 ℃) in a mixed solvent (cyclohexanone: butanone 1: 2 in volume ratio), and dehydrating to obtain a first mixture;
(b) and adding 100 parts of liquefied MDI into the first mixture, sealing, continuously shaking and mixing for 10-15 hours by using a shaking machine, sealing and standing for 3 days, and adjusting the solid content to 38-43% and the viscosity to 200-400 cps.
Example 2
This example provides a method for preparing a solvent-based PU flocking adhesive, which is substantially the same as that in example 1, except that: in step (a), the polyester diol, the polyester triol and the thermoplastic TPU are added in amounts of 100 parts, 50 parts and 25 parts, respectively.
Example 3
This example provides a method for preparing a solvent-based PU flocking adhesive, which is substantially the same as that in example 1, except that: in step (a), the amounts of polyester diol, polyester triol and thermoplastic TPU added were 100 parts, 55 parts and 15 parts, respectively.
Example 4
This example provides a method for preparing a solvent-based PU flocking adhesive, which is substantially the same as that in example 1, except that: in step (a), the polyester diol, the polyester triol and the thermoplastic TPU are added in amounts of 100 parts, 55 parts and 20 parts, respectively.
Comparative example 1
This example provides a method for preparing a solvent-based PU flocking adhesive, which is substantially the same as that in example 1, except that: thermoplastic TPU is not included.
Comparative example 2
This example provides a method for preparing a solvent-based PU flocking adhesive, which is substantially the same as that in example 3, except that: thermoplastic TPU is not included.
The PU flocking glue prepared in the embodiments 1-4 and the comparative examples 1-2 is applied to the preparation of flocking sample pieces, and the preparation method specifically comprises the following steps:
(1) scrubbing the PVC sealing strip by using isopropanol;
(2) uniformly coating glue on the surface of the PVC sealing strip, and flocking (conventional process; electrostatic flocking, voltage of 3-4 kv/cm); then heating and drying at 120 deg.C for 4min, and standing at room temperature for more than 3 days.
The performance test was carried out according to the test method for abrasion of flocked weather strip for vehicle, QC/T624-.
TABLE 1 Performance Table of flocked sample obtained by Using PU flocking adhesive in examples 1 to 4 and comparative examples 1 to 2
Figure BDA0001888958510000031
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.

Claims (3)

1. A preparation method of a solvent type PU flocking adhesive is characterized by comprising the following steps:
(a) dissolving polyester dihydric alcohol, polyester trihydric alcohol and thermoplastic TPU in a mixed solvent, and dehydrating to obtain a first mixture; the mass ratio of the polyester diol to the polyester triol to the thermoplastic TPU is 100: 40-60: 15-25;
(b) and adding liquefied MDI into the first mixture, sealing, continuously mixing for 10-15 hours by using a shaking machine, sealing, standing for a plurality of days, and adjusting to 38-43% of solid content and 200-400 cps of viscosity.
2. The preparation method of the solvent-type PU flocking adhesive according to claim 1, which is characterized in that: the mixed solvent is a mixture consisting of a plurality of cyclohexanone, butanone, toluene, xylene, ethyl acetate and butyl acetate.
3. The preparation method of the solvent-type PU flocking adhesive according to claim 1, which is characterized in that: in the step (b), the standing time is 3 days.
CN201811462504.XA 2018-12-03 2018-12-03 Preparation method of solvent type PU flocking adhesive Active CN109536115B (en)

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CN113025211A (en) * 2021-03-01 2021-06-25 陈猛 TPU glue for jean groove bottom flocking and production process thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0531437A (en) * 1991-08-02 1993-02-09 Toyoda Gosei Co Ltd Electrostatically flocked product
CN101012362A (en) * 2007-01-29 2007-08-08 上海九元石油化工有限公司 Method of preparing polyurethane flocking rubber for automobile sealing strip
KR100786584B1 (en) * 2005-01-18 2007-12-21 롬 앤드 하아스 컴패니 Water-based flock adhesives for thermoplastic substrates
CN102516919A (en) * 2011-11-26 2012-06-27 上海三恩化工有限公司 Preparation method of monocomponent polyurethane flocking adhesive

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0531437A (en) * 1991-08-02 1993-02-09 Toyoda Gosei Co Ltd Electrostatically flocked product
KR100786584B1 (en) * 2005-01-18 2007-12-21 롬 앤드 하아스 컴패니 Water-based flock adhesives for thermoplastic substrates
CN101012362A (en) * 2007-01-29 2007-08-08 上海九元石油化工有限公司 Method of preparing polyurethane flocking rubber for automobile sealing strip
CN102516919A (en) * 2011-11-26 2012-06-27 上海三恩化工有限公司 Preparation method of monocomponent polyurethane flocking adhesive

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