CN106749941A - The preparation method of polyurethane polyacrylate glued membrane - Google Patents

The preparation method of polyurethane polyacrylate glued membrane Download PDF

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Publication number
CN106749941A
CN106749941A CN201611156762.6A CN201611156762A CN106749941A CN 106749941 A CN106749941 A CN 106749941A CN 201611156762 A CN201611156762 A CN 201611156762A CN 106749941 A CN106749941 A CN 106749941A
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degree
preparation
aqueous polyurethane
glued membrane
emulsion
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Inventor
王耀斌
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Shaanxi Gaoxin Industry Co Ltd
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Shaanxi Gaoxin Industry Co Ltd
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Priority to CN201611156762.6A priority Critical patent/CN106749941A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4825—Polyethers containing two hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67—Unsaturated compounds having active hydrogen
    • C08G18/671—Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2351/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The preparation method of polyurethane polyacrylate glued membrane of the present invention is related to polyurethane industrial field, and in particular to the preparation method of polyurethane polyacrylate glued membrane, comprises the following steps：The preparation of aqueous polyurethane emulsion, by polyether Glycols, dihydromethyl propionic acid and the pyrrolidones of solvent N methyl 2 addition four-hole boiling flask, is warmed up to 60 degree, IPDI and catalyst dibutyl tin dilaurate, constant temperature is added to stir 4 h, be then warmed up to 80 85 degree, react 2 h, 60 degree are cooled to, 5h is reacted, 40 degree are cooled to, triethylamine is added dropwise to be neutralized, then add water and disperseed, while carrying out chain extension with ethylenediamine, prepare aqueous polyurethane emulsion；The present invention is simple to operate, convenient operation, and can guarantee that product quality, enhances product performance, and saves production cost, reducing energy consumption.

Description

The preparation method of polyurethane-polyacrylate glued membrane
Technical field
The present invention relates to polyurethane industrial field, and in particular to the preparation method of polyurethane-polyacrylate glued membrane.
Background technology
In recent years, with aqueous polyurethane（WPU）Substitution solvent borne polyurethane（PU）Research increasingly by people Concern.There is WPU films good physical and mechanical properties, excellent cold resistance, alkali resistance, elasticity and soft durometer to vary with temperature not Too big the advantages of, but its heat-resisting quantity, tack and water resistance are poor, limit its range of application.Compared with PU, polyacrylic acid Ester (PA) emulsion has the performances such as excellent weatherability, water resistance and gloss retention, but hardness is big, solvent resistant, i.e. Pu do not exist with PA There is complementarity in practical application performance.
According to these features, researcher uses physics blending method, segment copolymerization method, core-shell copolymerized method, grafting copolymerization process With the method such as interpenetrating polymer networks copolymerization method, WPU is modified with acrylic resin, modified aqueous polyurethane-poly- Acrylate (WPUA) emulsion has the advantage of Pu and PA concurrently, combines high-wearing feature and good mechanical performance and third of WPU Olefin(e) acid ester good weatherability and water resistance, make WPU glued membranes performance be improved significantly, be described as " the aqueous poly- ammonia of the third generation Ester ", is also one of most active and most promising direction.
The content of the invention
It is a kind of simple to operate present invention aim at providing, convenient operation, and product quality is can guarantee that, improve product Can, save production cost, the preparation method of the polyurethane-polyacrylate glued membrane of reducing energy consumption.
The preparation method of polyurethane-polyacrylate glued membrane of the present invention, comprises the following steps：
The first step, the preparation of aqueous polyurethane emulsion
By in polyether Glycols, dihydromethyl propionic acid and Solvents N-methyl -2-Pyrrolidone addition four-hole boiling flask, 60 are warmed up to Degree, adds IPDI and catalyst dibutyl tin dilaurate, constant temperature to stir 4 h, be then warmed up to 80-85 Degree, reacts 2 h, cools to 60 degree, reacts 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and then adds water and is disperseed, Chain extension is carried out with ethylenediamine simultaneously, aqueous polyurethane emulsion is prepared；
Second step, the preparation of aqueous polyurethane-polyacrylate emulsion
In above-mentioned aqueous polyurethane emulsion preparation process, 60 degree are cooled to, add hydroxyethyl methacrylate, continue to react 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and adds butyl acrylate and e pioic acid methyl ester monomer, then slowly add water into Row dispersion, adds ethylenediamine, is subsequently adding initiator, is warming up to 60 degree, and insulated and stirred 4h, reaction terminates, and obtains aqueous poly- ammonia Ester-polyacrylate emulsion；
3rd step, the preparation of aqueous polyurethane-polyacrylic acid glued membrane
Aqueous polyurethane-polyacrylic emulsion is poured on polyfluortetraethylene plate, and 2-3d is stood under normal temperature, and baking oven is put into after drying In, 48 h are dried under 60 degree, obtain aqueous polyurethane-polyacrylic acid glued membrane.
Preferably, catalyst is dibutyl tin dilaurate.
Preferably, initiator is azodiisobutyronitrile.
The present invention is simple to operate, convenient operation, and can guarantee that product quality, enhances product performance, and saves production cost, drop Low energy consumption.
Specific embodiment
Embodiment one：
The preparation method of polyurethane-polyacrylate glued membrane of the present invention, comprises the following steps：
The first step, the preparation of aqueous polyurethane emulsion
By in polyether Glycols, dihydromethyl propionic acid and Solvents N-methyl -2-Pyrrolidone addition four-hole boiling flask, 60 are warmed up to Degree, adds IPDI and catalyst dibutyl tin dilaurate, constant temperature to stir 4 h, be then warmed up to 80-85 Degree, reacts 2 h, cools to 60 degree, reacts 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and then adds water and is disperseed, Chain extension is carried out with ethylenediamine simultaneously, aqueous polyurethane emulsion is prepared；
Second step, the preparation of aqueous polyurethane-polyacrylate emulsion
In above-mentioned aqueous polyurethane emulsion preparation process, 60 degree are cooled to, add hydroxyethyl methacrylate, continue to react 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and adds butyl acrylate and e pioic acid methyl ester monomer, then slowly add water into Row dispersion, adds ethylenediamine, is subsequently adding initiator, is warming up to 60 degree, and insulated and stirred 4h, reaction terminates, and obtains aqueous poly- ammonia Ester-polyacrylate emulsion；
3rd step, the preparation of aqueous polyurethane-polyacrylic acid glued membrane
Aqueous polyurethane-polyacrylic emulsion is poured on polyfluortetraethylene plate, and 2-3d is stood under normal temperature, and baking oven is put into after drying In, 48 h are dried under 60 degree, obtain aqueous polyurethane-polyacrylic acid glued membrane.
Embodiment two：
The preparation method of polyurethane-polyacrylate glued membrane of the present invention, comprises the following steps：
The first step, the preparation of aqueous polyurethane emulsion
By in polyether Glycols, dihydromethyl propionic acid and Solvents N-methyl -2-Pyrrolidone addition four-hole boiling flask, 60 are warmed up to Degree, adds IPDI and catalyst dibutyl tin dilaurate, constant temperature to stir 4 h, be then warmed up to 80-85 Degree, reacts 2 h, cools to 60 degree, reacts 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and then adds water and is disperseed, Chain extension is carried out with ethylenediamine simultaneously, aqueous polyurethane emulsion is prepared；
Second step, the preparation of aqueous polyurethane-polyacrylate emulsion
In above-mentioned aqueous polyurethane emulsion preparation process, 60 degree are cooled to, add hydroxyethyl methacrylate, continue to react 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and adds butyl acrylate and e pioic acid methyl ester monomer, then slowly add water into Row dispersion, adds ethylenediamine, is subsequently adding initiator, is warming up to 60 degree, and insulated and stirred 4h, reaction terminates, and obtains aqueous poly- ammonia Ester-polyacrylate emulsion；
3rd step, the preparation of aqueous polyurethane-polyacrylic acid glued membrane
Aqueous polyurethane-polyacrylic emulsion is poured on polyfluortetraethylene plate, and 2-3d is stood under normal temperature, and baking oven is put into after drying In, 48 h are dried under 60 degree, obtain aqueous polyurethane-polyacrylic acid glued membrane.
Catalyst is dibutyl tin dilaurate.
Embodiment three：
The preparation method of polyurethane-polyacrylate glued membrane of the present invention, comprises the following steps：
The first step, the preparation of aqueous polyurethane emulsion
By in polyether Glycols, dihydromethyl propionic acid and Solvents N-methyl -2-Pyrrolidone addition four-hole boiling flask, 60 are warmed up to Degree, adds IPDI and catalyst dibutyl tin dilaurate, constant temperature to stir 4 h, be then warmed up to 80-85 Degree, reacts 2 h, cools to 60 degree, reacts 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and then adds water and is disperseed, Chain extension is carried out with ethylenediamine simultaneously, aqueous polyurethane emulsion is prepared；
Second step, the preparation of aqueous polyurethane-polyacrylate emulsion
In above-mentioned aqueous polyurethane emulsion preparation process, 60 degree are cooled to, add hydroxyethyl methacrylate, continue to react 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and adds butyl acrylate and e pioic acid methyl ester monomer, then slowly add water into Row dispersion, adds ethylenediamine, is subsequently adding initiator, is warming up to 60 degree, and insulated and stirred 4h, reaction terminates, and obtains aqueous poly- ammonia Ester-polyacrylate emulsion；
3rd step, the preparation of aqueous polyurethane-polyacrylic acid glued membrane
Aqueous polyurethane-polyacrylic emulsion is poured on polyfluortetraethylene plate, and 2-3d is stood under normal temperature, and baking oven is put into after drying In, 48 h are dried under 60 degree, obtain aqueous polyurethane-polyacrylic acid glued membrane.
Catalyst is dibutyl tin dilaurate.
Initiator is azodiisobutyronitrile.
The present invention is simple to operate, convenient operation, and can guarantee that product quality, enhances product performance, and saves production cost, drop Low energy consumption.

Claims (3)

1. a kind of preparation method of polyurethane-polyacrylate glued membrane, it is characterised in that comprise the following steps：
The first step, the preparation of aqueous polyurethane emulsion
By in polyether Glycols, dihydromethyl propionic acid and Solvents N-methyl -2-Pyrrolidone addition four-hole boiling flask, 60 are warmed up to Degree, adds IPDI and catalyst dibutyl tin dilaurate, constant temperature to stir 4 h, be then warmed up to 80-85 Degree, reacts 2 h, cools to 60 degree, reacts 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and then adds water and is disperseed, Chain extension is carried out with ethylenediamine simultaneously, aqueous polyurethane emulsion is prepared；
Second step, the preparation of aqueous polyurethane-polyacrylate emulsion
In above-mentioned aqueous polyurethane emulsion preparation process, 60 degree are cooled to, add hydroxyethyl methacrylate, continue to react 5h, is cooled to 40 degree, triethylamine is added dropwise and is neutralized, and adds butyl acrylate and e pioic acid methyl ester monomer, then slowly add water into Row dispersion, adds ethylenediamine, is subsequently adding initiator, is warming up to 60 degree, and insulated and stirred 4h, reaction terminates, and obtains aqueous poly- ammonia Ester-polyacrylate emulsion；
3rd step, the preparation of aqueous polyurethane-polyacrylic acid glued membrane
Aqueous polyurethane-polyacrylic emulsion is poured on polyfluortetraethylene plate, and 2-3d is stood under normal temperature, and baking oven is put into after drying In, 48 h are dried under 60 degree, obtain aqueous polyurethane-polyacrylic acid glued membrane.
2. the preparation method of polyurethane-polyacrylate glued membrane as claimed in claim 1, it is characterised in that the catalyst is Dibutyl tin dilaurate.
3. the preparation method of polyurethane-polyacrylate glued membrane as claimed in claim 2, it is characterised in that the initiator is Azodiisobutyronitrile.
CN201611156762.6A 2016-12-15 2016-12-15 The preparation method of polyurethane polyacrylate glued membrane Pending CN106749941A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107385924A (en) * 2017-07-17 2017-11-24 江苏兴龙光电发展有限公司 A kind of cable coating and its preparation technology
CN112680094A (en) * 2020-12-28 2021-04-20 成都启铎弗涂料科技有限公司 Preparation method of waterborne polyurethane acrylate waterborne paint

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107385924A (en) * 2017-07-17 2017-11-24 江苏兴龙光电发展有限公司 A kind of cable coating and its preparation technology
CN112680094A (en) * 2020-12-28 2021-04-20 成都启铎弗涂料科技有限公司 Preparation method of waterborne polyurethane acrylate waterborne paint

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