CN107760250A - A kind of preparation method of solvent-free dual-component polyurethane boiling adhesive - Google Patents
A kind of preparation method of solvent-free dual-component polyurethane boiling adhesive Download PDFInfo
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- CN107760250A CN107760250A CN201711053804.8A CN201711053804A CN107760250A CN 107760250 A CN107760250 A CN 107760250A CN 201711053804 A CN201711053804 A CN 201711053804A CN 107760250 A CN107760250 A CN 107760250A
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- 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
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- 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
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- 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
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/791—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups
- C08G18/792—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups formed by oligomerisation of aliphatic and/or cycloaliphatic isocyanates or isothiocyanates
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
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- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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 discloses a kind of preparation method of solvent-free dual-component polyurethane boiling adhesive, this solvent-free dual-component polyurethane boiling adhesive is made up of A glue and B glue, the preparation, the preparation of B glue and the preparation of object of A glue are disclosed, the advantages of this novel solvent-free dual-component polyurethane boiling adhesive：Have excellent water boiling resistance performance and peel strength concurrently.The advantages of this preparation method：Preparation process is simple, cheap and pollution-free.
Description
Technical field
The present invention relates to a kind of preparation method of solvent-free dual-component polyurethane boiling adhesive, belong to material and ground with food
Study carefully field.
Background technology
With the compound comparison of conventional dry, solvent-free be compounded in reduces cost, improves product quality, environmental protection, production peace
There are many advantages with stable etc. entirely.Solvent-free compound adhesive used is free of solvent, thus packing material is not polluted, more
Suitable for packaging for foodstuff.But common solventless adhesive can not meet the market demand, the especially packaging bag of boiling type
Special glue product.Using the packaging bag that common glue is made, its peel strength can be greatly lowered after high temperature boiling, seriously
When even can produce delamination, directly affect to the normal use of flexible package product.It is insufficient existing for existing product in order to overcome, it is full
The new demand in sufficient market, so as to develop a kind of Solvent-free double-constituent polyurethane compound adhesive of high temperature resistant boiling.
The content of the invention
It is described without molten it is an object of the invention to provide a kind of preparation method of solvent-free dual-component polyurethane boiling adhesive
Agent dual-component polyurethane boiling adhesive, is made up of, its preparation method A glue and B glue：
a：The preparation of A glue：
The PPG (degree of functionality of hydroxyl is 2), 350g liquefied mdis that 350g molecular weight is 1000~2000 are taken respectively
(NCO%=33.5) and 100g hexamethylene diisocyanate trimers (NCO%=21.7~22.2) are in four-hole boiling flask, rise
Temperature is to 100~120 DEG C, under the conditions of vacuum -0.1MPa, is dehydrated 2 hours, detection architecture water content less than 0.05% to be qualified, drop
Temperature produces A glue to 40 DEG C.
b：The preparation of B glue：
Take respectively 120g polyethylene glycol, 240g 1,3 butylene glycols, 120g adipic acids, 160g DMIPs in
In 1000mL four-hole boiling flasks, it is added dropwise after 0.1~0.25g tetrabutyl titanate catalysts, stirs and be to slowly warm up to 160 DEG C, this
Shi Fanying water outlets, then it is to slowly warm up to 240 DEG C and is incubated two hours, acid value is surveyed in now sampling, if acid value is less than 15mg KOH/
G, then esterification terminate, then temperature be 220~230 DEG C and pressure be under conditions of -0.1Mpa under to vacuumize 5 small
When, obtain the PEPA of acid value≤1mg KOH/g and hydroxyl value for 50 ± 5mg KOH/g；Take 200g obtained above poly-
Ester polyol is with PPG (degree of functionality of hydroxyl is 4.5) and 35g molecular weight that 200g molecular weight is 400~700
2800~3500 end hydroxy butadiene mixing, vacuum dehydration to content of water in system is less than 0.05% under the conditions of 120 DEG C, drop
Temperature is to 40 DEG C, as B glue.
c：The preparation of Solvent-free double-constituent polyurethane compound adhesive：A glue and B glue are with 10:7 are mixed to get no-solvent polyurethane glue
Stick.
Further, in step a, the molecular weight of PPG is 1000~2000；PPG, liquefied mdi and
The mass ratio of hexamethylene diisocyanate trimer is 1:1:0.4.
Further, in stepb, the mass ratio of polyethylene glycol, 1,3-BDO, adipic acid and DMIP
For 2：4：2：2.8；The molecular weight of PPG is 400~700；The molecular weight of end hydroxy butadiene is 2800~3500；
The mass ratio of PEPA, PPG and end hydroxy butadiene is 5.7:6:1.
The advantages of this novel solvent-free dual-component polyurethane boiling adhesive：Have excellent water boiling resistance performance and stripping concurrently
Intensity.
The advantages of this preparation method：Preparation process is simple, cheap and pollution-free.
Embodiment
Presently in connection with specific embodiment, the present invention will be further described, following examples be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1：
The step of preparing Solvent-free double-constituent polyurethane compound adhesive is as follows：
(1) synthesis of A glue, is comprised the following steps that：PPG (the hydroxyl that 350g molecular weight is 1000~2000 is taken respectively
The degree of functionality of base for 2), 350g liquefied mdis (NCO%=33.5) and 100g hexamethylene diisocyanate trimers (NCO%=
21.7~22.2) 100~120 DEG C are warming up in four-hole boiling flask, under the conditions of vacuum -0.1MPa, is dehydrated 2 hours, detection architecture
Water content is qualified less than 0.05%, is cooled to 40 DEG C, produces A glue；
(2) synthesis of B glue, is comprised the following steps that：Take respectively 120g polyethylene glycol, 240g 1,3 butylene glycols, 120g oneself two
Acid, 160g DMIPs are added dropwise after 0.1~0.25g tetrabutyl titanate catalysts in 1000mL four-hole boiling flasks,
Stir and be to slowly warm up to 160 DEG C, now react water outlet, be then to slowly warm up to 240 DEG C and be incubated two hours, now sampling is surveyed
Acid value, if acid value is less than 15mg KOH/g, esterification terminates, then temperature be 220~230 DEG C and pressure for-
Vacuumized under under conditions of 0.1Mpa 5 hours, obtain the polyester of acid value≤1mg KOH/g and hydroxyl value for 50 ± 5mg KOH/g
Polyalcohol；Take the PPG (official of hydroxyl that 200g PEPAs obtained above and 200g molecular weight are 400~700
3) and end hydroxy butadiene that 35g molecular weight be 2800~3500 mixes energy degree is, and vacuum dehydration is extremely under the conditions of 120 DEG C
Content of water in system is less than 0.05%, is cooled to 40 DEG C, as B glue；
(3) Solvent-free double-constituent polyurethane compound adhesive is prepared：A glue and B glue are with 10:7 are mixed to get no-solvent polyurethane glue
Stick.
Obtained solvent-free polyurethane adhesive is added in the glue spreading system of solvent-free laminating machine, spread is
2.0g/m2, using aluminium film and RCPP films as base material, aluminium plastic composite material is prepared, further tests its intensity after curing,
Intensity is 6.5 (N.15mm), and the aluminium plastic composite material for illustrating to obtain through solvent-free polyurethane adhesive possesses excellent after solidification
Different peel strength.
Embodiment 2：
The preparation process of Solvent-free double-constituent polyurethane compound adhesive is identical with embodiment one.
Obtained solvent-free polyurethane adhesive is added in the glue spreading system of solvent-free laminating machine, spread is
2.0g/m2, using aluminium film and RCPP films as base material, aluminium plastic composite material is prepared, further cures and old by 60 DEG C
Its intensity is tested after changing 7 days, intensity is 5.8 (N.15mm), illustrates to obtain through solvent-free polyurethane adhesive plastic-aluminum combined
Material possesses good ageing resistace.
Embodiment 3：
The preparation process of Solvent-free double-constituent polyurethane compound adhesive is identical with embodiment one.
Obtained solvent-free polyurethane adhesive is added in the glue spreading system of solvent-free laminating machine, spread is
2.0g/m2, using aluminium film and RCPP films as base material, aluminium plastic composite material is prepared, further cures and passes through 100 DEG C of water
Its intensity is tested after boiling, intensity is 5.0 (N.15mm), illustrates the aluminium plastic composite material obtained through solvent-free polyurethane adhesive
Possesses good water boiling resistance performance.
The Solvent-free double-constituent polyurethane compound adhesive that the present invention is prepared, preparation process is simple, inexpensively.
Claims (3)
1. a kind of preparation method of solvent-free dual-component polyurethane boiling adhesive, it is characterized in that：The solvent-free two-component is gathered
Urethane boiling adhesive, is made up of, its preparation method A glue and B glue：
a：The preparation of A glue：
The PPG (degree of functionality of hydroxyl is 2), 350g liquefied mdis that 350g molecular weight is 1000~2000 are taken respectively
(NCO%=33.5) and 100g hexamethylene diisocyanate trimers (NCO%=21.7~22.2) are in four-hole boiling flask, rise
Temperature is to 100~120 DEG C, under the conditions of vacuum -0.1MPa, is dehydrated 2 hours, detection architecture water content less than 0.05% to be qualified, drop
Temperature produces A glue to 40 DEG C.
b：The preparation of B glue：
Take respectively 120g polyethylene glycol, 240g 1,3 butylene glycols, 120g adipic acids, 160g DMIPs in
In 1000mL four-hole boiling flasks, it is added dropwise after 0.1~0.25g tetrabutyl titanate catalysts, stirs and be to slowly warm up to 160 DEG C, this
Shi Fanying water outlets, then it is to slowly warm up to 240 DEG C and is incubated two hours, acid value is surveyed in now sampling, if acid value is less than 15mg KOH/
G, then esterification terminate, then temperature be 220~230 DEG C and pressure be under conditions of -0.1Mpa under to vacuumize 5 small
When, obtain the PEPA of acid value≤1mgKOH/g and hydroxyl value for 50 ± 5mg KOH/g；Take 200g polyester obtained above
Polyalcohol is with PPG (degree of functionality of hydroxyl is 4.5) and 35g molecular weight that 200g molecular weight is 400~700
2800~3500 end hydroxy butadiene mixing, vacuum dehydration to content of water in system is less than 0.05% under the conditions of 120 DEG C, drop
Temperature is to 40 DEG C, as B glue.
c：The preparation of Solvent-free double-constituent polyurethane compound adhesive：A glue and B glue are with 10:7 to be mixed to get no-solvent polyurethane gluing
Agent.
2. the preparation method of solvent-free dual-component polyurethane boiling adhesive according to claim 1, it is characterized in that：In step
In a, the molecular weight of PPG is 1000~2000；PPG, liquefied mdi and hexamethylene diisocyanate trimerization
The mass ratio of body is 1:1:0.4.
3. the preparation method of solvent-free dual-component polyurethane boiling adhesive according to claim 1, it is characterized in that：In step
In b, polyethylene glycol, 1,3-BDO, the mass ratio of adipic acid and DMIP are 2：4：2：2.8；Polyether polyols
The molecular weight of alcohol is 400~700；The molecular weight of end hydroxy butadiene is 2800~3500；PEPA, PPG
Mass ratio with end hydroxy butadiene is 5.7:6:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711053804.8A CN107760250A (en) | 2017-10-31 | 2017-10-31 | A kind of preparation method of solvent-free dual-component polyurethane boiling adhesive |
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| CN201711053804.8A CN107760250A (en) | 2017-10-31 | 2017-10-31 | A kind of preparation method of solvent-free dual-component polyurethane boiling adhesive |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110475835A (en) * | 2017-04-06 | 2019-11-19 | Dic株式会社 | Curing agent, two-component type bonding agent, stacked film and the package body of two-component type bonding agent |
-
2017
- 2017-10-31 CN CN201711053804.8A patent/CN107760250A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110475835A (en) * | 2017-04-06 | 2019-11-19 | Dic株式会社 | Curing agent, two-component type bonding agent, stacked film and the package body of two-component type bonding agent |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180306 |
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| WD01 | Invention patent application deemed withdrawn after publication |