CN108300404A - Pre- gluing of a kind of iron overlay film dedicated solvent type mono-component polyurethane and preparation method thereof - Google Patents
Pre- gluing of a kind of iron overlay film dedicated solvent type mono-component polyurethane and preparation method thereof Download PDFInfo
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- CN108300404A CN108300404A CN201810139601.9A CN201810139601A CN108300404A CN 108300404 A CN108300404 A CN 108300404A CN 201810139601 A CN201810139601 A CN 201810139601A CN 108300404 A CN108300404 A CN 108300404A
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- component polyurethane
- gluing
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- solvent type
- overlay film
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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
- C09J175/06—Polyurethanes from polyesters
-
- 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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
- C08G18/4247—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids
- C08G18/425—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids the polyols containing one or two ether 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
- C08G18/70—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
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
-
- 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
-
- 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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- 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)
- Laminated Bodies (AREA)
Abstract
The invention discloses pre- gluings of a kind of iron overlay film dedicated solvent type mono-component polyurethane and preparation method thereof, prepare the pre- gluing of mono-component polyurethane by polyester polyol, curing agent, and disclose specific preparation method：Adhesive force is good to base material for the pre- gluing of this Novel iron overlay film dedicated solvent type mono-component polyurethane, and monocomponent adhesive can effectively overcome traditional solvent-borne two component adhesive hardening time very long defect, the parameter of preparation process is easily controllable, preparation process environmental protection.
Description
Technical field
The present invention relates to pre- gluings of a kind of iron overlay film dedicated solvent type mono-component polyurethane and preparation method thereof, belong to poly- ammonia
Ester gum sticks agent material research field.
Background technology
The pre- gluing of one-component solvent borne have it is easy for construction, be applicable in workpiece material diversification, condition of cure limitation less, moisture-proof
Property good, the destrabilizing moment and average high advantage of dismounting force moment, the locking performance of base material, and then the peace of product has been effectively ensured in this
Full reliability also just has better guarantee.In order to meet the requirement in market, to develop Novel iron overlay film dedicated solvent type
The pre- gluing of mono-component polyurethane.
Invention content
The object of the present invention is to provide pre- gluings of a kind of iron overlay film dedicated solvent type mono-component polyurethane and preparation method thereof.
A kind of pre- gluing of iron overlay film dedicated solvent type mono-component polyurethane, it is characterised in that：Step is prepared by the following procedure to obtain
：
Step 1, the preparation of polyester polyol：
Take 78~82g adipic acids, 400~410g M-phthalic acids and 445~450g diethylene glycol (DEG)s in tetra- mouthfuls of 1000mL respectively
In flask, 0.1~0.15g butyl titanates are added as catalyst, reaction system needs nitrogen protection.When reaction temperature reaches
At 160 ± 5 DEG C, then reaction system starts to be discharged, and needs control heating rate at this time, will when reaction temperature reaches 235 ± 5 DEG C
Heating is changed to keeping warm mode, soaking time 3h.After soaking time, acid value is surveyed in sampling, if acid value is less than 15mg KOH/g,
0.1g L-56 are then added dropwise and controlled at 230~240 DEG C and pressure to be vacuumized 2.5 hours under conditions of -0.1Mpa,
Acid value≤1mg KOH/g and hydroxyl value are obtained as the polyester polyol of 30 ± 5mg KOH/g.
Step 2, the preparation of curing agent：
Take 375~380g TDI, 250~253g MDI-50 and 255~258g ethyl acetate in tetra- mouthfuls of burnings of 1000mL respectively
In bottle, when being warming up to 45 DEG C, 30~32g trimethylolpropanes is added, is at this time exothermic reaction, suitable control is needed to cool down,
30min and then 67~68g trimethylolpropanes are added and controlled at 78 DEG C, curing agent can be obtained after insulation reaction 3h.
Step 3, the pre-gelatinized preparation of mono-component polyurethane：
Take 200~205g polyester polyol, 8~9g curing agent and 150~153g ethyl acetate in tetra- mouthfuls of 1000mL respectively
It in flask, is warming up to 85 DEG C and reacts 5h, the pre- gluing of mono-component polyurethane can be obtained by then adding 500~510g ethyl acetate.
Further, in step 1, adipic acid 78g, M-phthalic acid 400g, diethylene glycol (DEG) 445g.
Further, in step 2, TDI 375g, MDI-50 250g, ethyl acetate 255g.
Further, in step 3, polyester polyol 200g, curing agent 8g, ethyl acetate 150g.
The pre-gelatinized advantage of this Novel iron overlay film dedicated solvent type mono-component polyurethane：
Adhesive force is good to base material for this adhesive, and monocomponent adhesive can effectively overcome traditional solvent-borne bi-component
Adhesive hardening time very long defect.
The advantages of this preparation method：
The parameter of preparation process is easily controllable, preparation process environmental protection.
Specific implementation mode
Presently in connection with specific embodiment, the present invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment one：
A kind of pre-gelatinized preparation method of iron overlay film dedicated solvent type mono-component polyurethane is as follows：
Step 1, the preparation of polyester polyol：
It takes 78g adipic acids, 400g M-phthalic acids and 445g diethylene glycol (DEG)s in 1000mL four-hole boiling flasks respectively, adds
0.1g butyl titanates need nitrogen protection as catalyst, reaction system, when reaction temperature reaches 160 DEG C, then reaction system
Start to be discharged, needs control heating rate to will heat up when reaction temperature reaches 235 DEG C and be changed to keeping warm mode at this time, soaking time
For 3h.After soaking time, acid value is surveyed in sampling, if acid value is less than 15mg KOH/g, 0.1g L-56 and control temperature is added dropwise
It is vacuumized 2.5 hours under conditions of being -0.1Mpa for 230~240 DEG C and pressure, obtains acid value≤1mg KOH/g and hydroxyl
Value is the polyester polyol of 30 ± 5mg KOH/g.
Step 2, the preparation of curing agent：
It takes 375g TDI, 250g MDI-50 and 255g ethyl acetate in 1000mL four-hole boiling flasks respectively, waits being warming up to 45
DEG C when, be added 30g trimethylolpropanes, be at this time exothermic reaction, suitable control needed to cool down, 30min and then be added 67g tri-
Hydroxymethyl-propane and controlled at 78 DEG C, curing agent can be obtained after insulation reaction 3h.
Step 3, the pre-gelatinized preparation of mono-component polyurethane：
It takes 200g polyester polyol, 8g curing agent and 150g ethyl acetate in 1000mL four-hole boiling flasks respectively, is warming up to
85 DEG C and 5h is reacted, the pre- gluing of mono-component polyurethane can be obtained by then adding 500g ethyl acetate.
The pre- gluing of solvent type mono-component polyurethane obtained is added in the glue spreading system of solvent type laminating machine, spread
For 5.0g/m2, PET/ compound polyurethane materials are prepared using PET film as base material in working concentration 32%, then at 140 DEG C
Under conditions of PET/ compound polyurethane materials are pasted onto iron plate surface, after waiting for that temperature cools down, it is found that PET is fully adhered to
There is not tacky phenomenon on iron sheet surface, and peel strength is 25N, and the peel strength of the type product is 20N, explanation at present
This pre- gluing of solvent type mono-component polyurethane can be used successfully to the application of iron overlay film.
Embodiment two：
The pre-gelatinized preparation process of solvent type mono-component polyurethane is identical as embodiment one.
The pre- gluing of solvent type mono-component polyurethane obtained is added in the glue spreading system of solvent type laminating machine, spread
For 5.0g/m2, PET/ compound polyurethane materials are prepared using PET film as base material in working concentration 32%, then at 140 DEG C
Under conditions of PET/ compound polyurethane materials are pasted onto iron plate surface, the composite material is put into 200 DEG C of baking oven at this time
20min has found PET film not delamination after taking-up, and still can keep after cooling down the good adhesive strength, intensity to be
23N illustrates that this kind of glue has good high-temperature stability.
The preparation process environmental protection for the solvent borne polyurethane adhesive that the present invention is prepared, this adhesive is to the attached of base material
Put forth effort good, and can effectively overcome traditional solvent-borne two component adhesive hardening time very long defect.
Claims (4)
1. a kind of pre- gluing of iron overlay film dedicated solvent type mono-component polyurethane, it is characterised in that：Preparation method is as follows：
Step 1, the preparation of polyester polyol：
Take 78~82g adipic acids, 400~410g M-phthalic acids and 445~450g diethylene glycol (DEG)s in 1000mL four-hole boiling flasks respectively
In, 0.1~0.15g butyl titanates are added as catalyst, and reaction system needs nitrogen protection.When reaction temperature reaches 160
At ± 5 DEG C, then reaction system starts to be discharged, and control heating rate is needed to will heat up when reaction temperature reaches 235 ± 5 DEG C at this time
It is changed to keeping warm mode, soaking time 3h.After soaking time, acid value is surveyed in sampling, if acid value is less than 15mg KOH/g, is dripped
Add 0.1g L-56 and controlled at 230~240 DEG C and pressure to be vacuumized 2.5 hours under conditions of -0.1Mpa, obtains
Acid value≤1mgKOH/g and the polyester polyol that hydroxyl value is 30 ± 5mg KOH/g.
Step 2, the preparation of curing agent：
Take 375~380g TDI, 250~253g MDI-50 and 255~258g ethyl acetate in 1000mL four-hole boiling flasks respectively
In, when being warming up to 45 DEG C, 30~32g trimethylolpropanes are added, is at this time exothermic reaction, needs suitable control to cool down, 30min
And then 67~68g trimethylolpropanes are added and controlled at 78 DEG C, curing agent can be obtained after insulation reaction 3h.
Step 3, the pre-gelatinized preparation of mono-component polyurethane：
Take 200~205g polyester polyol, 8~9g curing agent and 150~153g ethyl acetate in 1000mL four-hole boiling flasks respectively
In, it is warming up to 85 DEG C and reacts 5h, the pre- gluing of mono-component polyurethane can be obtained by then adding 500~510g ethyl acetate.
2. the pre- gluing of iron overlay film dedicated solvent type mono-component polyurethane according to claim 1, it is characterised in that：In step 1
In, adipic acid 78g, M-phthalic acid 400g, diethylene glycol (DEG) 445g.
3. the pre- gluing of iron overlay film dedicated solvent type mono-component polyurethane according to claim 1, it is characterised in that：In step 2,
TDI is 375g, MDI-50 250g, ethyl acetate 255g.
4. the pre- gluing of iron overlay film dedicated solvent type mono-component polyurethane according to claim 1, it is characterised in that：In step 3
In, polyester polyol 200g, curing agent 8g, ethyl acetate 150g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810139601.9A CN108300404A (en) | 2018-02-11 | 2018-02-11 | Pre- gluing of a kind of iron overlay film dedicated solvent type mono-component polyurethane and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810139601.9A CN108300404A (en) | 2018-02-11 | 2018-02-11 | Pre- gluing of a kind of iron overlay film dedicated solvent type mono-component polyurethane and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN108300404A true CN108300404A (en) | 2018-07-20 |
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ID=62864949
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810139601.9A Pending CN108300404A (en) | 2018-02-11 | 2018-02-11 | Pre- gluing of a kind of iron overlay film dedicated solvent type mono-component polyurethane and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139017A (en) * | 2020-01-07 | 2020-05-12 | 广东东方一哥新材料股份有限公司 | Single-component polyurethane primer and preparation method thereof |
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| EP1607424A1 (en) * | 2004-06-14 | 2005-12-21 | Bayer MaterialScience LLC | A method of direct-to-metal coating |
| CN1624067A (en) * | 2004-10-29 | 2005-06-08 | 东华大学 | Dry type compound polyurethane adhesive and its preparation method |
| CN1629245A (en) * | 2004-10-29 | 2005-06-22 | 东华大学 | Boiling resistant polyurethane adhesive and method for preparing same |
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| CN111139017A (en) * | 2020-01-07 | 2020-05-12 | 广东东方一哥新材料股份有限公司 | Single-component polyurethane primer and preparation method thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20191218 Address after: 210000 room 298, building B, No. 606, ningliu Road, Changlu street, Jiangbei new district, Nanjing City, Jiangsu Province Applicant after: Nanjing xuansi New Material Co.,Ltd. Address before: 213200 No. 28, Yang Chemical Industrial Park, Jintan District, Jiangsu, Changzhou Applicant before: JIANGSU LIHE ADHESIVE Co.,Ltd. |
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| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180720 |