CN103030771A - Method for preparing high-transparency aqueous polyurethane emulsion - Google Patents
Method for preparing high-transparency aqueous polyurethane emulsion Download PDFInfo
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- CN103030771A CN103030771A CN2012105540736A CN201210554073A CN103030771A CN 103030771 A CN103030771 A CN 103030771A CN 2012105540736 A CN2012105540736 A CN 2012105540736A CN 201210554073 A CN201210554073 A CN 201210554073A CN 103030771 A CN103030771 A CN 103030771A
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- clear aqueous
- polyaminoester emulsion
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Abstract
The invention relates to a method for preparing a high-transparency aqueous polyurethane emulsion. The method comprises the following steps: preparing a prepolymer by taking isophorone diisocyanate (IPDI), aromatic polyester diol (PAD), 1, 4-butanediol (BDO) and dihydromethyl propionic acid (DPMA) as the raw materials; carrying out crosslinking and chain extending to the prepolymer by adopting trimethylolpropane (TMP); adding triethylamine for neutralizing the prepolymer; and adding a proper amount of deionized water for preparing the high-transparency aqueous polyurethane emulsion. The obtained aqueous polyurethane after film forming has better properties of optic transparency, cohesive property and yellowing resistance.
Description
Technical field
The present invention relates to a kind of high clear aqueous polyaminoester emulsion preparation method, belong to chemical field.
Technical background
In high-transparence composite, bonding between the base material is the key of this class matrix material of preparation, not only require binding agent to have good optical transparence, require simultaneously peel strength high, has anti-yellowing property, therefore technical requirements is higher, and adhesive for polyurethane is that a class is of many uses, the sizing agent of excellent property.In recent years based on the guiding of industry policy and to the requirement of environment protection; aqueous polyurethane is because it does not fire, the nontoxic and good good research direction that becomes polyurethane field of binding property, film-forming properties, mechanical property; its application is also more and more extensive; but it is the difficult point of Aqueous Polyurethane Adhesives that high cohesive strength is arranged when requiring it to have high transparent optical; this patent adopts the aqueous polyurethane of self-control aromatic polyester polyol preparation, has excellent high transparent, cohesiveness and yellowing resistance.
Summary of the invention
The purpose of this invention is to provide a kind of high clear aqueous polyaminoester emulsion preparation method, the aqueous polyurethane that obtains has excellent high transparent, cohesiveness and yellowing resistance.
For realizing above purpose, a kind of high clear aqueous polyaminoester emulsion preparation method of the present invention, its step is specially:
(1) prepare aromatic polyester dibasic alcohol (PAD) take poly adipate succinic acid ester (PBA) and tosic acid as raw material, temperature is that 170 ℃, rotating speed are stirring reaction 2h under the condition of 500r/min.
(2) with isophorone diisocyanate (IPDI), aromatic polyester dibasic alcohol (PAD), 1,4-butyleneglycol (BDO), dimethylol propionic acid (DPMA) prepare performed polymer for raw material, temperature is that 78 ℃, rotating speed are stirring reaction 2h under the condition of 800r/min, looks the system viscosity in the process and adds N-first class pyrrolidone (NMP).
(3) add the cross-linking modified base polyurethane prepolymer for use as of TriMethylolPropane(TMP) (TMP), reaction 1h.
(4) be cooled to 40 ℃, add the triethylamine neutralization, reaction 3min.
(5) add entry strong stirring emulsification 1h, rotating speed is 2000r/min, obtains high clear aqueous polyaminoester emulsion.
The proportioning of performed polymer raw material is in the step (1): the mol ratio of poly adipate succinic acid ester (PBA) and tosic acid is 1:1.
The proportioning of performed polymer raw material is in the step (2): the mol ratio of IPDI and PAD, BDO, DMPA is 1.25:1-1.35:1, and the consumption of BDO accounts for 3% of performed polymer quality, and the consumption of DMPA is 5% of performed polymer quality.The consumption of NMP is so that stir smooth being as the criterion.
The consumption of TriMethylolPropane(TMP) (TMP) is 2% of performed polymer quality in the step (3).
The amount of substance of triethylamine is identical with the amount of substance of DMPA in the step (4).
The consumption of the middle water of step (5) is 2 times of performed polymer total mass.
The beneficial effect that the present invention produces is, it is that raw material prepares aromatic polyester polyol (PAD) that this patent adopts poly adipate succinic acid ester (PBA) and tosic acid, then with isophorone diisocyanate (IPDI), aromatic polyester dibasic alcohol (PAD), 1,4-butyleneglycol (BDO), dimethylol propionic acid (DPMA) prepare performed polymer for raw material, adopt TriMethylolPropane(TMP) (TMP) to the crosslinked chain extension of performed polymer, make aqueous polyurethane emulsion with emulsion reaction in the warp.At first PAD is the aromatic polyester dibasic alcohol, contains the rigidity phenyl ring in the main chain, and the Regularization of molecular chain is arranged and is restricted, and the space motion of segment is obstructed, and therefore the transparency of the aqueous polyurethane emulsion of preparation is high.Secondly, owing to use IPDI as the polyisocyanates raw material, so that the aqueous polyurethane of preparation has excellent anti-yellowing property.At last, the use of TMP has excellent cohesiveness so that urethane forms the network cross-linked structure.
Embodiment
Embodiment 1:
Under rotating speed 500r/min, 170 ℃ condition, prepare aromatic polyester dibasic alcohol (PAD) take poly adipate succinic acid ester (PBA) and tosic acid as raw material, reaction 2h, the mol ratio of poly adipate succinic acid ester (PBA) and tosic acid is 1:1.Under rotating speed 800r/min, 78 ℃ condition, with isophorone diisocyanate (IPDI), aromatic polyester dibasic alcohol (PAD), 1,4-butyleneglycol (BDO), dimethylol propionic acid (DPMA) prepare performed polymer for raw material, reaction 2h, look the system viscosity in the process and add N-first class pyrrolidone (NMP), the mol ratio of IPDI and PAD, BDO, DMPA is 1.25:1, and the consumption of BDO accounts for 3% of performed polymer quality, and the consumption of DMPA is 5% of performed polymer quality.Add the cross-linking modified base polyurethane prepolymer for use as of TriMethylolPropane(TMP) (TMP), reaction 1h, the consumption of TMP is 2% of performed polymer quality.Be cooled to 40 ℃, add the triethylamine neutralization, reaction 3min, the amount of substance of triethylamine is identical with the amount of substance of DMPA.Under the condition of rotating speed 2000r/min, add entry strong stirring emulsification 1h, the consumption of water is that 2 times of performed polymer total mass obtain high clear aqueous polyaminoester emulsion.
Polyurethane laminate T stripping strength is 5.17N/25mm, and transmittance is 85%.
Embodiment 2:
Under rotating speed 500r/min, 170 ℃ condition, prepare aromatic polyester dibasic alcohol (PAD) take poly adipate succinic acid ester (PBA) and tosic acid as raw material, reaction 2h, the mol ratio of poly adipate succinic acid ester (PBA) and tosic acid is 1:1.Under rotating speed 800r/min, 78 ℃ condition, with isophorone diisocyanate (IPDI), aromatic polyester dibasic alcohol (PAD), 1,4-butyleneglycol (BDO), dimethylol propionic acid (DPMA) prepare performed polymer for raw material, reaction 2h, look the system viscosity in the process and add N-first class pyrrolidone (NMP), the mol ratio of IPDI and PAD, BDO, DMPA is 1.28:1, and the consumption of BDO accounts for 3% of performed polymer quality, and the consumption of DMPA is 5% of performed polymer quality.Add the cross-linking modified base polyurethane prepolymer for use as of TriMethylolPropane(TMP) (TMP), reaction 1h, the consumption of TMP is 2% of performed polymer quality.Be cooled to 40 ℃, add the triethylamine neutralization, reaction 3min, the amount of substance of triethylamine is identical with the amount of substance of DMPA.Under the condition of rotating speed 2000r/min, add entry strong stirring emulsification 1h, the consumption of water is that 2 times of performed polymer total mass obtain high clear aqueous polyaminoester emulsion.
Polyurethane laminate T stripping strength is 5.35N/25mm, and transmittance is 87%.
Embodiment 3:
Under rotating speed 500r/min, 170 ℃ condition, prepare aromatic polyester dibasic alcohol (PAD) take poly adipate succinic acid ester (PBA) and tosic acid as raw material, reaction 2h, the mol ratio of poly adipate succinic acid ester (PBA) and tosic acid is 1:1.Under rotating speed 800r/min, 78 ℃ condition, with isophorone diisocyanate (IPDI), aromatic polyester dibasic alcohol (PAD), 1,4-butyleneglycol (BDO), dimethylol propionic acid (DPMA) prepare performed polymer for raw material, reaction 2h, look the system viscosity in the process and add N-first class pyrrolidone (NMP), the mol ratio of IPDI and PAD, BDO, DMPA is 1.32:1, and the consumption of BDO accounts for 3% of performed polymer quality, and the consumption of DMPA is 5% of performed polymer quality.Add the cross-linking modified base polyurethane prepolymer for use as of TriMethylolPropane(TMP) (TMP), reaction 1h, the consumption of TMP is 2% of performed polymer quality.Be cooled to 40 ℃, add the triethylamine neutralization, reaction 3min, the amount of substance of triethylamine is identical with the amount of substance of DMPA.Under the condition of rotating speed 2000r/min, add entry strong stirring emulsification 1h, the consumption of water is that 2 times of performed polymer total mass obtain high clear aqueous polyaminoester emulsion.
Polyurethane laminate T stripping strength is 6.88N/25mm, and transmittance is 90%.
Embodiment 4:
Under rotating speed 500r/min, 170 ℃ condition, prepare aromatic polyester dibasic alcohol (PAD) take poly adipate succinic acid ester (PBA) and tosic acid as raw material, reaction 2h, the mol ratio of poly adipate succinic acid ester (PBA) and tosic acid is 1:1.Under rotating speed 800r/min, 78 ℃ condition, with isophorone diisocyanate (IPDI), aromatic polyester dibasic alcohol (PAD), 1,4-butyleneglycol (BDO), dimethylol propionic acid (DPMA) prepare performed polymer for raw material, reaction 2h, look the system viscosity in the process and add N-first class pyrrolidone (NMP), the mol ratio of IPDI and PAD, BDO, DMPA is 1.35:1, and the consumption of BDO accounts for 3% of performed polymer quality, and the consumption of DMPA is 5% of performed polymer quality.Add the cross-linking modified base polyurethane prepolymer for use as of TriMethylolPropane(TMP) (TMP), reaction 1h, the consumption of TMP is 2% of performed polymer quality.Be cooled to 40 ℃, add the triethylamine neutralization, reaction 3min, the amount of substance of triethylamine is identical with the amount of substance of DMPA.Under the condition of rotating speed 2000r/min, add entry strong stirring emulsification 1h, the consumption of water is that 2 times of performed polymer total mass obtain high clear aqueous polyaminoester emulsion.
Polyurethane laminate T stripping strength is 6.32N/25mm, and transmittance is 95%.
Claims (10)
1. one kind high clear aqueous polyaminoester emulsion preparation method, it is characterized in that: step is as follows:
(1) prepares aromatic polyester dibasic alcohol (PAD), 170 ℃ of stirring reaction 2h take poly adipate succinic acid ester (PBA) and tosic acid as raw material;
(2) with isophorone diisocyanate (IPDI), aromatic polyester dibasic alcohol (PAD), 1,4-butyleneglycol (BDO), dimethylol propionic acid (DPMA) prepare performed polymer for raw material, 78 ℃ of stirring reaction 2h look the system viscosity and add N-first class pyrrolidone (NMP) in the process;
(3) add the cross-linking modified base polyurethane prepolymer for use as of TriMethylolPropane(TMP) (TMP), reaction 1h;
(4) be cooled to 40 ℃, add the triethylamine neutralization, reaction 3min;
(5) add entry strong stirring emulsification 1h, obtain high clear aqueous polyaminoester emulsion.
2. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1, it is characterized in that: the proportioning of described step (1) Raw is: the mol ratio of poly adipate succinic acid ester (PBA) and tosic acid is 1:1.
3. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1 is characterized in that: mixing speed is 500r/min in the described step (1).
4. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1, it is characterized in that: the proportioning of performed polymer raw material is in the described step (2): the mol ratio of IPDI and PAD, BDO, DMPA is 1.25:1-1.35:1, the consumption of BDO accounts for 3% of performed polymer quality, and the consumption of DMPA is 5% of performed polymer quality.
5. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1 is characterized in that: the consumption of NMP is so that stir smooth being as the criterion in the described step (2).
6. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1 is characterized in that: mixing speed is 800r/min in the described step (2).
7. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1 is characterized in that: the consumption of TriMethylolPropane(TMP) (TMP) is 2% of performed polymer quality in the described step (3).
8. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1 is characterized in that: the amount of substance of triethylamine is identical with the amount of substance of DMPA in the described step (4).
9. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1 is characterized in that: the consumption of water is 2 times of performed polymer total mass in the described step (5).
10. a kind of high clear aqueous polyaminoester emulsion preparation method as claimed in claim 1 is characterized in that: mixing speed is 2000r/min in the described step (5).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892891A (en) * | 2015-06-25 | 2015-09-09 | 淄博德信联邦化学工业有限公司 | Waterborne polyurethane dispersion emulsion high in alcohol resistance and yellowing resistance and preparing method thereof |
| CN105175670A (en) * | 2015-09-28 | 2015-12-23 | 华南理工大学 | Amino resin modified waterborne polyurethane as well as preparation method and application thereof |
| CN105732944A (en) * | 2016-04-12 | 2016-07-06 | 温州市登达化工有限公司 | Preparation method of transparent polyurethane |
| CN109401714A (en) * | 2018-10-16 | 2019-03-01 | 深圳日高胶带新材料有限公司 | A kind of OCA optics adhesive and its preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101585903A (en) * | 2009-06-23 | 2009-11-25 | 丽水市优耐克水性树脂科技有限公司 | A kind of aqueous polyurethane and preparation method thereof |
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2012
- 2012-12-19 CN CN2012105540736A patent/CN103030771A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101585903A (en) * | 2009-06-23 | 2009-11-25 | 丽水市优耐克水性树脂科技有限公司 | A kind of aqueous polyurethane and preparation method thereof |
Non-Patent Citations (2)
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| 丛树枫等: "《聚氨酯涂料》", 30 September 2003, 化学工业出版社 * |
| 王毅等: "高透明水性聚氨酯胶粘剂的制备", 《广东化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892891A (en) * | 2015-06-25 | 2015-09-09 | 淄博德信联邦化学工业有限公司 | Waterborne polyurethane dispersion emulsion high in alcohol resistance and yellowing resistance and preparing method thereof |
| CN104892891B (en) * | 2015-06-25 | 2017-11-17 | 淄博德信联邦化学工业有限公司 | The aqueous polyurethane dispersion emulsion and preparation method thereof of high alcohol resistance, color inhibition |
| CN105175670A (en) * | 2015-09-28 | 2015-12-23 | 华南理工大学 | Amino resin modified waterborne polyurethane as well as preparation method and application thereof |
| CN105175670B (en) * | 2015-09-28 | 2017-10-20 | 华南理工大学 | A kind of amino resins modified aqueous polyurethane and preparation method and application |
| CN105732944A (en) * | 2016-04-12 | 2016-07-06 | 温州市登达化工有限公司 | Preparation method of transparent polyurethane |
| CN109401714A (en) * | 2018-10-16 | 2019-03-01 | 深圳日高胶带新材料有限公司 | A kind of OCA optics adhesive and its preparation method and application |
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Application publication date: 20130410 |