CN106700066A - Preparation of polyether amine diacid - Google Patents
Preparation of polyether amine diacid Download PDFInfo
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- CN106700066A CN106700066A CN201510793563.5A CN201510793563A CN106700066A CN 106700066 A CN106700066 A CN 106700066A CN 201510793563 A CN201510793563 A CN 201510793563A CN 106700066 A CN106700066 A CN 106700066A
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Abstract
The invention relates to preparation of polyether amine diacid. The preparation of the polyether amine diacid comprises the steps: adding 150 to 160 g of hydrogenated dimer acid, 25.50 g of sebacic acid, 18.12 g of polyether amine D-230, 39.40 g of polyether amine D-2000, 15.00 g of water and 1.8 g of tetra[beta-(3,5-ditert-butyl-4-hydroxyphenyl)propionic acid] pentaerythritol ester into a 500-mL four-neck flask with a thermometer, a stirrer, a condensation reflux pipe and a nitrogen pipe, putting 17.70 g of ethanediamine into a constant-pressure dropping funnel, rising temperature to120 to 130 DEG C, adding ethanediamine slowly and dropwise for 40 minutes, maintaining the temperature for 2 to 5 hours, vacuumizing for 2 to 4 hours by using a vacuum pump, and discharging under the protection of nitrogen to obtain a pale yellow material.
Description
Technical field
The present invention relates to a kind of preparation of polyethers diamide diacid material, belong to synthesis chemical field.
Background technology
Dimeric acid type polyamide hot melt adhesive is formed with diamine or polyamine condensation by dimeric dibasic acid, there is good adhesive property to various polar substrates, with preferable pliability, have a wide range of application, environment-friendly solvent-free, the advantages of preferable chemical-resistance and excellent processability, can be widely used for the industries such as electronic apparatus, automobile, packaging, machinery.But common polyamide hot resistance to low temperature is poor, softening point is relatively low, and high temperature viscosity is high to be unfavorable for shaping, it is impossible to meet the particular/special requirement of electronics, automobile and other industries.
The patent of Publication No. CN109887 provides a kind of synthetic method of dimer acid type polyamide resin, method by the initial period of reaction to appropriate organic inert solvent is added in reaction system, solve the uppity shortcoming of initial value, system is set to keep the reactiveness of stabilization in the early stage, and prevent the caking phenomenon that reaction system is likely to occur, but organic inert solvent has been used in invention, the pollution to environment has been easily caused.If melt polycondensation, temperature is raised quickly during early stage aliphatic diamine is added dropwise, and diamine highly volatile, and its equivalent is difficult control, and repeatability is poor.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation of polyethers diamide diacid material, and technical scheme is as follows：Added in the 500mL four-hole boiling flasks with thermometer, agitator, condensing reflux and nitrogen tube 150-160g hydrogenated dimer acids, 25.50g decanedioic acid, 18.12g polyetheramine D-230,39.40g polyetheramine D-2000,15.00g water, 1.8g tetra- [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester and 17.70g ethylenediamines are encased in constant pressure funnel; 120-130 DEG C is warmed up to start to be slowly added dropwise ethylenediamine; completion of dropping in 40 minutes; kept for 2-5 hours at this temperature; then vacuumized 2-4 hours with vavuum pump, finally discharging obtains pale yellow material under nitrogen protection.
The beneficial effects of the invention are as follows：Polyethers diamide diacid material of the invention, it is easy to be molded, preferable high and low temperature resistance and mechanical performance, water absorption rate are extremely low, environment-friendly solvent-free, can be widely applied to automobile, electron trade, and with water as solvent, material easily disperses, initial reaction stage temperature is low, and amine volatile quantity is small, environmentally safe.
Specific embodiment
Principle of the invention and feature are described below, example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Embodiment
1
Added in the 500mL four-hole boiling flasks with thermometer, agitator, condensing reflux and nitrogen tube 150g hydrogenated dimer acids, 25.50g decanedioic acid, 18.12g polyetheramine D-230,39.40g polyetheramine D-2000,15.00g water, 1.8g tetra- [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester and 17.70g ethylenediamines are encased in constant pressure funnel; 120 DEG C are warmed up to start to be slowly added dropwise ethylenediamine; completion of dropping in 40 minutes; kept for 2 hours at this temperature; then vacuumized 2 hours with vavuum pump, finally discharging obtains pale yellow material under nitrogen protection.
Embodiment
2
Added in the 500mL four-hole boiling flasks with thermometer, agitator, condensing reflux and nitrogen tube 160g hydrogenated dimer acids, 25.50g decanedioic acid, 18.12g polyetheramine D-230,39.40g polyetheramine D-2000,15.00g water, 1.8g tetra- [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester and 17.70g ethylenediamines are encased in constant pressure funnel; 130 DEG C are warmed up to start to be slowly added dropwise ethylenediamine; completion of dropping in 40 minutes; kept for 5 hours at this temperature; then vacuumized 4 hours with vavuum pump, finally discharging obtains pale yellow material under nitrogen protection.
Embodiment
3
Added in the 500mL four-hole boiling flasks with thermometer, agitator, condensing reflux and nitrogen tube 160g hydrogenated dimer acids, 25.50g decanedioic acid, 18.12g polyetheramine D-230,39.40g polyetheramine D-2000,15.00g water, 1.8g tetra- [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester and 17.70g ethylenediamines are encased in constant pressure funnel; 120 DEG C are warmed up to start to be slowly added dropwise ethylenediamine; completion of dropping in 40 minutes; kept for 4 hours at this temperature; then vacuumized 3 hours with vavuum pump, finally discharging obtains pale yellow material under nitrogen protection.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, made etc. should be included within the scope of the present invention.
Claims (2)
1. a kind of preparation of polyethers diamide diacid material, it is characterised in that including：Added in the 500mL four-hole boiling flasks with thermometer, agitator, condensing reflux and nitrogen tube 150-160g hydrogenated dimer acids, 25.50g decanedioic acid, 18.12g polyetheramine D-230,39.40g polyetheramine D-2000,15.00g water, 1.8g tetra- [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester and 17.70g ethylenediamines are encased in constant pressure funnel; 120-130 DEG C is warmed up to start to be slowly added dropwise ethylenediamine; completion of dropping in 40 minutes; kept for 2-5 hours at this temperature; then vacuumized 2-4 hours with vavuum pump, finally discharging obtains pale yellow material under nitrogen protection.
2. the preparation method according to belonging to claim 1, it is characterised in that coupling agent be four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510793563.5A CN106700066A (en) | 2015-11-18 | 2015-11-18 | Preparation of polyether amine diacid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510793563.5A CN106700066A (en) | 2015-11-18 | 2015-11-18 | Preparation of polyether amine diacid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106700066A true CN106700066A (en) | 2017-05-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510793563.5A Pending CN106700066A (en) | 2015-11-18 | 2015-11-18 | Preparation of polyether amine diacid |
Country Status (1)
| Country | Link |
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| CN (1) | CN106700066A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114316258A (en) * | 2022-01-12 | 2022-04-12 | 中山市好本意新材料有限公司 | PA color fixing agent and preparation method thereof |
-
2015
- 2015-11-18 CN CN201510793563.5A patent/CN106700066A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114316258A (en) * | 2022-01-12 | 2022-04-12 | 中山市好本意新材料有限公司 | PA color fixing agent and preparation method thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170524 |
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| WD01 | Invention patent application deemed withdrawn after publication |