CN109776745A - A kind of preparation method of butyl glycol ether modifying moieties Amino resin - Google Patents
A kind of preparation method of butyl glycol ether modifying moieties Amino resin Download PDFInfo
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- CN109776745A CN109776745A CN201811552863.4A CN201811552863A CN109776745A CN 109776745 A CN109776745 A CN 109776745A CN 201811552863 A CN201811552863 A CN 201811552863A CN 109776745 A CN109776745 A CN 109776745A
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- glycol ether
- butyl glycol
- modifying moieties
- amino resin
- methanol
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Abstract
The present invention relates to a kind of preparation methods of butyl glycol ether modifying moieties Amino resin, comprising steps of plus formaldehyde stirring, add methanol, liquid alkaline tune PH to 8；Polyformaldehyde, melamine, liquid alkaline tune PH to 8.5-9 are added, stirring 30mins heats up 75-80 DEG C；Timing 3h when hydroxylation reaction, 75-80 DEG C of hydroxylation reaction temperature；After hydroxylation reaction 3h, add methanol, open temperature lowering water, cool down 44 DEG C, add hydrochloric acid, PH to 4-4.5 keeps the temperature 1h, all turns liquid feeding alkali tune PH to 9-10 after neutralizing clearly；Normal pressure dealcoholysis heats up 82-86 DEG C, turns negative pressure dealcoholysis, opens vacuum pump, and dealcoholysis heats up 100 DEG C, adds butyl glycol ether, solid content 79-81%；Dealcoholysis terminates, filtering, desalination packaging.Compared with prior art, the present invention uses butyl glycol ether, and intermiscibility is good, and levelability, antifog wrinkle resistance, glossiness, adhesive force are good, can do finishing coat, and the service life is long and environmentally friendly.
Description
Technical field
The present invention relates to production of resins technical field, in particular to a kind of butyl glycol ether modifying moieties methyl-etherified amino tree
The preparation method of rouge.
Background technique
Amino resins belongs to one of principal item of thermoset synthetic resin, and Amino resin is through methanol height ether
The amino resins of change dissolves in organic solvent and water, and curing degree is fast, and hardness is high, and has higher gloss and impact resistance, excellent
Gesture is prominent；Its application surface is extensive, is mainly used for coiled material, automobile, aircraft circles；But traditional handicraft prepares part methyl-etherified amino
The method of resin, makees solvent frequently with mixed butanol, isobutanol, n-butanol etc., amino resins is diluted to 80% solid content, still
The performances such as product surface levelability made from this preparation method, antifog wrinkle resistance, glossiness are relatively poor, and can only do bottom back
Paint, service life is shorter, and is also easy to produce volatile organic matter (VOCs) using mixed butanol, isobutanol, n-butanol etc. as solvent, dirty
Contaminate environment.
In order to solve the above-mentioned technical problem, the present invention just proposes a kind of product levelability, antifog anti-of capable of more preferably improving
Wrinkle property and glossiness, can do finishing coat, prolong the service life and again environmentally friendly butyl glycol ether modifying moieties Amino resin
Preparation method.
Summary of the invention
The invention overcomes the defects existing in the prior art, and product levelling can more preferably be improved by proposing one kind
Property, antifog wrinkle resistance and glossiness, finishing coat can be done, prolonged the service life and again environmentally friendly butyl glycol ether modifying moieties methyl-etherified
The preparation method of amino resins.
The technical scheme of the present invention is realized as follows:
A kind of preparation method of butyl glycol ether modifying moieties Amino resin, includes the following steps:
(1) add formaldehyde in reaction kettle and stir, add methanol, liquid feeding alkali adjusts PH to 8；
(2) polyformaldehyde, melamine are added, liquid feeding alkali adjusts PH to 8.5-9, is warming up to 75- after stirring 30mins is uniform
80℃；
(3) start timing 3h when returning muddy crystallization hydroxylation reaction again after reactant turns clear dissolution, hydroxylation reaction temperature maintains
At 75-80 DEG C；
(4) after hydroxylation reaction 3h is arrived, add methanol, while opening temperature lowering water, be cooled to 44 DEG C, add hydrochloric acid, make PH to 4-4.5,
1h is kept the temperature, liquid feeding alkali adjusts PH to 9-10 after reactant all turns clear neutralization；
(5) normal pressure dealcoholysis after being warming up to 84 DEG C, switchs to negative pressure dealcoholysis, opens vacuum pump, and dealcoholysis is warming up to 100 DEG C, is added
Butyl glycol ether adjusts solid content to 79-81%；
(6) dealcoholysis terminates, and filters into filtering kettle and filter, and butyl glycol ether modifying moieties first is made in desalination packaging
Etherified amino resins.
Preferably, the material quality percentage of obtained butyl glycol ether modifying moieties Amino resin are as follows:
Formaldehyde 27.11-27.41%；Step (1) methanol 8.57-8.87%；Paraformaldehyde 3.45-3.75%；Melamine 10.75-
11.05%；Step (4) methanol 43.46-43.76%；Hydrochloric acid 0.04-0.34%；Liquid alkaline 0.12-0.42%；Butyl glycol ether
5.30-5.60%, and the sum of mass ratio of each raw material is 100%.
Preferably, the material quality percentage of obtained butyl glycol ether modifying moieties Amino resin are as follows:
Formaldehyde 27.26%；Step (1) methanol 8.72%；Paraformaldehyde 3.60%；Melamine 10.90%；Step (4) methanol
43.61%；Hydrochloric acid 0.19%；Liquid alkaline 0.27%；Butyl glycol ether 5.45%, and the sum of mass ratio of each raw material is 100%.
Preferably, the concentration of formaldehyde 37%, step (1) methanol concentration 60%, paraformaldehyde concentration 96%, melamine
Amine concentration 99.5%, step (4) methanol concentration 90%, concentration of hydrochloric acid 36%, liquid alkaline concentration 30%, butyl glycol ether concentration
99%.
Preferably, the vacuum degree 0.09MPa in step (5).
Using above-mentioned technical proposal the beneficial effects of the present invention are:
The invention proposes one kind can more preferably improve product levelability, antifog wrinkle resistance and glossiness, can do finishing coat, prolong
The preparation method of long life and again environmentally friendly butyl glycol ether modifying moieties Amino resin.The present invention uses second two
Alcohol butyl ether substitutes existing mixed butanol, isobutanol, n-butanol etc., and existing mixed butanol, isobutanol, n-butanol boiling point are relatively low
(mixed 117.6 DEG C of butanol), and 171 DEG C of butyl glycol ether boils up till, high boiling butyl glycol ether makees solvent, with amino resins
Intermiscibility it is more preferable, product surface of the paint film tension can be reduced, good leveling property is not wrinkled, can do finishing coat, promotes class, expands
The big scope of application, is specifically for use in airplane dope；The present invention improves baking temperature, and glossiness can be more prominent；Using ethylene glycol
Butyl ether substitutes existing mixed butanol, isobutanol, n-butanol etc., also reduces the discharge of volatile organic matter (VOCs), and environmental protection is excellent
Gesture is prominent.
Specific embodiment
A specific embodiment of the invention is as follows:
Embodiment 1:
A kind of preparation method of butyl glycol ether modifying moieties Amino resin, includes the following steps:
(1) add formaldehyde in reaction kettle and stir, add methanol, liquid feeding alkali adjusts PH to 8；
(2) polyformaldehyde, melamine are added, liquid feeding alkali adjusts PH to 8.5-9, is warming up to 75- after stirring 30mins is uniform
80℃；
(3) start timing 3h when returning muddy crystallization hydroxylation reaction again after reactant turns clear dissolution, hydroxylation reaction temperature maintains
At 75-80 DEG C；
(4) after hydroxylation reaction 3h is arrived, add methanol, while opening temperature lowering water, be cooled to 44 DEG C, add hydrochloric acid, make PH to 4-4.5,
1h is kept the temperature, liquid feeding alkali adjusts PH to 9-10 after reactant all turns clear neutralization；
(5) normal pressure dealcoholysis after being warming up to 84 DEG C, switchs to negative pressure dealcoholysis, opens vacuum pump, vacuum degree 0.09MPa, dealcoholysis liter
Butyl glycol ether is added to 100 DEG C in temperature, adjusts solid content to 79-81%；
(6) dealcoholysis terminates, and filters into filtering kettle and filter, and butyl glycol ether modifying moieties first is made in desalination packaging
Etherified amino resins.
Table 1 is that embodiment 1 prepares the concentration of each raw material of butyl glycol ether modifying moieties Amino resin and quality is matched
Side's (mass percent):
| Raw material | Concentration | Mass percent | The 1 specific quality of each raw material of embodiment (unit: gram) |
| Formaldehyde | 37% | 27.29% | 250.3 |
| Step (1) methanol | 60% | 8.73% | 80.1 |
| Paraformaldehyde | 96% | 3.60% | 33 |
| Melamine | 99.5% | 10.92% | 100.2 |
| Step (4) methanol | 90% | 43.70% | 400.8 |
| Hydrochloric acid | 36% | 0.19% | 1.7 |
| Liquid alkaline | 30% | 0.27% | 2.5 |
| Butyl glycol ether | 99% | 5.3% | 48.6 |
Table 1
Seen using butyl glycol ether modifying moieties Amino resin the performance test results obtained by above-described embodiment 1
Table 2:
Table 2
Embodiment 2:
A kind of preparation method of butyl glycol ether modifying moieties Amino resin, includes the following steps:
(1) add formaldehyde in reaction kettle and stir, add methanol, liquid feeding alkali adjusts PH to 8；
(2) polyformaldehyde, melamine are added, liquid feeding alkali adjusts PH to 8.5-9, is warming up to 75- after stirring 30mins is uniform
80℃；
(3) start timing 3h when returning muddy crystallization hydroxylation reaction again after reactant turns clear dissolution, hydroxylation reaction temperature maintains
At 75-80 DEG C；
(4) after hydroxylation reaction 3h is arrived, add methanol, while opening temperature lowering water, be cooled to 44 DEG C, add hydrochloric acid, make PH to 4-4.5,
1h is kept the temperature, liquid feeding alkali adjusts PH to 9-10 after reactant all turns clear neutralization；
(5) normal pressure dealcoholysis after being warming up to 84 DEG C, switchs to negative pressure dealcoholysis, opens vacuum pump, vacuum degree 0.09MPa, dealcoholysis liter
Butyl glycol ether is added to 100 DEG C in temperature, adjusts solid content to 79-81%；
(6) dealcoholysis terminates, and filters into filtering kettle and filter, and butyl glycol ether modifying moieties first is made in desalination packaging
Etherified amino resins.
Table 3 is that embodiment 2 prepares the concentration of each raw material of butyl glycol ether modifying moieties Amino resin and quality is matched
Side's (mass percent):
Table 3
Seen using butyl glycol ether modifying moieties Amino resin the performance test results obtained by above-described embodiment 2
Table 4:
| Detection project | Parameter |
| Appearance | It is water-white, smooth, smooth |
| Adhesive force | 100% |
| Intermiscibility (range estimation) | Uniformly |
| Levelability | Without brush mark |
| Glossiness (45 °) | 99.8 |
| Glossiness (60 °) | 96.8 |
| Free formaldehyde | 0.80% |
| Hardness (double pendulum) | 0.848 |
| Solid content/wt% (108 DEG C, 1.5h) | 80% |
| Viscosity/mPas (25 DEG C) | 2542 |
Table 4
Embodiment 3:
A kind of preparation method of butyl glycol ether modifying moieties Amino resin, includes the following steps:
(1) add formaldehyde in reaction kettle and stir, add methanol, liquid feeding alkali adjusts PH to 8；
(2) polyformaldehyde, melamine are added, liquid feeding alkali adjusts PH to 8.5-9, is warming up to 75- after stirring 30mins is uniform
80℃；
(3) start timing 3h when returning muddy crystallization hydroxylation reaction again after reactant turns clear dissolution, hydroxylation reaction temperature maintains
At 75-80 DEG C；
(4) after hydroxylation reaction 3h is arrived, add methanol, while opening temperature lowering water, be cooled to 44 DEG C, add hydrochloric acid, make PH to 4-4.5,
1h is kept the temperature, liquid feeding alkali adjusts PH to 9-10 after reactant all turns clear neutralization；
(5) normal pressure dealcoholysis after being warming up to 84 DEG C, switchs to negative pressure dealcoholysis, opens vacuum pump, and dealcoholysis is warming up to 100 DEG C, is added
Butyl glycol ether adjusts solid content to 79-81%；
(6) dealcoholysis terminates, and filters into filtering kettle and filter, and butyl glycol ether modifying moieties first is made in desalination packaging
Etherified amino resins.
Table 5 is that embodiment 3 prepares the concentration of each raw material of butyl glycol ether modifying moieties Amino resin and quality is matched
Side's (mass percent):
| Raw material | Concentration | Mass percent | The 1 specific quality of each raw material of embodiment (unit: gram) |
| Formaldehyde | 37% | 27.26% | 250 |
| Step (1) methanol | 60% | 8.72% | 80 |
| Paraformaldehyde | 96% | 3.60% | 33 |
| Melamine | 99.5% | 10.90% | 100 |
| Step (4) methanol | 90% | 43.61% | 400 |
| Hydrochloric acid | 36% | 0.19% | 1.7 |
| Liquid alkaline | 30% | 0.27% | 2.5 |
| Butyl glycol ether | 99% | 5.45% | 50 |
Table 5
Seen using butyl glycol ether modifying moieties Amino resin the performance test results obtained by above-described embodiment 3
Table 6:
| Detection project | Parameter |
| Appearance | It is water-white, smooth, smooth |
| Adhesive force | 100% |
| Intermiscibility (range estimation) | Uniformly |
| Levelability | Without brush mark |
| Glossiness (45 °) | 100 |
| Glossiness (60 °) | 97 |
| Free formaldehyde | 0.8% |
| Hardness (double pendulum) | 0.85 |
| Solid content/wt% (108 DEG C, 1.5h) | 80% |
| Viscosity/mPas (25 DEG C) | 2500 |
Table 6
Embodiment 4:
A kind of preparation method of butyl glycol ether modifying moieties Amino resin, includes the following steps:
(1) add formaldehyde in reaction kettle and stir, add methanol, liquid feeding alkali adjusts PH to 8；
(2) polyformaldehyde, melamine are added, liquid feeding alkali adjusts PH to 8.5-9, is warming up to 75- after stirring 30mins is uniform
80℃；
(3) start timing 3h when returning muddy crystallization hydroxylation reaction again after reactant turns clear dissolution, hydroxylation reaction temperature maintains
At 75-80 DEG C；
(4) after hydroxylation reaction 3h is arrived, add methanol, while opening temperature lowering water, be cooled to 44 DEG C, add hydrochloric acid, make PH to 4-4.5,
1h is kept the temperature, liquid feeding alkali adjusts PH to 9-10 after reactant all turns clear neutralization；
(5) normal pressure dealcoholysis after being warming up to 84 DEG C, switchs to negative pressure dealcoholysis, opens vacuum pump, vacuum degree 0.09MPa, dealcoholysis liter
Butyl glycol ether is added to 100 DEG C in temperature, adjusts solid content to 79-81%；
(6) dealcoholysis terminates, and filters into filtering kettle and filter, and butyl glycol ether modifying moieties first is made in desalination packaging
Etherified amino resins.
Table 7 is that embodiment 4 prepares the concentration of each raw material of butyl glycol ether modifying moieties Amino resin and quality is matched
Side's (mass percent):
| Raw material | Concentration | Mass percent | The 1 specific quality of each raw material of embodiment (unit: gram) |
| Formaldehyde | 37% | 27.23% | 249.8 |
| Step (1) methanol | 60% | 8.72% | 80 |
| Paraformaldehyde | 96% | 3.60% | 33 |
| Melamine | 99.5% | 10.86% | 99.6 |
| Step (4) methanol | 90% | 43.58% | 399.7 |
| Hydrochloric acid | 36% | 0.19% | 1.7 |
| Liquid alkaline | 30% | 0.27% | 2.5 |
| Butyl glycol ether | 99% | 5.55% | 50.9 |
Table 7
Seen using butyl glycol ether modifying moieties Amino resin the performance test results obtained by above-described embodiment 4
Table 8:
Table 8
Embodiment 5:
A kind of preparation method of butyl glycol ether modifying moieties Amino resin, includes the following steps:
(1) add formaldehyde in reaction kettle and stir, add methanol, liquid feeding alkali adjusts PH to 8；
(2) polyformaldehyde, melamine are added, liquid feeding alkali adjusts PH to 8.5-9, is warming up to 75- after stirring 30mins is uniform
80℃；
(3) start timing 3h when returning muddy crystallization hydroxylation reaction again after reactant turns clear dissolution, hydroxylation reaction temperature maintains
At 75-80 DEG C；
(4) after hydroxylation reaction 3h is arrived, add methanol, while opening temperature lowering water, be cooled to 44 DEG C, add hydrochloric acid, make PH to 4-4.5,
1h is kept the temperature, liquid feeding alkali adjusts PH to 9-10 after reactant all turns clear neutralization；
(5) normal pressure dealcoholysis after being warming up to 84 DEG C, switchs to negative pressure dealcoholysis, opens vacuum pump, vacuum degree 0.09MPa, dealcoholysis liter
Butyl glycol ether is added to 100 DEG C in temperature, adjusts solid content to 79-81%；
(6) dealcoholysis terminates, and filters into filtering kettle and filter, and butyl glycol ether modifying moieties first is made in desalination packaging
Etherified amino resins.
Table 9 is that embodiment 5 prepares the concentration of each raw material of butyl glycol ether modifying moieties Amino resin and quality is matched
Side's (mass percent):
Table 9
Seen using butyl glycol ether modifying moieties Amino resin the performance test results obtained by above-described embodiment 3
Table 6:
| Detection project | Parameter |
| Appearance | It is water-white, more smooth, smooth |
| Adhesive force | 100% |
| Intermiscibility (range estimation) | Uniformly |
| Levelability | Micro- brush mark |
| Glossiness (45 °) | 99.75 |
| Glossiness (60 °) | 96.87 |
| Free formaldehyde | 0.79% |
| Hardness (double pendulum) | 0.85 |
| Solid content/wt% (108 DEG C, 1.5h) | 79.8% |
| Viscosity/mPas (25 DEG C) | 2538 |
Table 10.
Claims (5)
1. a kind of preparation method of butyl glycol ether modifying moieties Amino resin, characterized by the following steps:
(1) add formaldehyde in reaction kettle and stir, add methanol, liquid feeding alkali adjusts PH to 8；
(2) polyformaldehyde, melamine are added, liquid feeding alkali adjusts PH to 8.5-9, is warming up to 75-80 DEG C after stirring 30mins is uniform；
(3) start timing 3h when returning muddy crystallization hydroxylation reaction again after reactant turns clear dissolution, hydroxylation reaction temperature maintains 75-
80℃；
(4) after hydroxylation reaction 3h is arrived, add methanol, while opening temperature lowering water, be cooled to 44 DEG C, add hydrochloric acid, make PH to 4-4.5, keep the temperature
1h, liquid feeding alkali adjusts PH to 9-10 after reactant all turns clear neutralization；
(5) normal pressure dealcoholysis after being warming up to 84 DEG C, switchs to negative pressure dealcoholysis, opens vacuum pump, and dealcoholysis is warming up to 100 DEG C, and second two is added
Alcohol butyl ether adjusts solid content to 79-81%；
(6) dealcoholysis terminates, and filters into filtering kettle and filter, and butyl glycol ether modifying moieties methyl-etherified is made in desalination packaging
Amino resins.
2. a kind of preparation method of butyl glycol ether modifying moieties Amino resin according to claim 1, special
Sign is: the material quality percentage of obtained butyl glycol ether modifying moieties Amino resin are as follows: formaldehyde 27.11-
27.41%；Step (1) methanol 8.57-8.87%；Paraformaldehyde 3.45-3.75%；Melamine 10.75-11.05%；Step
(4) methanol 43.46-43.76%；Hydrochloric acid 0.04-0.34%；Liquid alkaline 0.12-0.42%；Butyl glycol ether 5.30-5.60%, and
The sum of mass ratio of each raw material is 100%.
3. a kind of preparation method of butyl glycol ether modifying moieties Amino resin according to claim 1, special
Sign is: the material quality percentage of obtained butyl glycol ether modifying moieties Amino resin are as follows: formaldehyde
27.26%；Step (1) methanol 8.72%；Paraformaldehyde 3.60%；Melamine 10.90%；Step (4) methanol 43.61%；
Hydrochloric acid 0.19%；Liquid alkaline 0.27%；Butyl glycol ether 5.45%, and the sum of mass ratio of each raw material is 100%.
4. a kind of preparation side of butyl glycol ether modifying moieties Amino resin according to claim 1 or 2 or 3
Method, it is characterised in that: the concentration of formaldehyde 37%, step (1) methanol concentration 60%, paraformaldehyde concentration 96%, melamine
Concentration 99.5%, step (4) methanol concentration 90%, concentration of hydrochloric acid 36%, liquid alkaline concentration 30%, butyl glycol ether concentration 99%.
5. a kind of preparation method of butyl glycol ether modifying moieties Amino resin according to claim 1, special
Sign is: the vacuum degree 0.09MPa in step (5).
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|---|---|---|---|---|
| JPS50129629A (en) * | 1974-03-26 | 1975-10-14 | ||
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| CN104530806A (en) * | 2014-12-19 | 2015-04-22 | 江南大学 | Preparation method and application of high-golss and high-leveling-property water-based coating additive |
| CN104829797A (en) * | 2015-04-16 | 2015-08-12 | 浙江新华涂料有限责任公司 | Preparation method of partially methylated amino resin |
| CN104946103A (en) * | 2015-07-30 | 2015-09-30 | 浙江乔兴建设集团有限公司 | Resin paint brushing method |
| CN105585684A (en) * | 2016-01-12 | 2016-05-18 | 浙江新华新材料科技有限责任公司 | Method and equipment for preparing full-water-soluble high-imino partial-methylated amino resin |
-
2018
- 2018-12-19 CN CN201811552863.4A patent/CN109776745A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50129629A (en) * | 1974-03-26 | 1975-10-14 | ||
| US4163835A (en) * | 1976-01-31 | 1979-08-07 | Cassella Aktiengesellschaft | Preparation of electrolyte-free aminoplast resins |
| CN104530806A (en) * | 2014-12-19 | 2015-04-22 | 江南大学 | Preparation method and application of high-golss and high-leveling-property water-based coating additive |
| CN104829797A (en) * | 2015-04-16 | 2015-08-12 | 浙江新华涂料有限责任公司 | Preparation method of partially methylated amino resin |
| CN104946103A (en) * | 2015-07-30 | 2015-09-30 | 浙江乔兴建设集团有限公司 | Resin paint brushing method |
| CN105585684A (en) * | 2016-01-12 | 2016-05-18 | 浙江新华新材料科技有限责任公司 | Method and equipment for preparing full-water-soluble high-imino partial-methylated amino resin |
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| Title |
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| 刘占梅 等: ""乙二醇单丁醚对三聚氰胺-甲醛树脂浸渍纸的增塑作用"", 《木材工业》 * |
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