CN103059278B - Air dry alkyd resin and preparation method thereof - Google Patents
Air dry alkyd resin and preparation method thereof Download PDFInfo
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- CN103059278B CN103059278B CN201210560587.2A CN201210560587A CN103059278B CN 103059278 B CN103059278 B CN 103059278B CN 201210560587 A CN201210560587 A CN 201210560587A CN 103059278 B CN103059278 B CN 103059278B
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- dry alkyd
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Abstract
The invention discloses a kind of air dry alkyd resin and preparation method thereof, this air dry alkyd resin is made up of dryness or semi-drying vegetable oils 22 ~ 28 parts, dryness or semi-drying vegetable oils acid 2 ~ 5 parts, monopentaerythritol 6 ~ 10 parts, alcoholysis catalysts 0.005 0.02 parts, phthalic anhydride 12 ~ 15 parts, dimethylbenzene 13 parts, organic solvent 42 ~ 44 parts.The air dry alkyd resin that the present invention provides, screens composition and the proportioning of each raw material by great many of experiments, the air dry alkyd resin prepared have of light color, transparency good, gloss of film is high, gloss retention is good, weather-proof good, the advantage having wide range of applications.The preparation method of the air dry alkyd resin that the present invention provides, add dryness or the vegetable oil acid of semi-drying, the fusing point making monopentaerythritol reduces, alcoholysis reaction is made to be more prone to carry out, glycolysis temperature is lower, the alcoholysis time is short, and energy consumption is low, and environmental-protecting performance is more preferable, whole preparation technology is workable, it is easy to implement.
Description
Technical field
The present invention relates to a kind of resin, be specifically related to a kind of air dry alkyd resin and preparation method thereof.
Background technology
Air dry alkyd resin mainly by adding drier, in atmosphere autoxidation drying and forming-film, can be made into varnish,
Colored paint, various coating and auxiliary material become alkyd resin coating system.Paint film has good gloss, gloss retention and weatherability,
Prominent advantage is easy to brush application, good leveling property.Building coating, outdoor steel structural traverse are extensively applied.
The air dry alkyd of prior art mainly has two kinds of manufacture methods, and one is fatty acid process, the color of resin worked it out
Shallow, due to fatty acid be all by the hydrolysis of the leftover bits and pieces of vegetable oil producer-acidification oil, distillation, the gloss retention of resin with
Weatherability is bad.Another kind is alcoholysis method, be authentic vegetable oil and monopentaerythritol, the gloss retention of resin and weatherability
Very well, so Paint Factory is when doing enamel paint, the general alkyd resin selecting alcoholysis method.But owing to the fusing point of monopentaerythritol is high,
Temperature to more than 240 DEG C just alcoholysis, and the alcoholysis complete time at least want 100 minutes, the alcoholysis time is long, and preparation efficiency is low, and
And if slightly impurity in reaction mass, the alcoholysis time completely can be longer, and alcoholysis sometimes can not be thorough.So alcoholysis legal system
Color of resin is deep, and transparency is bad sometimes, receives bigger restriction in enamel paint application.Therefore, necessary in prior art
Basis on, a kind of of light color, paint film of R & D design has good gloss, gloss retention and weatherability, is prone to brush application,
The air dry alkyd resin of good leveling property.
Summary of the invention
Goal of the invention: the technical problem to be solved is to overcome the deficiencies in the prior art, it is provided that a kind of of light color,
Transparency is good, paint film has good gloss, gloss retention and weatherability, be prone to brush application, the air dry alkyd tree of good leveling property
Fat.Another object of the present invention is to provide one, and glycolysis temperature is low, the alcoholysis time is short, alcoholysis reaction is more prone to carry out, energy consumption
The preparation method of lower air dry alkyd resin.
Technical scheme: for solving above technical problem, the present invention adopts the following technical scheme that:
A kind of air dry alkyd resin, it is made up of the raw material of following parts by weight:
Dryness or semi-drying vegetable oils 22 ~ 28 parts, dryness or semi-drying vegetable oils acid 2 ~ 5 parts, monopentaerythritol 6 ~ 10 parts,
Alcoholysis catalysts 0.005-0.02 part, phthalic anhydride 12 ~ 15 parts, dimethylbenzene 1-3 part, organic solvent 42 ~ 44 parts.
Preferably, above-described air dry alkyd resin, it is made up of the raw material of following parts by weight:
Dryness or semi-drying vegetable oils 24 ~ 26 parts, dryness or semi-drying vegetable oils acid 3 ~ 4 parts, monopentaerythritol 8 ~ 10 parts,
Alcoholysis catalysts 0.010.02 part, phthalic anhydride 13 ~ 14 parts, dimethylbenzene 2-3 part, organic solvent 42 ~ 43 parts.
Preferably, above-described air dry alkyd resin, described dryness or semi-drying vegetable oils are Oleum Glycines, certain herbaceous plants with big flowers
Caul-fat or oleum lini.
Preferably, above-described air dry alkyd resin, described dryness or semi-drying vegetable oils acid are Oleum Glycines
Fatty acid, cotton oil fatty acid, linseed oil fatty acid.
Preferably, above-described air dry alkyd resin, described alcoholysis catalysts is aphthenic acids lithium, hydroxide
A kind of in lithium, calcium naphthenate, calcium hydroxide or their mixture.
Preferably, above-described a kind of air dry alkyd resin, described organic solvent be solvent naphtha 190#,
200# or D-40.
The preparation method of the air dry alkyd resin that the present invention provides, comprises the following steps:
(1) by dryness or semi-drying vegetable oils 22 ~ 28 parts, dryness or semi-drying vegetable oils acid 2 ~ 5 parts, monopentaerythritol 6 ~
10 parts join in reactor, are passed through nitrogen, when being warming up to 230 DEG C, add alcoholysis catalysts 0.005-0.02 part, make material exist
Alcoholysis reaction between 230 DEG C ~ 235 DEG C；
(2) when after step (1) alcoholysis reaction 30 ~ 40 minutes, be cooled to less than 180 DEG C, be subsequently adding phthalic anhydride 12 ~ 15 parts and
Backflow dimethylbenzene 1-3 part, is then rapidly heated and carries out esterification between 220 DEG C ~ 233 DEG C, be subsequently adding organic solvent 42 ~
44 parts, obtain air dry alkyd resin.
Preferably, the preparation method of above-described air dry alkyd resin, described dryness or semi-drying plant
Oil is Oleum Glycines, sunflower oil or oleum lini；Described dryness or semi-drying vegetable oils acid are soy(a)-bean oil fatty acid, cotton oil fatty acid, Asia
Oleum Sesami fatty acid.
Preferably, the preparation method of above-described air dry alkyd resin, described alcoholysis catalysts is cycloalkanes
A kind of or their mixture in acid lithium, Lithium hydrate, calcium naphthenate, calcium hydroxide.
Preferably, the preparation method of above-described air dry alkyd resin, described organic solvent is solvent naphtha
190#, 200# or D-40.
Preferably, the preparation method of above-described air dry alkyd resin, step (2) esterification is until reaching
Acid number≤15(is solid), viscosity: 15-20 second * form pipe (organic solvent is converted 55 and admittedly contained, 25 DEG C).
Beneficial effect: compared to the prior art the air dry alkyd resin that the present invention provides has the advantage that
1, the air dry alkyd resin that the present invention provides, screens composition and the proportioning of each raw material, each component by great many of experiments
Proportioning is scientific and reasonable, the air dry alkyd resin prepared have of light color, transparency good, gloss of film is high, gloss retention is good, resistance to
Hou Hao, the advantage having wide range of applications.
2, the preparation method of the air dry alkyd resin that the present invention provides, with the addition of the vegetable oil of a small amount of dryness or semi-drying
Acid, while alcoholysis, dryness or the vegetable oil acid of semi-drying and monopentaerythritol reaction generate tetramethylolmethane one acid esters and season
Penta tetrol two acid esters, makes the fusing point of monopentaerythritol reduce, and makes alcoholysis reaction be more prone to carry out, and glycolysis temperature is lower, alcoholysis
Time is short, and energy consumption is low, and environmental-protecting performance is more preferable, and whole preparation technology is workable, it is easy to implement.
Detailed description of the invention
Below in conjunction with specific embodiment, it is further elucidated with the present invention, it should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention, after having read the present invention, the those skilled in the art's various equivalences to the present invention
The amendment of form all falls within the application claims limited range.
Embodiment 1
1, a kind of air dry alkyd resin, it is made up of the raw material of following parts by weight:
28 parts of Oleum Glycines, soy(a)-bean oil fatty acid 5 parts, monopentaerythritol 10 parts, alcoholysis catalysts aphthenic acids lithium 0.02 part, phthalic anhydride 15
Part, backflow dimethylbenzene 3 parts, solvent naphtha 190# 44 parts.
2, the preparation method of air dry alkyd resin, comprises the following steps:
(1) 28 parts of Oleum Glycines, soy(a)-bean oil fatty acid 5 parts, monopentaerythritol 10 parts are joined in reactor, be passed through nitrogen, rise
When temperature is to 230 DEG C, adds alcoholysis catalysts aphthenic acids lithium 0.02 part, make material alcoholysis reaction between 230 DEG C ~ 235 DEG C；
(2) when after step (1) alcoholysis reaction 30 minutes, it is cooled to less than 180 DEG C, is subsequently adding 15 parts of phthalic anhydrides and backflow two
Toluene 3 parts, is then rapidly heated and carries out esterification between 220 DEG C ~ 233 DEG C, be subsequently adding solvent naphtha 190# 44 parts,
To air dry alkyd resin.
Embodiment 2
1, a kind of air dry alkyd resin, it is made up of the raw material of following parts by weight:
Sunflower oil 22 parts, cotton oil fatty acid 2 parts, monopentaerythritol 6 parts, alcoholysis catalysts Lithium hydrate 0.005 part, phthalic anhydride
12 parts, backflow dimethylbenzene 1 part, solvent naphtha 200# 42 parts.
2, the preparation method of air dry alkyd resin, comprises the following steps:
(1) sunflower oil 22 parts, cotton oil fatty acid 2 parts, monopentaerythritol 6 parts are joined in reactor, be passed through nitrogen, rise
When temperature is to 230 DEG C, adds alcoholysis catalysts Lithium hydrate 0.005 part, make material alcoholysis reaction between 230 DEG C ~ 235 DEG C；
(2) when after step (1) alcoholysis reaction 30 minutes, it is cooled to less than 180 DEG C, is subsequently adding 12 parts of phthalic anhydrides and 3 parts and returns
Stream dimethylbenzene, is then rapidly heated and carries out esterification between 220 DEG C ~ 233 DEG C, until it reaches acid number≤15(is solid), viscosity:
15-20 second * form pipe (organic solvent is converted 55 and admittedly contained, 25 DEG C) is subsequently adding solvent naphtha 200# 42 parts, obtains air dry alkyd tree
Fat.
Embodiment 3
1, a kind of air dry alkyd resin, it is made up of the raw material of following parts by weight:
Oleum lini 24 parts, linseed oil fatty acid 3 parts, monopentaerythritol 8 parts, alcoholysis catalysts calcium naphthenate 0.005 part, hydrogen
Calcium oxide 0.005 part, phthalic anhydride 14 parts, backflow dimethylbenzene 2 parts, solvent naphtha D-40 43 parts.
2, the preparation method of air dry alkyd resin, comprises the following steps:
(1) oleum lini 23 parts, linseed oil fatty acid 4 parts, monopentaerythritol 8 parts are joined in reactor, are passed through nitrogen,
When being warming up to 230 DEG C, add alcoholysis catalysts calcium naphthenate 0.005 part and calcium hydroxide 0.005 part, make material 230 DEG C ~
Alcoholysis reaction between 235 DEG C；
(2) when after step (1) alcoholysis reaction 40 minutes, it is cooled to less than 180 DEG C, is subsequently adding 14 parts of phthalic anhydrides and 2 parts and returns
Stream dimethylbenzene, is then rapidly heated and carries out esterification between 220 DEG C ~ 233 DEG C, until it reaches acid number≤15(is solid), viscosity:
15-20 second * form pipe (organic solvent is converted 55 and admittedly contained, 25 DEG C) is subsequently adding solvent naphtha D-40 43 parts, obtains air dry alkyd tree
Fat.
Embodiment 4
1, a kind of air dry alkyd resin, it is made up of the raw material of following parts by weight:
Oleum lini 24 parts, soy(a)-bean oil fatty acid 3 parts, monopentaerythritol 8 parts, alcoholysis catalysts Lithium hydrate 0.005 part, cycloalkanes
Acid calcium 0.005 part, calcium hydroxide 0.005 part, phthalic anhydride 13 parts, backflow dimethylbenzene 3 parts, solvent naphtha D-40 43 parts.
2, the preparation method of air dry alkyd resin, comprises the following steps:
(1) oleum lini 24 parts, soy(a)-bean oil fatty acid 3 parts, monopentaerythritol 8 parts are joined in reactor, be passed through nitrogen, rise
When temperature is to 230 DEG C, adds alcoholysis catalysts Lithium hydrate 0.005 part, calcium naphthenate 0.005 part, calcium hydroxide 0.005 part, make
Material is alcoholysis reaction between 230 DEG C ~ 235 DEG C；
(2) when after step (1) alcoholysis reaction 40 minutes, it is cooled to less than 180 DEG C, is subsequently adding 13 parts of phthalic anhydrides and 3 parts and returns
Stream dimethylbenzene, is then rapidly heated and carries out esterification between 220 DEG C ~ 233 DEG C, be subsequently adding solvent naphtha D-40 43 parts,
To air dry alkyd resin.
Embodiment 5 performance test experience
Take the present invention to implement the air dry alkyd resin that 1 to embodiment 4 prepares and carry out performance detection, specific experiment result
As shown in table 1:
The performance test results of table 1 air dry alkyd resin
| Testing index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Color and luster (ferrum-cobalt) | 7 | 6 | 7 | 6 |
| Surface drying time (min) | 15 | 18 | 13 | 14 |
| Gloss | 95 | 97 | 96 | 97 |
| Adhesive force (draws circle method) | 1 grade | 1 grade | 1 grade | 1 grade |
| Impact strength (kg.cm) | 50 | 50 | 50 | 50 |
| Hardness (Pencil scratch) | HB | HB | HB | HB |
By the test result of table 1 it can be seen that the air dry alkyd resin that the present invention prepares to have surface drying time short, light
Pool degree is good, and adhesive force is strong, and shock resistance degree is good, and hardness is strong, and also has that of light color (the alcoholysis color of resin of prior art exists
More than No. 10 colors), transparency good, gloss of film is high, gloss retention is good, good weatherability, the advantages such as range of application is more extensive.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (1)
1. the preparation method of an air dry alkyd resin, it is characterised in that comprise the following steps:
(1) by dryness or semi-drying vegetable oils 22～28 parts, dryness or semi-drying vegetable oils acid 2～5 parts, monopentaerythritol 6～
10 parts join in reactor, are passed through nitrogen, when being warming up to 230 DEG C, add alcoholysis catalysts 0.005-0.02 part, make material exist
Alcoholysis reaction between 230 DEG C～235 DEG C；
(2) when after step (1) alcoholysis reaction 30～40 minutes, it is cooled to less than 180 DEG C, is subsequently adding phthalic anhydride 12～15 parts and returns
Stream dimethylbenzene 1-3 part, be then rapidly heated between 220 DEG C～233 DEG C and carry out esterification, be subsequently adding organic solvent 42～
44 parts, obtain air dry alkyd resin；
Described dryness or semi-drying vegetable oils are Oleum Glycines, sunflower oil or oleum lini；Described dryness or semi-drying vegetable oils acid
For soy(a)-bean oil fatty acid, cotton oil fatty acid, linseed oil fatty acid；
Described alcoholysis catalysts is a kind of in aphthenic acids lithium, Lithium hydrate, calcium naphthenate, calcium hydroxide or theirs is mixed
Compound；
Described organic solvent is solvent naphtha 190#, 200# or D-40.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210560587.2A CN103059278B (en) | 2012-12-21 | 2012-12-21 | Air dry alkyd resin and preparation method thereof |
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| CN201210560587.2A CN103059278B (en) | 2012-12-21 | 2012-12-21 | Air dry alkyd resin and preparation method thereof |
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| CN103059278A CN103059278A (en) | 2013-04-24 |
| CN103059278B true CN103059278B (en) | 2016-11-23 |
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| CN106957414B (en) * | 2017-04-07 | 2019-05-03 | 重庆三峡油漆股份有限公司 | High solid is from dry alkyd resin and preparation method thereof |
| CN107082874A (en) * | 2017-05-19 | 2017-08-22 | 江苏三木化工股份有限公司 | A kind of net taste Matt alkyd resin and preparation method |
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| US7256226B2 (en) * | 2004-03-15 | 2007-08-14 | Hexion Specialty Chemicals, Inc. | Storage-stable acrylate-functional alkyd resin compositions |
| CN101671519B (en) * | 2009-09-28 | 2011-11-30 | 北京红狮漆业有限公司 | Odor-free alcoholic acid paint and preparation method thereof |
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