CN107118337A - A kind of preparation method of polyester resin for powder coating - Google Patents
A kind of preparation method of polyester resin for powder coating Download PDFInfo
- Publication number
- CN107118337A CN107118337A CN201710448206.4A CN201710448206A CN107118337A CN 107118337 A CN107118337 A CN 107118337A CN 201710448206 A CN201710448206 A CN 201710448206A CN 107118337 A CN107118337 A CN 107118337A
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- preparation
- acid
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- acid number
- polyester resin
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- 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
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- 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
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
-
- 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
- C08G2150/00—Compositions for coatings
- C08G2150/20—Compositions for powder coatings
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of preparation method of polyester resin for powder coating, this preparation method is by by binary acid and dibasic alcohol ester course of reaction, the acid number and viscosity number of a certain reaction node in course of reaction being fixed, diversity is provided for preparation method.
Description
Technical field
The present invention relates to the preparation method in powder coating technology field, more particularly to polyester resin for powder coating.
Background technology
The preparation of existing polyester resin for powder coating is all according to specific material characteristic, to specific preparation method
It is fixed, once the amount of reactant somewhat changes, its preparation technology will be adjusted, technique originally can not make again
With.
For example：The esterification that neopentyl glycol and cyclohexanedimethanol are carried out with terephthalic acid (TPA) and adipic acid, one
The amount of denier any material therein changes, and its technique will change, and this also illustrates present preparation side on the one hand
Method is too single, and applicability is narrower, and the uniformity of product quality is poor.
The content of the invention
In view of this, the invention provides the preparation method of polyester resin for powder coating, this preparation method is by by two
In first acid and dibasic alcohol ester course of reaction, the acid number and viscosity number of a certain reaction node in course of reaction are fixed, to prepare
Method provides diversity.
The preparation method of polyester resin for powder coating, the preparation method includes：
By neopentyl glycol and cyclohexanedimethanol, reactor is put into, it is heated, programming rate is 3-5 DEG C/min, together
When it is stirred, mixing speed is 60-100r/min, rises to 70-90 DEG C, insulation, is melted completely to dihydric alcohol, toward reaction
Terephthalic acid (TPA) and adipic acid are added in kettle, while adding catalyst, mixing speed is adjusted to 260-300r/min, heating speed
Degree is adjusted to for 5-8 DEG C/min, be warming up to 205-210 DEG C, make dihydric alcohol cooling for reflux in a kettle., make binary acid and dihydric alcohol
The water that esterification is produced is fractionated, and is incubated 2-2.5 hours, is come out into reactor without distilled water, is added stabilizer, is warming up to
240-245 DEG C, insulation becomes clarification to reaction solution completely, measures its acid number, acid number is reached 6-11mgKOH/g；
Stop heating, reaction solution is naturally cooled to 215-218 DEG C, into reactor add M-phthalic acid with oneself two
Acid, 350-400r/min is adjusted to by mixing speed, is heated simultaneously, and programming rate is 1-2 DEG C/min, temperature is risen to 245-250
DEG C, 3-3.5h is incubated, cools 215-220 DEG C, is vacuumized under the inert conditions of nitrogen, the acid number of polyester resin is surveyed, makes
Acid number reach 43-46mgKOH/g, viscosity number reaches 60-62p/200 DEG C, stops vacuumizing.
Preferably, in addition to by the reactor for exhausting vacuum, add accelerator, be stirred, stir, material from
Reactor is removed, and target acid number 30-33mgKOH/g, target viscosities value reaches 59-61p/200 DEG C.
Preferably, the alcoholic extract hydroxyl group of the glycol and cyclohexanedimethanol and M-phthalic acid and the carboxyl ratio of adipic acid
It is worth for 1.08-1.1.
Preferably, the catalyst is Mono-n-butyltin.
Preferably, the stabilizer is triphenyl phosphite.
Preferably, the accelerator is benzoyl peroxide methyl ether.
The preparation method for the polyester resin for powder coating that the present invention is provided, this preparation method is by by binary acid and binary
In alcohol esterification course of reaction, the acid number and viscosity number of a certain reaction node in course of reaction are fixed, provided for preparation method
Diversity.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is a part of embodiment of the invention, rather than whole embodiments.Based on the implementation in the present invention
Example, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made is belonged to
The scope of protection of the invention.
It should be appreciated that ought be in this specification and in the appended claims in use, term " comprising " and "comprising" be indicated
Described feature, entirety, step, operation, the presence of element and/or component, but be not precluded from one or more of the other feature, it is whole
Body, step, operation, element, component and/or its presence or addition for gathering.
It will be further appreciated that, the term "and/or" used in description of the invention and appended claims is
Refer to any combinations of one or more of the associated item listed and be possible to combination, and including these combinations.
Embodiment 1
The preparation method of polyester resin for powder coating, preparation method includes：By neopentyl glycol and cyclohexanedimethanol,
Reactor is put into, it is heated, programming rate is 3 DEG C/min, while being stirred to it, mixing speed is 60r/min, is risen to
90 DEG C, insulation is melted completely to dihydric alcohol, and terephthalic acid (TPA) and adipic acid are added into reactor, while catalyst is added,
Mixing speed is adjusted to 260r/min, programming rate is adjusted to for 8 DEG C/min, be warming up to 210 DEG C, make dihydric alcohol cold in a kettle.
But flow back, be fractionated the water that binary acid and dibasic alcohol ester are produced, be incubated 2.5 hours, go out into reactor without distilled water
Come, add stabilizer, be warming up to 245 DEG C, insulation becomes clarification to reaction solution completely, measures its acid number, acid number is reached 6mgKOH/
g；
Stop heating, reaction solution is naturally cooled to 218 DEG C, M-phthalic acid and adipic acid are added into reactor, will
Mixing speed is adjusted to 400r/min, heats simultaneously, and programming rate is 2 DEG C/min, temperature is risen to 250 DEG C, is incubated 3.5h, cooling
215 DEG C, vacuumized under the inert conditions of nitrogen, survey the acid number of polyester resin, be allowed to acid number and reach 46mgKOH/g, glued
Angle value reaches 62p/200 DEG C, stops vacuumizing.
By in the reactor for exhausting vacuum, accelerator is added, is stirred, stirs, material is removed from reactor, mesh
Acid number 30mgKOH/g is marked, target viscosities value reaches 61p/200 DEG C.
The carboxyl ratio of the alcoholic extract hydroxyl group of glycol and cyclohexanedimethanol and M-phthalic acid and adipic acid is 1.08.
Embodiment 2
The preparation method of polyester resin for powder coating, preparation method includes：By neopentyl glycol and cyclohexanedimethanol,
Reactor is put into, it is heated, programming rate is 5 DEG C/min, while being stirred to it, mixing speed is 100r/min, is risen
To 70 DEG C, insulation is melted completely to dihydric alcohol, and terephthalic acid (TPA) and adipic acid are added into reactor, while adding only son
Base tin oxide, 300r/min is adjusted to by mixing speed, and programming rate is adjusted to for 5 DEG C/min, be warming up to 205 DEG C, make dihydric alcohol exist
Cooling for reflux in reactor, is fractionated the water that binary acid and dibasic alcohol ester are produced, 2.5 hours is incubated, into reactor
Come out without distilled water, add triphenyl phosphite, be warming up to 245 DEG C, insulation becomes clarification to reaction solution completely, measures its acid number,
Acid number is set to reach 11mgKOH/g；
Stop heating, reaction solution is naturally cooled to 215 DEG C, M-phthalic acid and adipic acid are added into reactor, will
Mixing speed is adjusted to 350r/min, heats simultaneously, and programming rate is 1 DEG C/min, temperature is risen to 245 DEG C, is incubated 3h, cooling
220 DEG C, vacuumized under the inert conditions of nitrogen, survey the acid number of polyester resin, be allowed to acid number and reach 43mgKOH/g, glued
Angle value reaches 60p/200 DEG C, stops vacuumizing.
By in the reactor for exhausting vacuum, benzoyl peroxide methyl ether is added, is stirred, stirs, material is from reactor
Remove, target acid number 33mgKOH/g, target viscosities value reaches 59p/200 DEG C.
The carboxyl ratio of the alcoholic extract hydroxyl group of glycol and cyclohexanedimethanol and M-phthalic acid and adipic acid is 1.1.
Embodiment 3
The preparation method of polyester resin for powder coating, preparation method includes：By neopentyl glycol and cyclohexanedimethanol,
Reactor is put into, it is heated, programming rate is 4 DEG C/min, while being stirred to it, mixing speed is 80r/min, is risen to
85 DEG C, insulation is melted completely to dihydric alcohol, and terephthalic acid (TPA) and adipic acid are added into reactor, while adding monobutyl
Tin oxide, 375r/min is adjusted to by mixing speed, and programming rate is adjusted to for 6 DEG C/min, be warming up to 208 DEG C, make dihydric alcohol anti-
Cooling for reflux in kettle is answered, the water that binary acid and dibasic alcohol ester are produced is fractionated, is incubated 2.2 hours, the nothing into reactor
Distilled water comes out, and adds triphenyl phosphite, is warming up to 242 DEG C, insulation becomes clarification to reaction solution completely, measures its acid number, makes
Acid number reaches 9mgKOH/g；
Stop heating, reaction solution is naturally cooled to 217 DEG C, M-phthalic acid and adipic acid are added into reactor, will
Mixing speed is adjusted to 380r/min, heats simultaneously, and programming rate is 1.5 DEG C/min, temperature is risen to 247 DEG C, is incubated 3.2h, drop
216 DEG C of temperature, is vacuumized under the inert conditions of nitrogen, is surveyed the acid number of polyester resin, is allowed to acid number and reaches 44mgKOH/g,
Viscosity number reaches 61p/200 DEG C, stops vacuumizing.
By in the reactor for exhausting vacuum, benzoyl peroxide methyl ether is added, is stirred, stirs, material is from reactor
Remove, target acid number 32mgKOH/g, target viscosities value reaches 60p/200 DEG C.
The carboxyl ratio of the alcoholic extract hydroxyl group of glycol and cyclohexanedimethanol and M-phthalic acid and adipic acid is 1.09.
Step in present invention method can be sequentially adjusted, merged and deleted according to actual needs.
It is described in detail herein, applies specific case and the principle and embodiment of the present invention are explained
State, above example is only intended to the method and its core concept for helping to understand the present invention；Simultaneously for the general skill of this area
Art personnel, according to the thought of the present invention, will change in specific embodiments and applications, in summary, this
Description should not be construed as limiting the invention.
It is apparent to those skilled in the art that, for convenience and simplicity of description, the system of foregoing description
With the specific work process of unit, the corresponding process in preceding method embodiment is may be referred to, be will not be repeated here.
Claims (6)
1. the preparation method of polyester resin for powder coating, it is characterised in that the preparation method includes：
By neopentyl glycol and cyclohexanedimethanol, reactor is put into, it is heated, programming rate is 3-5 DEG C/min, while right
It is stirred, and mixing speed is 60-100r/min, rises to 70-90 DEG C, insulation is melted, into reactor completely to dihydric alcohol
Terephthalic acid (TPA) and adipic acid are added, while adding catalyst, mixing speed 260-300r/min is adjusted to, programming rate is adjusted
Most 5-8 DEG C/min, 205-210 DEG C is warming up to, makes dihydric alcohol cooling for reflux in a kettle., makes binary acid and dibasic alcohol ester
The water of generation is fractionated, and is incubated 2-2.5 hours, is come out into reactor without distilled water, is added stabilizer, is warming up to 240-
245 DEG C, insulation becomes clarification to reaction solution completely, measures its acid number, acid number is reached 6-11mgKOH/g；
Stop heating, reaction solution is naturally cooled to 215-218 DEG C, M-phthalic acid and adipic acid are added into reactor, will
Mixing speed is adjusted to 350-400r/min, heats simultaneously, and programming rate is 1-2 DEG C/min, temperature is risen to 245-250 DEG C, guarantor
Warm 3-3.5h, cools 215-220 DEG C, is vacuumized under the inert conditions of nitrogen, surveys the acid number of polyester resin, is allowed to acid number
43-46mgKOH/g is reached, viscosity number reaches 60-62p/200 DEG C, stop vacuumizing.
2. preparation method as claimed in claim 1, it is characterised in that：Also include, by the reactor for exhausting vacuum, adding and promoting
Enter agent, be stirred, stir, material is removed from reactor, target acid number 30-33mgKOH/g, target viscosities value reaches
59-61p/200℃。
3. preparation method as claimed in claim 1, it is characterised in that：The alcoholic extract hydroxyl group of the glycol and cyclohexanedimethanol with
The carboxyl ratio of M-phthalic acid and adipic acid is 1.08-1.1.
4. preparation method as claimed in claim 1, it is characterised in that：The catalyst is Mono-n-butyltin.
5. preparation method as claimed in claim 1, it is characterised in that：The stabilizer is triphenyl phosphite.
6. preparation method as claimed in claim 1, it is characterised in that：The accelerator is benzoyl peroxide methyl ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710448206.4A CN107118337A (en) | 2017-06-14 | 2017-06-14 | A kind of preparation method of polyester resin for powder coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710448206.4A CN107118337A (en) | 2017-06-14 | 2017-06-14 | A kind of preparation method of polyester resin for powder coating |
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| Publication Number | Publication Date |
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| CN107118337A true CN107118337A (en) | 2017-09-01 |
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| CN201710448206.4A Pending CN107118337A (en) | 2017-06-14 | 2017-06-14 | A kind of preparation method of polyester resin for powder coating |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000256582A (en) * | 1999-03-08 | 2000-09-19 | Nippon Ester Co Ltd | Production of polyester resin for powdered coating material |
| CN103304790A (en) * | 2013-06-06 | 2013-09-18 | 广东伊诗德新材料科技有限公司 | Polyester resin for outdoor aluminum profile heat transfer printing powder coating and preparation method thereof |
| CN103396537A (en) * | 2013-07-17 | 2013-11-20 | 芜湖艾力特新材料科技有限公司 | Preparation method of high temperature yellowing resistant thermosetting polyester resin |
| CN105601892A (en) * | 2015-11-17 | 2016-05-25 | 广东伊诗德新材料科技有限公司 | Polyester resin for powdery coating and with low volatile component content and preparation method thereof |
-
2017
- 2017-06-14 CN CN201710448206.4A patent/CN107118337A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000256582A (en) * | 1999-03-08 | 2000-09-19 | Nippon Ester Co Ltd | Production of polyester resin for powdered coating material |
| CN103304790A (en) * | 2013-06-06 | 2013-09-18 | 广东伊诗德新材料科技有限公司 | Polyester resin for outdoor aluminum profile heat transfer printing powder coating and preparation method thereof |
| CN103396537A (en) * | 2013-07-17 | 2013-11-20 | 芜湖艾力特新材料科技有限公司 | Preparation method of high temperature yellowing resistant thermosetting polyester resin |
| CN105601892A (en) * | 2015-11-17 | 2016-05-25 | 广东伊诗德新材料科技有限公司 | Polyester resin for powdery coating and with low volatile component content and preparation method thereof |
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Application publication date: 20170901 |