CN106084190A - The preparation technology of the polyester resin that a kind of low temperature curing type is used for powder coating - Google Patents
The preparation technology of the polyester resin that a kind of low temperature curing type is used for powder coating Download PDFInfo
- Publication number
- CN106084190A CN106084190A CN201610512665.XA CN201610512665A CN106084190A CN 106084190 A CN106084190 A CN 106084190A CN 201610512665 A CN201610512665 A CN 201610512665A CN 106084190 A CN106084190 A CN 106084190A
- Authority
- CN
- China
- Prior art keywords
- low temperature
- polyester resin
- powder coating
- preparation technology
- curing type
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Classifications
-
- 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
- C08G63/199—Acids or hydroxy compounds containing cycloaliphatic rings
-
- 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
- C08G63/78—Preparation processes
-
- 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
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
-
- 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
Abstract
The invention provides the preparation technology of a kind of low temperature curing type polyester resin used for powder coating, first: the alcohol of formula ratio is put into reactor, and mixing speed is 40～90r/min, is heated to 120～135 DEG C, treat that alcohol is completely melt, rotating speed is risen to the rotating speed stirring of 130～150r/min, puts into catalyst for the first time, be warming up to 190 DEG C, it is warming up to 245～250 DEG C with the programming rate of 12 DEG C/60min, insulation 120min, acid number 16～19mgKOH/g, viscosity is 10～12P/160 DEG C；Secondly: becoming clear to solution, be cooled to 215～225 DEG C, second time puts into the acid of residue formula, is warming up to 240～245 DEG C；Again: becoming clear to solution, cool the temperature to 220～225 DEG C, vacuum is 0.1 atmospheric pressure, controls acid number 2～3mgKOH/g, viscosity maintains 52～55P/200 DEG C；Last: the water-repelling agent of formula ratio to be added in solution, 190～195 DEG C of insulation 30min, acid number is 70～72mgKOH/g, and viscosity maintains 23～25P/200 DEG C, discharging.
Description
Technical field
The present invention relates to technical field of coatings, particularly relate to the system of a kind of low temperature curing type polyester resin used for powder coating
Standby technique.
Background technology
Powdery paints, with the superior function of its environmental protection and economy, is widely used in the external coating of various metalwork.Along with economy
The development of society, people are more and more deep to the concept of environmental protection, and the range of application of powdery paints is the most increasing, and people are to powder
The requirement of the condition of cure of coating is more and more higher.The condition of cure of common powdery paints is mostly that baking temperature is higher, dries
The roasting time is longer, and this kind of technique easily causes the waste of the energy.Therefore, from saving the energy, from the point of view of reducing cost, low temperature
Curing type powdery paints has wide market prospect.But, low temperature curing type powdery paints it is crucial that low temperature curing resin.
Summary of the invention
In view of this, the preparation technology of the polyester resin providing a kind of low temperature curing type used for powder coating it is a need for.
The preparation technology of the polyester resin that a kind of low temperature curing type is used for powder coating, comprises the following steps:
First stage: the alcohol of formula ratio is put into reactor, and mixing speed is 40～90r/min, is heated to 120～135
DEG C, treat that alcohol is completely melt, rotating speed is risen to the rotating speed stirring of 130～150r/min, puts into the catalysis of acid and formula ratio for the first time
Agent, is warming up to 190 DEG C, is warming up to 245～250 DEG C with the programming rate of 12 DEG C/60min, be incubated 120min, maintain acid number 16～
19mgKOH/g, viscosity maintains 10～12P/160 DEG C.
Second stage: becoming clear to solution, be cooled to 215～225 DEG C, second time puts into the acid of residue formula, is warming up to 240
～245 DEG C.
Phase III: becoming clear to solution, cool the temperature to 220～225 DEG C, carry out evacuation, vacuum is at 0.1 air
Pressure, the pumpdown time is 4.5～5h, controls acid number 2～3mgKOH/g, and viscosity maintains 52～55P/200 DEG C.
Fourth stage: added by the cross-linking agent of formula ratio in solution, 190～195 DEG C of insulation 30min, acid number controls 70
～72mgKOH/g, viscosity maintains 23～25P/200 DEG C of discharging.
Preferably, what the acid that the described first stage puts into was p-phthalic acid or p-phthalic acid with cyclohexane cyclohexanedimethanodibasic is mixed
Compound.
Preferably, the acid that the described first stage puts into is 225～235 parts.
Preferably, the alcohol of described input be neopentyl glycol, 1,6-hexanediol, 2-ethyl-2-butyl-1,3-PD, ring
Hexane dimethanol.
Preferably, the amount of described alcohol is 170～180 parts.
Preferably, the acid that described second stage puts into is 25～45 parts.
Preferably, described first stage holding temperature is 247 DEG C.
Preferably, described second stage holding temperature is 242 DEG C.
Preferably, described fourth stage holding temperature is 193 DEG C.
Preferably, the amount of described input acid altogether is 250～280 parts.
The beneficial effects of the present invention is: provide a kind of low temperature curing polyester resin preparation technology, this technique is simple, holds
Easily realize, the products application mainly produced in low temperature cured powder coating, energy-conserving and environment-protective.
Detailed description of the invention
Embodiment 1
The preparation technology of the polyester resin that a kind of low temperature curing type is used for powder coating, acid be p-phthalic acid or to benzene
The mixture of dioctyl phthalate and cyclohexane cyclohexanedimethanodibasic, alcohol be neopentyl glycol, 1,6-hexanediol, 2-ethyl-2-butyl-1,3-third
Glycol, cyclohexanedimethanol, catalyst be Mono-n-butyltin, cross-linking agent is organosilicon.Comprise the following steps:
First stage, by the neopentyl glycols of 170 parts, 1,6-hexanediol, 2-ethyl-2-butyl-1,3-PD, hexamethylene
Dimethanol puts into reactor, and mixing speed is 40r/min, is heated to 120 DEG C, treats that alcohol is completely melt, rotating speed is risen to 130r/
The rotating speed stirring of min, the p-phthalic acid of first time input 225 parts or p-phthalic acid and cyclohexane cyclohexanedimethanodibasic and formula ratio
Catalyst, catalyst is Mono-n-butyltin, is warming up to 190 DEG C, is warming up to 245 DEG C with the programming rate of 12 DEG C/60min, protects
Temperature 120min, maintains acid number 16mgKOH/g, and viscosity maintains 10P/160 DEG C.
Second stage: becoming clear to solution, be cooled to 215 DEG C, second time puts into the acid of residue formula 25 parts, is warming up to 240
℃。
Phase III: becoming clear to solution, cool the temperature to 220 DEG C, carry out evacuation, vacuum, at 0.1 atmospheric pressure, is taken out
Vacuum time is 4.5h, controls acid number 2mgKOH/g, and viscosity maintains 52P/200 DEG C.
Fourth stage: being added in solution by the cross-linking agent of formula ratio, cross-linking agent is organosilicon, at temperature is 190 DEG C, protects
Temperature 30min, acid number controls at 70KOH/g, and viscosity maintains 23P/200 DEG C of discharging.
Embodiment 2
The alcohol of 180 parts are put into reactor, and mixing speed is 90r/min, is heated to 135 DEG C, treats that alcohol is completely melt, will turn
Speed rises to the rotating speed stirring of 150r/min, puts into acid and the catalyst of formula ratio of 235 parts for the first time, and catalyst is monobutyl oxygen
Change stannum, be warming up to 190 DEG C, be warming up to 250 DEG C with the programming rate of 12 DEG C/60min, be incubated 120min, maintain acid number
19mgKOH/g, viscosity maintains 12P/160 DEG C.
Second stage: becoming clear to solution, be cooled to 225 DEG C, second time puts into the acid of residue 45 parts, is warming up to 240～245
℃。
Phase III: becoming clear to solution, cool the temperature to 225 DEG C, carry out evacuation, vacuum, at 0.1 atmospheric pressure, is taken out
Vacuum time is 5h, controls acid 3mgKOH/g, and viscosity maintains 55P/200 DEG C.
Fourth stage: added by the cross-linking agent of formula ratio in solution, 195 DEG C of insulation 30min, acid number controls at 72mgKOH/
G, viscosity maintains 25P/200 DEG C, discharging.
Embodiment 3
The alcohol of formula ratio is put into reactor, and mixing speed is 60r/min, is heated to 130 DEG C, treats that alcohol is completely melt, will
Rotating speed rises to the rotating speed stirring of 140r/min, puts into for the first time the catalyst of acid and formula ratio, is warming up to 190 DEG C, with 12 DEG C/
The programming rate of 60min is warming up to 247 DEG C, is incubated 120min, maintains acid number 18mgKOH/g, and viscosity maintains 11P/160 DEG C.
Second stage: becoming clear to solution, be cooled to 220 DEG C, second time puts into the acid of residue formula, is warming up to 242 DEG C.
Phase III: becoming clear to solution, cool the temperature to 222 DEG C, carry out evacuation, vacuum, at 0.1 atmospheric pressure, is taken out
Vacuum time is 4.8h, controls acid number 2.5mgKOH/g, and viscosity maintains 54P/200 DEG C.
Fourth stage: added by the cross-linking agent of formula ratio in solution, 193 DEG C of insulation 30min, acid number controls at 71mgKOH/
G, viscosity maintains 24P/200 DEG C, discharging.
Having the beneficial effects that of this technique: provide a kind of low temperature curing polyester resin preparation technology, this technique is simple, holds
Easily realize, the products application mainly produced in low temperature cured powder coating, energy-conserving and environment-protective.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (10)
1. the preparation technology of the polyester resin that a low temperature curing type is used for powder coating, it is characterised in that comprise the following steps:
First stage: the alcohol of formula ratio is put into reactor, and mixing speed is 40～90r/min, is heated to 120～135 DEG C, treats
Alcohol is completely melt, rotating speed rises to the rotating speed stirring of 130～150r/min, puts into the catalyst of acid and formula ratio for the first time, rise
Temperature to 190 DEG C, be warming up to 245～250 DEG C with the programming rate of 12 DEG C/60min, be incubated 120min, maintain acid number 16～
19mgKOH/g, viscosity maintains 10～12P/160 DEG C；
Second stage: becoming clear to solution, be cooled to 215～225 DEG C, second time puts into the acid of residue formula, be warming up to 240～
245℃；
Phase III: become clear to solution, cool the temperature to 220～225 DEG C, carry out evacuation, vacuum at 0.1 atmospheric pressure,
Pumpdown time is 4.5～5h, controls acid number 2～3mgKOH/g, and viscosity maintains 52～55P/200 DEG C；
Fourth stage: the water-repelling agent of formula ratio is added in solution, 190～195 DEG C of insulation 30min, acid number control 70～
72mgKOH/g, viscosity maintains 23～25P/200 DEG C, discharging.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 1 is used for powder coating, it is characterised in that:
The acid that the described first stage puts into is the mixture of p-phthalic acid or p-phthalic acid and cyclohexane cyclohexanedimethanodibasic.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 2 is used for powder coating, it is characterised in that:
The acid that the described first stage puts into is 225～235 parts.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 1 is used for powder coating, it is characterised in that:
The alcohol of described input is neopentyl glycol, 1,6-HD, 2-ethyl-2-butyl-1,3-propylene glycol, cyclohexanedimethanol.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 4 is used for powder coating, it is characterised in that:
The amount of described alcohol is 170～180 parts.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 1 is used for powder coating, it is characterised in that:
The acid that described second stage puts into is 25～45 parts.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 1 is used for powder coating, it is characterised in that:
Described first stage holding temperature is 247 DEG C.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 1 is used for powder coating, it is characterised in that:
Described second stage holding temperature is 242 DEG C.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 1 is used for powder coating, it is characterised in that:
Described fourth stage holding temperature is 193 DEG C.
The preparation technology of the polyester resin that low temperature curing type the most according to claim 1 is used for powder coating, its feature exists
In: the amount of described input acid altogether is 250～280 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610512665.XA CN106084190A (en) | 2016-06-30 | 2016-06-30 | The preparation technology of the polyester resin that a kind of low temperature curing type is used for powder coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610512665.XA CN106084190A (en) | 2016-06-30 | 2016-06-30 | The preparation technology of the polyester resin that a kind of low temperature curing type is used for powder coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106084190A true CN106084190A (en) | 2016-11-09 |
Family
ID=57213402
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610512665.XA Pending CN106084190A (en) | 2016-06-30 | 2016-06-30 | The preparation technology of the polyester resin that a kind of low temperature curing type is used for powder coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106084190A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000178474A (en) * | 1998-12-18 | 2000-06-27 | Nippon Ester Co Ltd | Production of polyester resin for powder coating |
| CN101775127A (en) * | 2009-12-30 | 2010-07-14 | 中国纺织科学研究院 | Hydrophobic modified polyester and preparation method thereof |
| CN102718952A (en) * | 2012-07-04 | 2012-10-10 | 佛山市顺德区伊诗德新材料科技有限公司 | Polyester resin for low-temperature cured powder paint and preparation method of polyester resin |
| CN104311804A (en) * | 2014-10-31 | 2015-01-28 | 安徽神剑新材料股份有限公司 | Preparation method of polyester resin |
| CN104387569A (en) * | 2014-10-31 | 2015-03-04 | 安徽神剑新材料股份有限公司 | Polyester resin |
| CN104497289A (en) * | 2015-01-08 | 2015-04-08 | 黄山市向荣新材料有限公司 | Low-temperature-curing polyester resin for powder paints, powder paint using resin and preparation method thereof |
-
2016
- 2016-06-30 CN CN201610512665.XA patent/CN106084190A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000178474A (en) * | 1998-12-18 | 2000-06-27 | Nippon Ester Co Ltd | Production of polyester resin for powder coating |
| CN101775127A (en) * | 2009-12-30 | 2010-07-14 | 中国纺织科学研究院 | Hydrophobic modified polyester and preparation method thereof |
| CN102718952A (en) * | 2012-07-04 | 2012-10-10 | 佛山市顺德区伊诗德新材料科技有限公司 | Polyester resin for low-temperature cured powder paint and preparation method of polyester resin |
| CN104311804A (en) * | 2014-10-31 | 2015-01-28 | 安徽神剑新材料股份有限公司 | Preparation method of polyester resin |
| CN104387569A (en) * | 2014-10-31 | 2015-03-04 | 安徽神剑新材料股份有限公司 | Polyester resin |
| CN104497289A (en) * | 2015-01-08 | 2015-04-08 | 黄山市向荣新材料有限公司 | Low-temperature-curing polyester resin for powder paints, powder paint using resin and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 叶扬祥等: "《涂装技术实用手册》", 30 June 2003 * |
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Application publication date: 20161109 |