CN109957300A - A kind of preparation method of more official's polyester acrylates - Google Patents
A kind of preparation method of more official's polyester acrylates Download PDFInfo
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- CN109957300A CN109957300A CN201711340779.1A CN201711340779A CN109957300A CN 109957300 A CN109957300 A CN 109957300A CN 201711340779 A CN201711340779 A CN 201711340779A CN 109957300 A CN109957300 A CN 109957300A
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- polyester acrylates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/01—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to unsaturated polyesters
-
- 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
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
- C09D11/104—Polyesters
-
- 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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Polyesters Or Polycarbonates (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of preparation method of more official's polyester acrylates, includes the following steps, S1: polyalcohol, polyacid, catalyst, antioxidant and solvent being added in reaction kettle and reacted；S2: being to slowly warm up to 170 DEG C, and heat preservation measures the acid value of reaction system, until acid value≤3mgKOH/g；S3: 50 DEG C are cooled to and is reacted hereinafter, acrylic acid, catalyst, polymerization inhibitor, antioxidant and solvent are added in reaction kettle, the acid value of reaction system is measured, until acid value≤15mgKOH/g, cooling i.e. much official's polyester acrylate, has curing rate fast, environment-protecting and non-poisonous, the low advantage of production cost.
Description
Technical field
The present invention relates to chemical fields, more particularly, to a kind of preparation method of more official's polyester acrylates.
Background technique
UV-curing technology is a kind of efficient, energy-saving and environmental protection, good surface treatment technology of material.Its solidification rate
It is current various coating, ink, most fast in adhesive, is able to satisfy the automated production requirement of large-scale pipeline, photocuring
Product is applicable to a variety of substrates such as paper, metal, plastics, glass, timber.Without volatile solvent, reduce to environment and
The harm of human body.Attention with countries in the world to atmosphere discharge VOC, the superiority of photocuring product seem more prominent.
Polyester acrylate is a kind of common photo curable oligomer.The polyester acrylate of low-viscosity can be used as
Oligomer also can be used as reactive diluent use.Compared with conventional single-activity diluent, polyester acrylate can basis
Use demand adjusts the structure of polyester portion, brings more changeable performance and more flexible use space.
Existing polyester acrylate synthetic method be usually reacted direct discharging, or react except after solvent out
Material.This method can remain the auxiliary agents such as reacting middle catalyst antioxidant and remaining acrylic acid.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation methods of more official's polyester acrylates.
Technical solution provided by the invention is as follows: a kind of preparation method of more official's polyester acrylates includes the following steps,
S1: polyalcohol, polyacid, catalyst, antioxidant and solvent are added in reaction kettle and reacted；
S2: being to slowly warm up to 170 DEG C, and heat preservation measures the acid value of reaction system, until acid value≤3mgKOH/g；
S3: 50 DEG C are cooled to and is reacted hereinafter, acrylic acid, catalyst, polymerization inhibitor, antioxidant and solvent are added in reaction kettle, is surveyed
The acid value of quantitative response system cools the temperature to room temperature i.e. much official's polyester acrylate until acid value≤15mgKOH/g.
Further, in the step S1, polyalcohol is the mixture of trimethylolpropane and any ratio of neopentyl glycol.
Further, in the step S1, polyacid is the mixture of adipic acid and any ratio of maleic anhydride.
Further, in the step S1, reaction temperature is 110-120 DEG C, and the reaction time is 1-1.5 hours.
Further, in the step S1, catalyst is methane sulfonic acid.
Further, in the step S1, antioxidant is hypophosphorous acid.
Further, in the step S3, reaction temperature is 110-120 DEG C, and the reaction time is 4-4.5 hours.
Further, in the step S3, catalyst is methane sulfonic acid.
Further, in the step S3, polymerization inhibitor is p-hydroxyanisole and copper chloride.
Further, in the step S3, antioxidant is hypophosphorous acid.
The present invention compared with prior art, has following advantages: more official's polyester acrylates prepared by the present invention can draw in light
Hair agent coexists down, through ultraviolet radiation, free radical polymerization can occur rapidly, thus crosslinking curing.The resin is mainly used as in light
It is coating material solidified, light-curable ink.It is suitable for plastic cement, the photocuring coating of paper.Extremely low cure shrinkage can be provided for cured film,
Excellent adhesive attraction and flexibility.It is a kind of with good prospect and the superior light-cured resin of comprehensive performance.
More official's polyester acrylates of method preparation of the invention, curing rate is fast, and flexibility is good, when the preparation process period
Between it is short.Improve the brittleness of resin to a certain extent, modified resin has curing rate fast, and viscosity is low, and flexibility is good
Feature.The chemical resistance of UV curing system is effectively increased, while flexility is good, product has good coating film gloss
Degree and flexibility, environment-protecting and non-poisonous, production cost is low.
Specific embodiment
The preferred embodiments of the present invention will be described in detail below, so that advantages and features of the invention are easier to by this field skill
Art personnel understand, to make apparent define to protection scope of the present invention.
Embodiment 1
A kind of preparation method of more official's polyester acrylates, comprising the following steps:
By 32.7g trimethylolpropane, 8.8g neopentyl glycol, 28.1g adipic acid, 4.2g cis-butenedioic anhydride, 0.2g methane sulfonic acid, 0.08g
Hypophosphorous acid, 3.3g toluene are sequentially added into the four-hole boiling flask with stirring, are warming up to 110 DEG C, in 115 DEG C of heat preservation 1.5h, heating
To 170 DEG C, 3 hours are kept the temperature at 170 DEG C, measures acid value less than 3mgKOH/g.50 DEG C are cooled to, 40.2g acrylic acid, 2.5g is added
Methane sulfonic acid, 0.025g p-hydroxyanisole, 0.09g copper chloride, 0.75g hypophosphorous acid, 37.3g toluene, in 115 DEG C of reaction 4h,
Acid value is measured less than 15 mgKOH/g, cooling the temperature to room temperature can much official's polyester acrylate.
Embodiment 2
A kind of preparation method of more official's polyester acrylates, comprising the following steps:
By 32.7g trimethylolpropane, 8.8g neopentyl glycol, 28.1g adipic acid, 4.2g cis-butenedioic anhydride, 0.2g methane sulfonic acid, 0.08g
Hypophosphorous acid, 3.3g toluene are sequentially added into the four-hole boiling flask with stirring, are warming up to 110 DEG C, in 120 DEG C of heat preservation 1h, are warming up to
170 DEG C, 3 hours are kept the temperature at 170 DEG C, measures acid value less than 3mgKOH/g.50 DEG C are cooled to, 40.2g acrylic acid, 2.5g first is added
Base sulfonic acid, 0.025g p-hydroxyanisole, 0.09g copper chloride, 0.75g hypophosphorous acid, 37.3g toluene, in 110 DEG C of reaction 4.5h,
Acid value is measured less than 15 mgKOH/g, cooling the temperature to room temperature can much official's polyester acrylate.
Embodiment 3
A kind of preparation method of more official's polyester acrylates, comprising the following steps:
By 32.7g trimethylolpropane, 8.8g neopentyl glycol, 28.1g adipic acid, 4.2g cis-butenedioic anhydride, 0.2g methane sulfonic acid, 0.08g
Hypophosphorous acid, 3.3g toluene are sequentially added into the four-hole boiling flask with stirring, are warming up to 110 DEG C, in 115 DEG C of heat preservation 1h, are warming up to
170 DEG C, 3 hours are kept the temperature at 170 DEG C, measures acid value less than 3mgKOH/g.50 DEG C are cooled to, 40.2g acrylic acid, 2.5g first is added
Base sulfonic acid, 0.025g p-hydroxyanisole, 0.09g copper chloride, 0.75g hypophosphorous acid, 37.3g toluene, in 110 DEG C of reaction 4.5h,
Acid value is measured less than 15 mgKOH/g, cooling the temperature to room temperature can much official's polyester acrylate.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination, letter
Change, should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of more official's polyester acrylates, which is characterized in that include the following steps,
S1: polyalcohol, polyacid, catalyst, antioxidant and solvent are added in reaction kettle and reacted；
S2: being to slowly warm up to 170 DEG C, and heat preservation measures the acid value of reaction system, until acid value≤3mgKOH/g；
S3: 50 DEG C are cooled to and is reacted hereinafter, acrylic acid, catalyst, polymerization inhibitor, antioxidant and solvent are added in reaction kettle, is surveyed
The acid value of quantitative response system cools the temperature to room temperature i.e. much official's polyester acrylate until acid value≤15mgKOH/g.
2. a kind of preparation method of more official's polyester acrylates according to claim 1, which is characterized in that the step S1
In, polyalcohol is the mixture of trimethylolpropane and any ratio of neopentyl glycol.
3. a kind of preparation method of more official's polyester acrylates according to claim 1, which is characterized in that the step S1
In, polyacid is the mixture of adipic acid and any ratio of maleic anhydride.
4. a kind of preparation method of more official's polyester acrylates according to claim 1, which is characterized in that the step S1
In, reaction temperature is 110-120 DEG C, and the reaction time is 1-1.5 hours.
5. a kind of preparation method of more official's polyester acrylates according to claim 1, which is characterized in that the step S1
In, catalyst is methane sulfonic acid.
6. a kind of preparation method of more official's polyester acrylates according to claim 1, which is characterized in that the step S1
In, antioxidant is hypophosphorous acid.
7. a kind of preparation method of more official's polyester acrylates according to claim 1, which is characterized in that the step S3
In, reaction temperature is 110-120 DEG C, and the reaction time is 4-4.5 hours.
8. a kind of preparation method of more official's polyester acrylates according to claim 1, which is characterized in that the step S3
In, catalyst is methane sulfonic acid.
9. a kind of preparation method of more official's polyester acrylates according to claim 1, which is characterized in that the step S3
In, polymerization inhibitor is p-hydroxyanisole and copper chloride.
10. -9 described in any item a kind of preparation methods of more official's polyester acrylates according to claim 1, which is characterized in that
In the step S3, antioxidant is hypophosphorous acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711340779.1A CN109957300A (en) | 2017-12-14 | 2017-12-14 | A kind of preparation method of more official's polyester acrylates |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711340779.1A CN109957300A (en) | 2017-12-14 | 2017-12-14 | A kind of preparation method of more official's polyester acrylates |
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| Publication Number | Publication Date |
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| CN109957300A true CN109957300A (en) | 2019-07-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711340779.1A Withdrawn CN109957300A (en) | 2017-12-14 | 2017-12-14 | A kind of preparation method of more official's polyester acrylates |
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| CN (1) | CN109957300A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716647A (en) * | 2022-04-07 | 2022-07-08 | 广州今朝环保材料有限公司 | Photocuring acrylate and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030745A (en) * | 2012-12-07 | 2013-04-10 | 武汉工程大学 | Water-based photo-cured unsaturated polyester and preparation method thereof |
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2017
- 2017-12-14 CN CN201711340779.1A patent/CN109957300A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030745A (en) * | 2012-12-07 | 2013-04-10 | 武汉工程大学 | Water-based photo-cured unsaturated polyester and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716647A (en) * | 2022-04-07 | 2022-07-08 | 广州今朝环保材料有限公司 | Photocuring acrylate and preparation method thereof |
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Application publication date: 20190702 |