CN109180920A - A kind of quick-dry type alkyd resin and preparation method thereof - Google Patents
A kind of quick-dry type alkyd resin and preparation method thereof Download PDFInfo
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- CN109180920A CN109180920A CN201811320050.2A CN201811320050A CN109180920A CN 109180920 A CN109180920 A CN 109180920A CN 201811320050 A CN201811320050 A CN 201811320050A CN 109180920 A CN109180920 A CN 109180920A
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- dimethylbenzene
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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
- C08G63/46—Polyesters chemically modified by esterification
- C08G63/48—Polyesters chemically modified by esterification by unsaturated higher fatty oils or their acids; by resin acids
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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
- C08G63/78—Preparation processes
- C08G63/81—Preparation processes using solvents
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a kind of quick-dry type alkyd resins, include following component according to weight percent wt%: oleic acid 16-32wt%, pentaerythrite 5-20wt%, glycerol 2-10wt%, phthalic anhydride 7-25wt%, benzoic acid 3-15wt%, reflux dimethylbenzene 0.5-4wt%, dimethylbenzene 20-40wt%, the reflux dimethylbenzene are solvent xylene.The present invention largely uses pentaerythrite since degree of functionality is big, and symmetrical configuration, and alkyd resin obtained is close compared with the Structure Detemination of Alkyd Resins of same type, close oil content, fast drying, hardness of paint film are higher.Replace part pentaerythrite with glycerol, further reduces costs, improve the competitiveness of enterprise.Benzoic acid is added, the degree of functionality of balance formula system stablizes production and the stemness and gloss of final resin is greatly improved.
Description
Technical field
The present invention relates to a kind of resin, specifically a kind of quick-dry type alkyd resin.
Background technique
Alkyd resin be by polyalcohol, phthalic anhydride and fatty acid or oil (fatty acid triglyceride) condensation polymerization and
At oil modified polyester resin, rich in gloss and toughness after film-forming, adhesive force is strong, and have good wearability,
Weatherability and insulating properties etc., people are never interrupted the modification of alkyd resin and the research of preparation method, catch at higher
The alkyd resin of performance is simultaneously applied to more areas.
CN 101012302A discloses a kind of for preparing the resin dimer acid modified alkyd resin and its system of paint
Make method, be to replace Activities of Some Plants oleic acid with the dimeric dibasic acid that vegetable oil acid is processed into using vegetable oil acid as raw material, with polyalcohol,
Polyacid, reflux solvent and retarder thinner are auxiliary materials synthesis.It changes traditional alkyd resins with aromatic acid polyester
The molecular structure of main chain integrates the drying mould of the oxidation polymerization between side chain and side chain, side chain and main chain, main chain and main chain
Formula, the significant raising of paint stemness of preparation, does not increase production cost compared with traditional alkyd resins.
CN 101128500A discloses a kind of alkyd resin ABCD of urethane-modified dilutable water, packet
Containing derived from polyalcohol A, by being grafted fatty acid B modified prepared by ethylenically unsaturated carboxylic acids B2, not on fatty acid B1
The structure division of the fatty acid C of grafting and multiple functionalized isocyanates D.
CN 101831234A discloses a kind of preparation method of aqueous acrylic acid modified alkyd resin coating, by following
Step is realized: (1) preparing a kind of acrylic acid modified monomer copolymer；(2) a kind of monoglyceride is prepared；It (3) will be acrylic acid modified
Monomer copolymer and monoglyceride and polyacid, polyol reaction, prepare acrylic acid modified alkyd resin；(4) by acrylic acid
Modified alkyd resin self-emulsifying, be made partial size be 20-100nm, solid content 25-35wt% water-based acrylic acid modified alcoholic acid tree
Rouge；(5) using waterborne acrylic modified alkyd resins as base-material, auxiliary agent is added, aqueous acrylic acid modified alkyd resin coating is made.
The production process of the invention shortens the reaction time, reduces production energy consumption, and product is nontoxic, non-ignitable using water as diluent, to ring
Border is pollution-free, can be applied to anti-corrosion of metal field, prepared paint film is with good mechanical performance, glossiness and has certain
Corrosion resistance.
CN 101531755A discloses a kind of modified waterborne alkyd resin of organic acid salt and preparation method thereof, the invention
Modified waterborne alkyd resin of organic acid salt is prepared using following raw materials according: 4-9 parts of dihydric alcohol, 10-17 parts of polyalcohol, and binary acid
Or 11-23 parts of acid anhydrides A, 5-10 parts of acylate, 5-10 parts of unsaturated acids B, 0.03-0.1 parts of esterification catalyst, trimellitic acid
3-8 parts of acid anhydride, 10-20 parts of dimethylbenzene, 25-35 parts of ethylene glycol monobutyl ether；Described part is mass parts.The acylate of the invention changes
Property preparation aqueous alkide resin only need that water can be directly dissolved in seldom alkali neutralization；The storage of coating made of it is stablized
Property it is good, when being used for coating metal surface, be not easy to form flash rusting, dried coating film is fast, and hardness of film is high, simple production process, cost
It is low.
CN 101967224A discloses a kind of novel stearic acid modified short oil-ity alcohol acid resin, and the resin is by essential oil
Acid, stearic acid, phthalic anhydride, benzoic acid, diethylene glycol (DEG), trimethylolpropane, glycerol, pentaerythrite and antioxidant reaction are made.The alcohol
Acid resin mainly contains stearic acid and primary hydroxyl, improves the glass transition temperature of resin, and release solvent is fast in drying process, is equipped with
A small amount of curing agent can achieve the effect that dry rapidly, while reducing reaction compartment steric hindrance, improve activity of curing reaction, add
The fast drying and forming-film speed of paint application；And the acid value of resin designs between 10-12mgKOH/g, to the wetability of powder
Preferably, and the problems such as rising by tank is not present；And the hydroxyl value of this alkyd resin, in 60mgKOH/g or so, obtained woodcare paint is water-fast
Property and gloss retention are good.
As most important one of coating synthetic resin, raw material is easy to get alkyd resin, and manufacturing process is easy to be mature, tool
There is good versatility and cheap, but phthalic resin coating has the drawback that dried coating film is slow, hardness is low, water resistance
Difference.Quick-drying alkide resin currently on the market is all generally TDI, acrylic acid, styrenated alkyd.Such quick-drying alkyd
Although resin can reach satisfied stemness, synthesis technology is complicated, extremely unstable in production, brings certain hidden danger.The present invention adopts
With the general raw material of alkyd, technological operation is simple, stable production process.Made alkyd paint has good quick-drying, gloss, hard
Degree and water resistance.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of quick-dry type alkyd resins, provide a kind of simple process, former
Expect the quick-dry type alkyd resin being easy to get.
A kind of quick-dry type alkyd resin includes following component according to weight percent wt%: oleic acid 16-32wt%, Ji Wusi
Alcohol 5-20wt%, glycerol 2-10wt%, phthalic anhydride 7-25wt%, benzoic acid 3-15wt%, reflux dimethylbenzene 0.5-4wt%, two
Toluene 20-40wt%.
The oleic acid is to prepare one of conventional raw material of alkyd resin, in the weight of quick-dry type alkyd resin of the present invention
Amount percentage is 16-32wt%, such as can be 16-27wt%, 16-20wt%, 17.1-30.3wt%, 23-29wt%, 21.6-
30wt%、15wt%、17.5wt%、19wt%、20.3wt%、21wt%、22.7wt%、23.5wt%、24wt%、25.9wt%、26wt%、
27wt%,27.2wt%,28wt%,29.3wt%,30wt%；Preferably 17.1-30.3wt%；Most preferably 20.3wt%.
The pentaerythrite is since degree of functionality is big, and symmetrical configuration, and alkyd resin obtained is compared with same type, close oil content
Structure Detemination of Alkyd Resins it is close, it is dry it is very fast, hardness of paint film is higher, in the weight hundred of quick-dry type alkyd resin of the present invention
Dividing ratio is 5-20wt%, such as can be 5.1-19wt%, 6.7-19.6wt%, 7.2-17wt%, 7.8-16.6wt%, 8.8-
19.1wt%、6.1wt%、7.15wt%、8.26wt%、9.29wt%、10.35wt%、10.4wt%、10.41wt%、10.48wt%、
11.54wt%,12.57wt%,13.6wt%,14.63wt%,15.7wt%,16.72wt%；Preferably 6.7-19.6wt%；Most preferably
For 12wt%.
The glycerol is to prepare one of conventional raw material of alkyd resin, selects glycerol to substitute appropriate Ji Wusi in the present invention
Alcohol can reduce cost and can reduce resin molecular weight.Weight percent of the glycerol in quick-dry type alkyd resin of the present invention
For 2-10wt%, for example, can be 2-9wt%, 2.5-7.8wt%, 3-10wt%, 3.5-9.5wt%, 4-7wt%, 4wt%, 6.7wt%,
7.5wt%, 8.1wt%, 8.8wt%, 9wt%, 10wt% are preferably 2.5-7.8wt%；Most preferably 4wt%.
The phthalic anhydride is to prepare one of conventional raw material of alkyd resin, in quick-dry type alkyd of the present invention
The weight percent of resin be 7-25wt%, such as can be 6-17wt%, 8.5-22wt%, 7.6-20.5wt%, 12-20wt%,
19-22wt%、6wt%、6.4wt%、7.5wt%、8.2wt%、8.7wt%、9wt%、10wt%、11.5wt%、12.1wt%、13wt%、
14wt%,15.4wt%,16wt%,17.8wt%,19wt%,20wt%,20.3wt%,21wt%,21.7wt%,22wt%；Preferably
8.5-22wt%；Most preferably 18.5wt%.
The benzoic acid is a kind of natural resin from a wealth of sources, can reduce resin viscosity, and make paint film release solvent
Comparatively fast, it does rate to improve, parches quickening.The quick-drying of resin can be significantly improved.
The benzoic acid is 3-15wt% in the weight percent of quick-dry type alkyd resin of the present invention, such as be can be
3-9wt%、5-12wt%、6.4-13.5wt%、4-12wt%、8-15wt%、3wt%、3.6wt%、4wt%、4.5wt%、5.7wt%、
6wt%、7.2wt%、8.4wt%、8.9wt%、9.2wt%、10wt%、11.5wt%、12.6wt%、13wt%、13.3wt%、14.1wt%、
15wt%；Preferably 4-12wt%；Most preferably 11.8wt%.
The reflux dimethylbenzene refers to solvent xylene, can take the by-product of reaction out of with circulating reflux in production system
Object water, and reaction temperature is adjusted, it is 0.5-4wt% in the weight percent of quick-dry type alkyd resin of the present invention, such as can
Be 0.56-3.8wt%, 0.7-2.6wt%, 1.15-3.75wt%, 2-3wt%, 3-4wt%, 0.5wt%, 0.64wt%, 0.87wt%,
1wt%、1.15wt%、1.4wt%、1.6wt%、1.93wt%、2wt%、2.22wt%、2.35wt%、2.5wt%、2.7wt%、
2.86wt%,3wt%,3.05wt%,3.29wt%,3.41wt%,3.8wt%,4wt%；Preferably 0.56-3.8wt%；Most preferably
3.5wt%。
The dimethylbenzene is the common solvent of paint industry and diluent, strong and stability is good for the dissolving power of oil, rouge,
Its quick-dry type alkyd resin of the present invention weight percent be 20-40wt%, such as can be 22.5-38.6wt%,
32.6-35wt%、33.4-40wt%、37-40wt%、33-40wt%、30wt%、32.5wt%、34wt%、35.1wt%、36.2wt%、
37.6wt%,38.7wt%,39wt%,39.4wt%；Preferably 22.5-38.6wt%；Most preferably 29.9wt%.
In conclusion the technical solution after present invention optimization are as follows:
A kind of quick-dry type alkyd resin includes following component according to weight percent wt%: oleic acid 17.1-30.3wt%, Ji Wusi
Alcohol 6.7-19.6wt%, glycerol 2.5-7.8wt%, phthalic anhydride 8.5-22wt%, benzoic acid 4-12wt%, reflux dimethylbenzene
0.56-3.8wt%, dimethylbenzene 22.5-38.6wt%.
The technical solution that the present invention optimizes are as follows:
A kind of quick-dry type alkyd resin includes following component according to weight percent wt%: oleic acid 20.3wt%, pentaerythrite
12wt%, glycerol 4wt%, phthalic anhydride 18.5wt%, benzoic acid 11.8wt%, reflux dimethylbenzene 3.5wt%, dimethylbenzene
29.9wt%。
Various raw materials in inventive formulation can be commercially available by commercially available approach.
" comprising " of the present invention, it is intended that it exceptionally, can also contain other components, these other components except described group
The quick-dry type alkyd resin is assigned with different characteristics.In addition to this, " comprising " of the present invention may be replaced by sealing
" for " of enclosed or " by ... be made ".Regardless of quick-dry type alkyd resin of the present invention includes which kind of ingredient, the quick-dry type
The sum of weight percent of alkyd resin is 100%.
The present invention also provides the preparation methods of above-mentioned quick-dry type alkyd resin, include the following steps:
(1) oleic acid of formula ratio, pentaerythrite, glycerol, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, stirring is started and is warming up to 175-195 DEG C.
Preferably, the stirring is carried out with the rate of 50-150rpm, such as can be 50-85rpm, 67-98rpm, 72-
120rpm、95-135rpm、107-150rpm、50rpm、56rpm、60rpm、65rpm、71rpm、79rpm、84rpm、88rpm、
90pm、96rpm、100rpm、105rpm、110rpm、115rpm、122rpm、125rpm、130rpm、131rpm、136rpm、
140rpm,145rpm,150rpm；Further preferably 60-100rpm；Most preferably 80rpm.
It is described to be warming up to 175-195 DEG C, such as can be 180-195 DEG C, 185-190 DEG C, 175-190 DEG C, 175-180
℃,176℃,180℃,182℃,187℃,193℃；Preferably 180-190 DEG C；Most preferably 180 DEG C.
Temperature keeps the temperature 1-3h after being raised to.
The time of the heat preservation be 1-3h, such as can be 1-2h, 1-1.8h, 1.4-2.9h, 1.5-2.5h, 2-3h, 1h,
1.6h,1.82h,1.9h,2h,2.1h,2.3h,2.5,2.7h,3h；Preferably 1-3h；Most preferably 2h.
(3) it is continuously heating to 220-260 DEG C, heat preservation is until sample detection acid value≤10mgKOH/g, viscosity 12-16 seconds (25
DEG C grignard pipe).
It is described to be warming up to 220-260 DEG C, such as can be 220-250 DEG C, 222-245 DEG C, 235-240 DEG C, 229-255
℃、231-260℃、220℃、223℃、225℃、230℃、233℃、237℃、240℃、241℃、245℃、248℃、250
℃,252℃,256℃,259℃,260℃；Preferably 230-250 DEG C；Most preferably 230 DEG C.
After qualification cooling 200 DEG C hereinafter, the dimethylbenzene of formula ratio is added, stir；
The temperature be down to 200 DEG C hereinafter, for example can be 190 DEG C or less, 179 DEG C or less, 170 DEG C or less, 160 DEG C or less,
135 DEG C or less, 178 DEG C, 175 DEG C, 167 DEG C, 165 DEG C, 155 DEG C, 150 DEG C, 145 DEG C, 140 DEG C, 135 DEG C, 125 DEG C, 111 DEG C,
108℃；Preferably 200 DEG C or less；Most preferably 200 DEG C or less.
Preferably, the stirring is carried out with the rate of 50-150rpm, such as can be 50-85rpm, 67-98rpm, 72-
120rpm、95-135rpm、107-150rpm、50rpm、56rpm、60rpm、65rpm、71rpm、79rpm、84rpm、88rpm、
90pm、96rpm、100rpm、105rpm、110rpm、115rpm、122rpm、125rpm、130rpm、131rpm、136rpm、
140rpm,145rpm,150rpm；Further preferably 60-100rpm；Most preferably 80rpm.
Preferably, the time of the stirring be 10-50min, such as can be 10-25min, 15-38min, 20-45min,
27-35min、19-50min、10min、11.5min、17min、20min、23min、28.2min、30min、32.1min、
36.4min,40min,44min,49.8min,50min；Further preferably 20-40min；Most preferably 30min.
(5) up to quick-dry type alkyd resin of the invention after filtering.
The present invention uses solvent method, and since entire reaction process is always in solvent refluxing state, air is difficult to enter, and is made
Final color of resin shoals.And reaction in some molecular weight polymers that can be dissolved in dimethylbenzene by reflux be again introduced into reaction
Reaction is participated in kettle, reduces the loss of molecular weight polymers.Avoid the depth of color of resin caused by being produced with fusion method, consumption
The disadvantages of high.
In conclusion the technical solution after present invention optimization are as follows:
A kind of preparation method of quick-dry type alkyd resin, includes the following steps:
(1) oleic acid of formula ratio, pentaerythrite, glycerol, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, stirring is started and is warming up to 175-195 DEG C, the stirring is carried out with the rate of 50-150rpm；
(2) after temperature is raised to, 1-3h is kept the temperature；
(3) it is continuously heating to 220-260 DEG C, heat preservation is until 12-16 seconds sample detection acid value≤10mgKOH/g, viscosity (25 DEG C of lattice
Family name's pipe)；
(4) 200 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 10- of 50-150rpm
50min；
(5) up to quick-dry type alkyd resin of the invention after filtering.
The present invention advanced optimize after technical solution are as follows:
A kind of preparation method of quick-dry type alkyd resin, includes the following steps:
(1) oleic acid of formula ratio, pentaerythrite, glycerol, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, stirring is started and is warming up to 180-190 DEG C, the stirring is carried out with the rate of 60-100rpm；
(2) after temperature is raised to, 1-3h is kept the temperature；
(3) it is continuously heating to 230-250 DEG C, heat preservation is until 12-16 seconds sample detection acid value≤10mgKOH/g, viscosity (25 DEG C of lattice
Family name's pipe)；
(4) 200 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 20- of 60-100rpm
40min；
(5) up to quick-dry type alkyd resin of the invention after filtering.
The technical solution that the present invention optimizes are as follows:
A kind of preparation method of quick-dry type alkyd resin, includes the following steps:
(1) oleic acid of formula ratio, pentaerythrite, glycerol, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, stirring is started and is warming up to 180 DEG C, the stirring is carried out with the rate of 80rpm；
(2) after temperature is raised to, 2h is kept the temperature；
(3) 230 DEG C are continuously heating to, heat preservation is until 12-16 seconds sample detection acid value≤10mgKOH/g, viscosity (25 DEG C of grignard
Pipe)；
(4) 200 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 30min of 80rpm；
(5) up to quick-dry type alkyd resin of the invention after filtering.
Compared with prior art, the present invention has the advantage that (1) is largely using pentaerythrite since degree of functionality is big, and
And symmetrical configuration, alkyd resin obtained is close compared with the Structure Detemination of Alkyd Resins of same type, close oil content, fast drying, hardness of paint film
It is higher.(2) replace part pentaerythrite with glycerol, further reduce costs, improve the competitiveness of enterprise.(3) benzene is added
Formic acid, the degree of functionality of balance formula system stablize production and the stemness and gloss of final resin are greatly improved.(4) molten
Agent method technique avoids the loss of color of resin deepened with material, prepares quick-drying while greatly reducing production cost
The alkyd resin of type.
Below with reference to embodiment, the present invention is described in more detail.But following embodiments is only of the invention simple
Example, does not represent or limits the scope of the present invention, and interest field of the invention is subject to claims.
Specific embodiment
Embodiment 1
A kind of quick-dry type alkyd resin includes following component according to weight percent wt%: oleic acid 20.3wt%, pentaerythrite
12wt%, glycerol 4wt%, phthalic anhydride 18.5wt%, benzoic acid 11.8wt%, reflux dimethylbenzene 3.5wt%, dimethylbenzene
29.9wt%。
Above-mentioned quick-dry type alkyd resin specific the preparation method is as follows:
(1) oleic acid of formula ratio, pentaerythrite, glycerol, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, start stirring and be warming up to 180 DEG C, the stirring is carried out with the rate of 80rpm；
(2) after temperature is raised to, 2h is kept the temperature；
(3) 230 DEG C are continuously heating to, heat preservation is until 12-16 seconds sample detection acid value≤10mgKOH/g, viscosity (25 DEG C of grignard
Pipe)；
(4) 200 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 30min of 80rpm；
(5) up to quick-dry type alkyd resin of the invention after filtering.
Observe and measure the performance indexes of the quick-dry type alkyd resin of this implementation column, detection method and index, appearance
Referring to GB1729, color (iron cobalt colorimetric) is referring to GB9281, and viscosity (applying -4 glasss) is referring to GB6753.4, fineness reference
GB6753.1, acid value do solid work time reference referring to GB1728 second method referring to GB6751, surface drying time referring to GB6743, solid part
GB1728 first method.Testing result is as shown in table 1.
Embodiment 2
A kind of quick-dry type alkyd resin includes following component according to weight percent wt%: oleic acid 22wt%, glycerol 3wt%, season penta
Tetrol 14wt%, phthalic anhydride 17.5wt%, benzoic acid 9.88wt%, reflux dimethylbenzene 2.8wt%, dimethylbenzene 26.7wt%.
Above-mentioned quick-dry type alkyd resin specific the preparation method is as follows:
(1) oleic acid of formula ratio, glycerol, pentaerythrite, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, start stirring and be warming up to 185 DEG C, the stirring is carried out with the rate of 80rpm；
(2) after temperature is raised to, 2.5h is kept the temperature；
(3) 240 DEG C are continuously heating to, heat preservation is until 12-16 seconds sample detection acid value≤10mgKOH/g, viscosity (25 DEG C of grignard
Pipe)；
(4) 190 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 40min of 60rpm；
(5) up to quick-dry type alkyd resin of the invention after filtering.
Observe and measure the performance indexes of the quick-dry type alkyd resin of this implementation column, detection method and index and implementation
Example 1 is identical, and the results are shown in Table 1.
Embodiment 3
A kind of quick-dry type alkyd resin includes following component according to weight percent wt%: oleic acid 18wt%, glycerol 2.8wt%, season
Penta tetrol 13.2wt%, phthalic anhydride 16.5wt%, benzoic acid 8.18wt%, reflux dimethylbenzene 3.8wt%, dimethylbenzene
22.7wt%。
Above-mentioned quick-dry type alkyd resin specific the preparation method is as follows:
(1) oleic acid of formula ratio, glycerol, pentaerythrite, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, start stirring and be warming up to 190 DEG C, the stirring is carried out with the rate of 100rpm；
(2) after temperature is raised to, 2.6h is kept the temperature；
(3) 245 DEG C are continuously heating to, heat preservation is until 12-16 seconds sample detection acid value≤10mgKOH/g, viscosity (25 DEG C of grignard
Pipe)；
(4) 195 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 20min of 100rpm；
(5) up to quick-dry type alkyd resin of the invention after filtering.
Observe and measure the performance indexes of the quick-dry type alkyd resin of this implementation column, detection method and index and implementation
Example 1 is identical, and the results are shown in Table 1.
Embodiment 4
A kind of quick-dry type alkyd resin includes following component according to weight percent wt%: oleic acid 22wt%, glycerol 3.1wt%, season
Penta tetrol 14.1wt%, phthalic anhydride 15.8wt%, benzoic acid 6.18wt%, reflux dimethylbenzene 2.8wt%, dimethylbenzene
25.1wt%。
Above-mentioned quick-dry type alkyd resin specific the preparation method is as follows:
(1) oleic acid of formula ratio, glycerol, pentaerythrite, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, start stirring and be warming up to 193 DEG C, the stirring is carried out with the rate of 50rpm；
(2) after temperature is raised to, 3h is kept the temperature；
(3) 250 DEG C are continuously heating to, heat preservation is until 12-16 seconds sample detection acid value≤10mgKOH/g, viscosity (25 DEG C of grignard
Pipe)；
(4) 198 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 50min of 50rpm；
(5) up to quick-dry type alkyd resin of the invention after filtering.
Observe and measure the performance indexes of the quick-dry type alkyd resin of this implementation column, detection method and index and implementation
Example 1 is identical, and the results are shown in Table 1.
Embodiment 5
A kind of quick-dry type alkyd resin includes following component according to weight percent wt%: oleic acid 22.16wt%, glycerol 6.2wt%,
Pentaerythrite 11.6wt%, phthalic anhydride 16.82wt%, benzoic acid 6.78wt%, reflux dimethylbenzene 3.95wt%, dimethylbenzene
20.68wt%。
Above-mentioned quick-dry type alkyd resin specific the preparation method is as follows:
(1) oleic acid of formula ratio, glycerol, pentaerythrite, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, start stirring and be warming up to 180 DEG C, the stirring is carried out with the rate of 150rpm；
(2) after temperature is raised to, 2h is kept the temperature；
(3) 235 DEG C are continuously heating to, heat preservation is until 12-16 seconds sample detection acid value≤10mgKOH/g, viscosity (25 DEG C of grignard
Pipe)；
(4) 200 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 10min of 150rpm；
(5) up to quick-dry type alkyd resin of the invention after filtering.
Observe and measure the performance indexes of the quick-dry type alkyd resin of this implementation column, detection method and index and implementation
Example 1 is identical, and the results are shown in Table 1.
Table 1
| Detection project | Index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Appearance | As clear as crystal mucus | Meet | Meet | Meet | Meet | Meet |
| Color (iron cobalt colorimetric) | ≤ No. 10 | 7 | 7 | 7 | 9 | 8 |
| Viscosity (applies -4 glasss) | 200-300 | 260 | 250 | 250 | 247 | 248 |
| Fineness (μM) | ≤25 | 20 | 21 | 21.5 | 22.3 | 22 |
| Acid value | ≤12mgKOH/g | 9.2 | 8.8 | 8.9 | 9 | 8.7 |
| Solid part (%) | 55±1 | 55.6 | 54.8 | 54.7 | 55.2 | 55.5 |
| Surface drying (25 DEG C/min) | ≤20 | 5 | 6.2 | 6.3 | 5.6 | 7.5 |
| Do solid work (25 DEG C/h) | ≤8 | 7 | 7.5 | 6.8 | 7.6 | 7.7 |
It should be noted that and understand, the case where not departing from the spirit and scope of the present invention required by appended claims
Under, various modifications and improvements can be made to the present invention of foregoing detailed description.It is therefore desirable to the range of the technical solution of protection
It is not limited by given any specific exemplary teachings.
The Applicant declares that the above content is combine specific preferred embodiment made for the present invention further specifically
It is bright, and it cannot be said that specific implementation of the invention is only limited to these instructions.For the ordinary skill of the technical field of the invention
For personnel, without departing from the inventive concept of the premise, a number of simple deductions or replacements can also be made, all should be considered as belonging to
In protection scope of the present invention.
Claims (6)
1. a kind of quick-dry type alkyd resin, which is characterized in that according to weight percent wt% include following component: oleic acid 16-
32wt%, pentaerythrite 5-20wt%, glycerol 2-10wt%, phthalic anhydride 7-25wt%, benzoic acid 3-15wt%, reflux diformazan
Benzene 0.5-4wt%, dimethylbenzene 20-40wt%, the reflux dimethylbenzene are solvent xylene.
2. a kind of quick-dry type alkyd resin as described in claim 1, which is characterized in that according to weight percent wt% including such as
Lower component: oleic acid 17.1-30.3wt%, pentaerythrite 6.7-19.6wt%, glycerol 2.5-7.8wt%, phthalic anhydride 8.5-
22wt%, benzoic acid 4-12wt%, reflux dimethylbenzene 0.56-3.8wt%, dimethylbenzene 22.5-38.6wt%.
3. a kind of quick-dry type alkyd resin as claimed in claim 1 or 2, which is characterized in that include according to weight percent wt%
Following component: oleic acid 20.3wt%, pentaerythrite 12wt%, glycerol 4wt%, phthalic anhydride 18.5wt%, benzoic acid
11.8wt%, reflux dimethylbenzene 3.5wt%, dimethylbenzene 29.9wt%.
4. a kind of preparation method of quick-dry type alkyd resin as claimed in claim 3, it is characterised in that: the following steps are included:
(1) oleic acid of formula ratio, pentaerythrite, glycerol, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, stirring is started and is warming up to 175-195 DEG C.
(2) after temperature is raised to, 1-3h is kept the temperature；
(3) it is continuously heating to 220-260 DEG C, heat preservation is until sample detection acid value≤10mgKOH/g, 25 DEG C of grignard pipe viscosity 12-
16 seconds；
(4) after qualified cooling 200 DEG C hereinafter, the dimethylbenzene of formula ratio is added, stir；
(5) up to quick-dry type alkyd resin after filtering.
5. a kind of preparation method of quick-dry type alkyd resin as claimed in claim 4, it is characterised in that: in the process (1),
Stirring is carried out with the rate of 50-150rpm, in the process (4), stirs 10-50min with the rate uniform of 50-150rpm.
6. a kind of preparation method of quick-dry type alkyd resin as claimed in claim 4, which comprises the steps of:
(1) oleic acid of formula ratio, pentaerythrite, glycerol, phthalic anhydride, benzoic acid, reflux dimethylbenzene are put into reaction kettle
In, it is passed through N2, stirring is started and is warming up to 180 DEG C, the stirring is carried out with the rate of 80rpm；
(2) after temperature is raised to, 2h is kept the temperature；
(3) be continuously heating to 230 DEG C, heat preservation until sample detection acid value≤10mgKOH/g, 25 DEG C grignard pipe viscosity 12-16 seconds；
(4) 200 DEG C are cooled down after qualification hereinafter, the dimethylbenzene of formula ratio is added, with the rate uniform stirring 30min of 80rpm；
(5) up to quick-dry type alkyd resin of the invention after filtering.
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| CN201811320050.2A CN109180920A (en) | 2018-11-07 | 2018-11-07 | A kind of quick-dry type alkyd resin and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811320050.2A CN109180920A (en) | 2018-11-07 | 2018-11-07 | A kind of quick-dry type alkyd resin and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113881326A (en) * | 2021-10-28 | 2022-01-04 | 陕西宝塔山油漆股份有限公司 | Thick-coatable modified alkyd finish paint and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153406A (en) * | 2015-10-12 | 2015-12-16 | 湖南开磷雁峰塔涂料有限公司 | Quick-drying alkyd resin and preparation method thereof as well as quick-drying varnish |
-
2018
- 2018-11-07 CN CN201811320050.2A patent/CN109180920A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153406A (en) * | 2015-10-12 | 2015-12-16 | 湖南开磷雁峰塔涂料有限公司 | Quick-drying alkyd resin and preparation method thereof as well as quick-drying varnish |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113881326A (en) * | 2021-10-28 | 2022-01-04 | 陕西宝塔山油漆股份有限公司 | Thick-coatable modified alkyd finish paint and preparation method thereof |
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Application publication date: 20190111 |