CN102408551A - Preparation method of alkyd resin - Google Patents
Preparation method of alkyd resin Download PDFInfo
- Publication number
- CN102408551A CN102408551A CN 201110317246 CN201110317246A CN102408551A CN 102408551 A CN102408551 A CN 102408551A CN 201110317246 CN201110317246 CN 201110317246 CN 201110317246 A CN201110317246 A CN 201110317246A CN 102408551 A CN102408551 A CN 102408551A
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- synolac
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- esterification
- phthalic anhydride
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Abstract
The invention relates to a preparation method of alkyd resin. The preparation method comprises the following specific steps: (1) adding neopentyl glycol, trihydroxymethyl propane, phthalic anhydride, hydrogenated phthalic anhydride and antioxidant to a reaction container, and heating to carry out melt esterification on the materials at the temperature of 200-240 DEG C; (2) when esterification is carried out to an acid value being 40-45 mgKOH/g, cooling to 120-160 DEG C, and adding short-chain synthetic fatty acid and an aliphatic hydrocarbon solvent; (3) heating to carry out reflux esterification at the temperature of 180-200 DEG C, and diluting with acetic acid ester organic solvent when the acid value is smaller than or equal to 8 mgKOH/g; and (4) cooling to 100 DEG C and filtering to obtain alkyd resin. The paint prepared from the alkyd resin obtained in the invention and nitrocellulose has the characteristics of rapid drying, high hardness, good fullness, good adhesion force, and good water resistance.
Description
Technical field
The present invention relates to polymeric material field, especially relate to a kind of method for preparing Synolac.
Background technology
The nitro nail varnish generally matches with nitro-cotton and vinyl resin or Synolac and forms, and requires that dryness is good, gloss is high, fullness ratio good, sticking power is good, hardness is high, water-tolerant, the more important thing is and wants environmental protection, and is harmless to health.General vinyl resin gloss do not have Synolac outstanding, also have residual monomer in addition in the vinyl resin, though seldom, still be deleterious to health.The water tolerance and the sticking power of general Synolac are difficult to reach requirement, and " triphen " content (being toluene, YLENE, benzene content) and phthalic acid salts contg in the general Synolac are difficult to reach requirement.
Summary of the invention
To the problems referred to above that prior art exists, the invention provides a kind of preparation method of Synolac.The lacquer of prepared Synolac of the present invention and nitro-cotton configuration preparation has fast doing under the normal temperature, and hardness is high, and fullness ratio is good, and sticking power is good, the characteristics of water-tolerant.
Technical scheme of the present invention is following:
A kind of preparation method of Synolac, concrete preparation process is following:
(1) NSC 6366, TriMethylolPropane(TMP), phthalic anhydride, hydrogenation phthalic anhydride, oxidation inhibitor are dropped into reaction vessel, heat up, make material between 200 ~ 240 ℃, carry out fusion esterification;
(2) when esterification to acid number is at 40 ~ 45mgkOH/g in the step (1), be cooled to 120 ~ 160 ℃, add the synthetic fatty acid and the aliphatic solvents of short chain;
(3) heat up, the esterification that between 180 ~ 200 ℃, refluxes is when acid number during smaller or equal to 8mgkOH/g, with acetic ester organic solvent latting drown;
(4) be cooled to 100 ℃, filter, promptly get Synolac;
Above-mentioned each raw material and weight percent thereof are respectively:
NSC 6366 13 ~ 18%
TriMethylolPropane(TMP) 13 ~ 17%
Phthalic anhydride 21 ~ 28%
Hydrogenation phthalic anhydride 5 ~ 10%
Oxidation inhibitor 0.1 ~ 0.3%
The synthetic fatty acid 12 ~ 18% of short chain
D-40 organic solvent 2 ~ 4%
Acetic ester organic solvent 16 ~ 18%.
Said hydrogenation phthalic anhydride is THPA or HHPA.Said oxidation inhibitor is Hypophosporous Acid, 50.Said short chain synthetic fatty acid is n-caprylic acid, certain herbaceous plants with big flowers acid or laurostearic acid.Said aliphatic solvents is for take off the later aliphatic hydrocarbon organic solvent of aromatic hydrocarbons fully.Said aliphatic solvents is the D-40 of Mobil Corp..Said acetic ester organic solvent is at least a in vinyl acetic monomer, 2-butyl acetate, the N-BUTYL ACETATE.In the said fusion esterification of step (1), the water of generation is discharged by condensing surface; In the said backflow esterification of step (3), the water of generation and reflux solvent azeotropic are discharged by condensing surface later.
Beneficial technical effects of the present invention is:
1, the present invention uses a certain amount of THPA or HHPA, can improve the sticking power of Synolac paint film; The lipid acid of short chain makes Synolac have fullness ratio, and promptly color and luster is full, good brightness, no gloomy color and luster; TriMethylolPropane(TMP) and NSC 6366 make Synolac have gloss and water tolerance; Phthalic anhydride makes Synolac have certain rigidity.
2, the present invention according to the molecular designing principle, has adopted two step esterification process in the process of preparation Synolac, makes MWD more even, and has reduced micromolecular formation, improves the water tolerance of Synolac.When second goes on foot esterification, add lipid acid, can make carbochain be evenly distributed in the molecular backbone chain both sides, improved the compatibility of resin and nitro-cotton and the gloss and the fullness ratio of nail varnish, also protected ester bond simultaneously, prevent hydrolysis, increase water tolerance.
3, the first step esterification acid number according to the invention is controlled between 40 ~ 45mgkOH/g and lowers the temperature, and is in order to prevent macromolecular formation, and it is for end-blocking that the second step esterification adds lipid acid, the second step esterification temperature between 180 ~ 00 ℃, can make reaction temperature with; If temperature is too high, reaction then can be comparatively violent, forms macromole easily, the fullness ratio and the gloss of injury nail varnish.
4, the present invention does reflux solvent with D-40, has stopped " triphen " existence in resin, with acetates organic solvent environmental protection, nontoxic.
5, the selected lipid acid of the present invention is the lipid acid of short chain; Because the lipid acid of short chain is active stronger than the lipid acid (like palmitic acid, Triple Pressed Stearic Acid) of long-chain; Esterification easily avoids the reaction of synthetic fatty acid not exclusively to remain in the resin, and water tolerance and sticking power are produced bad influence.
Embodiment
Embodiment 1
(1) NSC 6366, TriMethylolPropane(TMP), phthalic anhydride, THPA, Hypophosporous Acid, 50 are dropped into reaction vessel, heat up, make material at 230 ℃ of fusion esterifications, the water of generation is discharged by condensing surface;
(2) when esterification to acid number is at 40mgkOH/g in the step (1), be cooled to 120 ℃, add certain herbaceous plants with big flowers acid and D-40 organic solvent;
(3) heat up,, discharge by condensing surface after the water of generation and the reflux solvent azeotropic, when acid number is 8mgkOH/g, use the N-BUTYL ACETATE latting drown 190 ℃ of backflow esterifications;
(4) be cooled to 100 ℃, filter, promptly get Synolac;
Above-mentioned each raw material and weight thereof are seen shown in the table 1.
Embodiment 2
(1) NSC 6366, TriMethylolPropane(TMP), phthalic anhydride, THPA, Hypophosporous Acid, 50 are dropped into reaction vessel, heat up, make material at 240 ℃ of fusion esterifications, the water of generation is discharged by condensing surface;
(2) when esterification to acid number is at 45mgkOH/g in the step (1), be cooled to 140 ℃, add laurostearic acid and D-40 organic solvent;
(3) heat up,, discharge by condensing surface after the water of generation and the reflux solvent azeotropic, when acid number is 8mgkOH/g, use the N-BUTYL ACETATE latting drown 200 ℃ of backflow esterifications;
(4) be cooled to 100 ℃, filter, promptly get Synolac;
Above-mentioned each raw material and weight thereof are seen shown in the table 1.
Embodiment 3
(1) NSC 6366, TriMethylolPropane(TMP), phthalic anhydride, HHPA, Hypophosporous Acid, 50 are dropped into reaction vessel, heat up, make material at 200 ℃ of fusion esterifications, the water of generation is discharged by condensing surface;
(2) when esterification to acid number is at 42mgkOH/g in the step (1), be cooled to 160 ℃, add sad and the D-40 organic solvent;
(3) heat up,, discharge by condensing surface after the water of generation and the reflux solvent azeotropic, when acid number is 8mgkOH/g, use the vinyl acetic monomer latting drown 180 ℃ of backflow esterifications;
(4) be cooled to 100 ℃, filter, promptly get Synolac;
Above-mentioned each raw material and weight thereof are seen shown in the table 1.
Embodiment 4
(1) NSC 6366, TriMethylolPropane(TMP), phthalic anhydride, THPA, Hypophosporous Acid, 50 are dropped into reaction vessel, heat up, make material at 220 ℃ of fusion esterifications, the water of generation is discharged by condensing surface;
(2) when esterification to acid number is at 43mgkOH/g in the step (1), be cooled to 150 ℃, add certain herbaceous plants with big flowers acid and D-40 organic solvent;
(3) heat up,, discharge by condensing surface after the water of generation and the reflux solvent azeotropic, when acid number is 8mgkOH/g, use the 2-butyl acetate latting drown 190 ℃ of backflow esterifications;
(4) be cooled to 100 ℃, filter, promptly get Synolac;
Above-mentioned each raw material and weight thereof are seen shown in the table 1.
Table 1
The performance index of embodiment 1 ~ 4 gained Synolac are seen shown in the table 2.
Table 2
Detect the objectionable impurities of embodiment 1 ~ 4 gained Synolac, its detection method and prescribed limit values are seen shown in the table 3.DBP is a DBP in the table 3, and DEHP is phthalic acid two (2-ethylhexyl) ester, and DMEP is a dimethyl glycol phthalate.
Table 3
Detected result is seen shown in the table 4.Detected result N.D. representes not detect related substances content in the table.
Table 4
Application examples:
Embodiment 1 ~ 4 gained Synolac is become the single component nail varnish according to the formulation shown in the table 5.
Table 5
The NC slurry is meant that nitrated cotton pulp, BYK306 are meant a kind of silicane flow agent that Bi Ke company produces in the table 5, and epoxy resin E-52D is the commercially available prod.
After embodiment 1 ~ 4 gained Synolac become nail varnish according to above-mentioned formulation, spraying plate-making was at room temperature solidified, and detects its performance.The instrument and the method that detect see that shown in the table 6, detected result is seen shown in the table 7.
Table 6
Table 7
Can see that from table 7 nail varnish each item performance of utilizing the prepared alkyd resin production of the present invention to come out all meets index request.
Claims (8)
1. the preparation method of a Synolac is characterized in that concrete preparation process is following:
(1) NSC 6366, TriMethylolPropane(TMP), phthalic anhydride, hydrogenation phthalic anhydride, oxidation inhibitor are dropped into reaction vessel, heat up, make material between 200 ~ 240 ℃, carry out fusion esterification;
(2) when esterification to acid number is at 40 ~ 45mgkOH/g in the step (1), be cooled to 120 ~ 160 ℃, add the synthetic fatty acid and the aliphatic solvents of short chain;
(3) heat up, the esterification that between 180 ~ 200 ℃, refluxes is when acid number during smaller or equal to 8mgkOH/g, with acetic ester organic solvent latting drown;
(4) be cooled to 100 ℃, filter, promptly get Synolac;
Above-mentioned each raw material and weight percent thereof are respectively:
NSC 6366 13 ~ 18%
TriMethylolPropane(TMP) 13 ~ 17%
Phthalic anhydride 21 ~ 28%
Hydrogenation phthalic anhydride 5 ~ 10%
Oxidation inhibitor 0.1 ~ 0.3%
The synthetic fatty acid 12 ~ 18% of short chain
D-40 organic solvent 2 ~ 4%
Acetic ester organic solvent 16 ~ 18%.
2. the preparation method of a kind of Synolac according to claim 1 is characterized in that said hydrogenation phthalic anhydride is THPA or HHPA.
3. the preparation method of a kind of Synolac according to claim 1 is characterized in that said oxidation inhibitor is Hypophosporous Acid, 50.
4. the preparation method of a kind of Synolac according to claim 1 is characterized in that said short chain synthetic fatty acid is n-caprylic acid, certain herbaceous plants with big flowers acid or laurostearic acid.
5. the preparation method of a kind of Synolac according to claim 1 is characterized in that said aliphatic solvents is for take off the later aliphatic hydrocarbon organic solvent of aromatic hydrocarbons fully.
6. according to the preparation method of claim 1 and 5 described a kind of Synolac, it is characterized in that said aliphatic solvents is the D-40 of Mobil Corp..
7. the preparation method of a kind of Synolac according to claim 1 is characterized in that said acetic ester organic solvent is at least a in vinyl acetic monomer, 2-butyl acetate, the N-BUTYL ACETATE.
8. the preparation method of a kind of Synolac according to claim 1 is characterized in that the water of generation is discharged by condensing surface in the said fusion esterification of step (1); In the said backflow esterification of step (3), the water of generation and reflux solvent azeotropic are discharged by condensing surface later.
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| CN 201110317246 CN102408551B (en) | 2011-10-19 | 2011-10-19 | Preparation method of alkyd resin |
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| CN 201110317246 CN102408551B (en) | 2011-10-19 | 2011-10-19 | Preparation method of alkyd resin |
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| CN102408551B CN102408551B (en) | 2013-02-27 |
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Cited By (21)
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| CN103965451A (en) * | 2013-01-30 | 2014-08-06 | 合众（佛山）化工有限公司 | Preparation method of environmentally-friendly low-viscosity nearly smell-less alkyd resin |
| CN103965453A (en) * | 2013-01-30 | 2014-08-06 | 合众（佛山）化工有限公司 | Preparation method of benzene-free nearly smell-less scratch-resistant alkyd resin |
| CN104726012A (en) * | 2013-12-18 | 2015-06-24 | 合众（佛山）化工有限公司 | Semi-transparent bubinga color raw umber flavor-clearing type polyurethane wood paint and preparation method |
| CN104726004A (en) * | 2013-12-18 | 2015-06-24 | 合众（佛山）化工有限公司 | Semitransparent orange brown calcined sienna smell cleaning type polyurethane woodenware paint and preparation method thereof |
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| CN104726009A (en) * | 2013-12-18 | 2015-06-24 | 合众（佛山）化工有限公司 | Semi-transparent orange red calcined sienna flavor-clearing type polyurethane wood paint and preparation method |
| CN104726010A (en) * | 2013-12-18 | 2015-06-24 | 合众（佛山）化工有限公司 | Semi-transparent deep bubinga color calcined sienna flavor-clearing type polyurethane wood paint and preparation method |
| CN104726007A (en) * | 2013-12-18 | 2015-06-24 | 合众（佛山）化工有限公司 | Semitransparent black reddish brown Vandyke smell cleaning type polyurethane woodenware paint and preparation method thereof |
| CN104726011A (en) * | 2013-12-18 | 2015-06-24 | 合众（佛山）化工有限公司 | Semi-transparent santos rose wood color raw umber flavor-clearing type polyurethane wood paint and preparation method |
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| CN103965451A (en) * | 2013-01-30 | 2014-08-06 | 合众（佛山）化工有限公司 | Preparation method of environmentally-friendly low-viscosity nearly smell-less alkyd resin |
| CN103965453A (en) * | 2013-01-30 | 2014-08-06 | 合众（佛山）化工有限公司 | Preparation method of benzene-free nearly smell-less scratch-resistant alkyd resin |
| CN103965453B (en) * | 2013-01-30 | 2016-05-18 | 合众（佛山）化工有限公司 | A kind of preparation method without the low clean taste scratch resistance alkyd resins of benzene |
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| CN108395524A (en) * | 2018-02-01 | 2018-08-14 | 新纶科技（常州）有限公司 | A kind of saturated fatty acid alkyd resin intermediate and its synthetic method |
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