CN102604054A - Saturated alkyd resin for wood lacquer and preparation method thereof - Google Patents
Saturated alkyd resin for wood lacquer and preparation method thereof Download PDFInfo
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- CN102604054A CN102604054A CN201210070226XA CN201210070226A CN102604054A CN 102604054 A CN102604054 A CN 102604054A CN 201210070226X A CN201210070226X A CN 201210070226XA CN 201210070226 A CN201210070226 A CN 201210070226A CN 102604054 A CN102604054 A CN 102604054A
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Abstract
The invention belongs to the technical field of chemical industry and particularly discloses saturated alkyd resin for a wood lacquer. The saturated alkyd resin for the wood lacquer comprises the following components in percentage by mass: 15.0 to 22.0 percent of caprylic/capric mixed acid, 5.2 to 9.2 percent of neopentyl glycol, 20.6 to 30.6 percent of trimethylolpropane, 28.6 to 38.6 percent of phthalic anhydride, 0.1 to 0.2 percent of color reducer, 2.5 to 4.5 percent of reflux solvent and 10.5 to 20.5 percent of diluting solvent. The alkyd resin has excellent performance, simple preparation method and low cost. The wood lacquer obtained by the alkyd resin has excellent performance.
Description
Technical field
The present invention relates to a kind of coating of chemical field, particularly a kind of wood lacquer is with saturated alcohol acid resin and preparation method thereof.
Background technology
Saturated polyester coating has good outdoor weatherability and tint retention, and characteristics such as higher hardness, good toughness and sticking power are arranged, and generally is the organic polymer resin that is made through the condensation chemical reaction by Organic Chemicals such as polyvalent alcohol and many anacidities.Saturated alkyd resin coating is mainly used in coil coating, car paint in traditional use, because of its special performances; Limited its widespread use; In order to expand the use of saturated polyester, its special performances can be applied in the wood lacquer, be the improvement direction of present saturated polyester research and development.Particularly carried out after the modification, its special performances is more outstanding, more can embody its advantage.At present; There is a lot of production of resins producers mainly to adopt hexanodioic acid, m-phthalic acid, terephthalic acid, trimellitic acid, phthalic acid etc.; Above material all is that the paint film that paint forms provides good toughness and hardness, but also is merely the saturated polyester that is applied to coiled material and automobile industry, wants to develop a kind of saturated polyester that can be applied in the wood lacquer; Its performance is essential to be changed because wood lacquer ornamental have relatively high expectations less demanding to the paint film mechanical property.
Summary of the invention
To the foregoing invention purpose, the technical problem that the present invention will solve be supply a kind of adopt hot last of the ten Heavenly stems mixing acid be raw material, excellent performance, the simple and cheap wood lacquer of preparation method use saturated alkyd resin.
For solving the problems of the technologies described above; The technical scheme that the present invention adopted is: a kind of wood lacquer is used the saturated alcohol acid resin, by mass percentage: suffering mixing acid 15.0 % in the last of the ten Heavenly stems～22.0%, NSC 6366 5.2 ~ 9.2%, TriMethylolPropane(TMP) 20.6 ~ 30.6%, Tetra hydro Phthalic anhydride 28.6 ~ 38.6%, the agent 0.1 ~ 0.2% of losing lustre, reflux solvent 2.5 ~ 4.5%, letdown solvent dun 10.5 ~ 20.5%.
Further: above-mentioned wood lacquer with the saturated alcohol acid resin in, the described agent of losing lustre is a Hypophosporous Acid, 50; Described reflux solvent and letdown solvent dun are YLENE.
The present invention also provides the preparation method of above-mentioned Synolac, the steps include:
After step 1. drops into reaction kettle with suffering mixing acid in the last of the ten Heavenly stems, NSC 6366, TriMethylolPropane(TMP), Tetra hydro Phthalic anhydride, Hypophosporous Acid, 50 and reflux solvent; Logical nitrogen in reaction kettle, and be warming up to 80 ± 10 ℃, begin to stir and continue to be warmed up to 160 ± 5 ℃; Be incubated 2 ± 0.5 hours;
Step 2. continues to be rapidly heated to 180 ± 10 ℃ then, is incubated 1 ± 0.5 hour;
Step 3. continues to be rapidly heated to 210-220 ℃ of insulation, and esterification to viscosity, acid number are qualified;
Step 4. is cooled to below 150 ℃, adds letdown solvent dun, promptly obtains required wood lacquer and uses the saturated alcohol acid resin.
The described agent of losing lustre is a Hypophosporous Acid, 50; Described reflux solvent and letdown solvent dun are YLENE.
Because wood lacquer is had relatively high expectations to color of resin with resin, therefore need in the prescription of the present invention to add inhibitor to reduce prepared color of resin, make it to be lower than No. 2 looks of iron cobalt tintometer, the color of resin that generally makes is about No. 1 look; The said agent of losing lustre can be adopted Hypophosporous Acid, 50, phosphorous acid ester or phosphite.
In the above-mentioned prescription; The inventor is through discovering; Only in scorification, solvent method and the interfacial polymerization in carrying out polymerization method is solvent method; Our custom is referred to as the polymerization that refluxes in the industry, reacting balance and side reaction is few, and the small molecules that produces in the condensation also can be removed with the solvent azeotropic.The viscosity of products obtained therefrom also reduces, and be easy to construction, and temperature of reaction is better controlled the circulation ratio that helps reacting.Because the present invention has used and the different mixing acid of the saturated polyester of traditional mode of production; In order further to illustrate the benefit of solvent method; So the inventor passes through experimental study; In above-mentioned prescription, come comparison with the application of conventional formulation and the saturated polyester of the present invention's prescription, and the experiment of solvent method and scorification is to likening explanation to.
Compare with existing technology and Application Areas; The present invention has following positive effect: at first; The present invention has started and has prepared another new industrial chemicals of saturated alkyd resin; On original production unit, just can successfully produce performance and be superior to traditional Synolac and can be applied to the saturated polyester in the wood lacquer, enlarge the range of application of saturated polyester; Secondly, the present invention has also proved that through experimental study solvent method is a kind of production technique that is more suitable for being applied to producing the saturated polyester of wood lacquer.This saturated alkyd resin excellent performance, preparation method are simple, and production cost is low.
Embodiment:
Embodiment 1
Wood lacquer in this instance is used saturated alkyd resin, and its composition of raw materials is counted by weight percentage, and is made up of following component:
Suffering mixing acid in the last of the ten Heavenly stems 15.5%
NSC 6366 10.2%
TriMethylolPropane(TMP) 22.6%
Tetra hydro Phthalic anhydride 32.6%
Hypophosporous Acid, 50 0.1%
YLENE 3.5%
Letdown solvent dun (YLENE) 15.5%
The above starting material is all commercially available technical grade product;
In the present embodiment, wood lacquer is used saturated alkyd resin, is to adopt the above-mentioned raw materials prescription, gets through following method preparation:
After step 1. drops into reaction kettle with suffering mixing acid in the last of the ten Heavenly stems, NSC 6366, TriMethylolPropane(TMP), Tetra hydro Phthalic anhydride, Hypophosporous Acid, 50 and YLENE, logical nitrogen in reaction kettle, and be warming up to 80 ℃, and begin to stir and continue to be warmed up to 160 ℃, be incubated 2 hours;
Step 2. continues to be rapidly heated to 180 ℃ then, is incubated 1 hour;
Step 3. continues to be rapidly heated to 210-220 ℃ of insulation, and esterification began sampling Detection after 3 hours; Qualified to sample viscosity, acid number, be cooled at once below 150 ℃, add letdown solvent dun; Stir, filter and package, promptly obtain required wood lacquer and use the saturated alcohol acid resin.The gained resin property is measured excellent performance as a result, and is as shown in table 1.
Table 1:
Comparison example 1-1 (scorification)
Wood lacquer in this instance is used saturated alkyd resin, and its composition of raw materials is counted by weight percentage, and is made up of following component:
Suffering mixing acid in the last of the ten Heavenly stems 15.5%
NSC 6366 10.2%
TriMethylolPropane(TMP) 22.6%
Tetra hydro Phthalic anhydride 32.6%
Hypophosporous Acid, 50 0.1%
Letdown solvent dun (YLENE) 19%
The above starting material is all commercially available technical grade product;
This instance wood lacquer is used saturated alkyd resin, is to adopt the above-mentioned raw materials prescription, gets through following method preparation:
After step 1. drops into reaction kettle with suffering mixing acid in the last of the ten Heavenly stems, NSC 6366, TriMethylolPropane(TMP), Tetra hydro Phthalic anhydride, Hypophosporous Acid, 50, logical nitrogen in reaction kettle, and be warming up to 80 ℃, and begin to stir and continue to be warmed up to 160 ℃, be incubated 2 hours;
Step 2. continues to be rapidly heated to 180 ℃ then, is incubated 1 hour;
Step 3. continues to be rapidly heated to 210-220 ℃ of insulation, and esterification began sampling Detection after 3 hours; Qualified to sample viscosity, acid number, be cooled at once below 150 ℃, add letdown solvent dun; Stir, filter and package, promptly obtain required wood lacquer and use the saturated alcohol acid resin.It is as shown in table 2 that the gained resin property is measured the result.
Table 2:
Through embodiment 1 is carried out finding after the performance comparison with two resins of Comparative Examples 1-1 preparation; Under the identical situation of preparation condition; The color of embodiment 1 resin that makes an experiment of utilization solvent method is shallow than Comparative Examples 1-1's, and experimentation is controlled easily, and measured rotary viscosity is lower under identical temperature; When constructing, embodiment 1 is than more the saving time of Comparative Examples 1-1, more convenient.
Embodiment 2
Hexanodioic acid 13.5%
NSC 6366 10.2%
TriMethylolPropane(TMP) 22.6%
Tetra hydro Phthalic anhydride 34.6%
Hypophosporous Acid, 50 0.1%
YLENE 3.5%
Letdown solvent dun (YLENE) 15.5%
The above starting material is all commercially available technical grade product;
The present embodiment wood lacquer is used saturated alkyd resin, is to adopt above-mentioned traditional raw material prescription, makes through following method:
After step 1. drops into reaction kettle with hexanodioic acid, NSC 6366, TriMethylolPropane(TMP), Tetra hydro Phthalic anhydride, Hypophosporous Acid, 50 and YLENE, logical nitrogen in reaction kettle, and be warming up to 80 ℃, and begin to stir and continue to be warmed up to 160 ℃, be incubated 2 hours;
Step 2. continues to be rapidly heated to 180 ℃ then, is incubated 1 hour;
Step 3. continues to be rapidly heated to 210-220 ℃ of insulation, and esterification is after 3 hours, begins sampling, and is qualified to sample viscosity, acid number, is cooled at once below 150 ℃, adds letdown solvent dun, promptly obtains required wood lacquer and uses the saturated alcohol acid resin.It is as shown in table 3 that the gained resin property is measured the result.
Table 3:
Through embodiment 1 and embodiment 2, prepared saturated alcohol acid resin is more or less the same on each performance index.
With the saturated alkyd resin of embodiment 1 preparation and traditional alkyd resins YTM3380 (long profit is sent out company and produced) with identical lacquer as woodenware finish prescription, be uniformly dispersed under the identical condition and join coat with lacquer spray the plate film forming after, it is as shown in table 4 to detect its results of property.
Two kinds of resin system lacquers of table 4 performance comparison
| Test event | The finish paint that saturated alkyd resin is joined of embodiment 1 preparation | YTM3380 finish paint that traditional alkyd resins is joined |
| Surface drying time | 28 minutes | 35 minutes |
| Do solid work the time | 2 hours 15 minutes | 3 hours 30 minutes |
| Pencil hardness 48h | HBˉ | B |
| Fullness ratio | Good | Better |
| Leveling characteristics | Good | Good |
| Snappiness | 4 grades | 2 grades |
| The transparency | Good | Better |
| Pot-life h | Viscosity thickening behind the 3h | 3.5h back viscosity thickening |
| Anti-heavy property | Better | Better |
| Gloss 60 o glossometers | 85o | 70o |
| Yellowing resistance is pressed the GB/T23983-2009 standard | △E=1.7 | △E=4.1 |
Can find out that from the test result of table 4 paint of the saturated alkyd resin gained of embodiment 1 preparation occupies certain advantage on dryness, hardness and yellowing resistance, other performance is suitable.
Contrast through above instance; Explain that wood lacquer of the present invention given saturated alkyd resin good performance with each components selection in the prescription of saturated alkyd resin really; And the partial properties of this prescription gained also is superior to the made paint of existing Synolac, its yellowing resistance
More traditional Synolac has more advantage.
Claims (4)
1. a wood lacquer is used the saturated alcohol acid resin, by mass percentage: suffering mixing acid 15.0 % in the last of the ten Heavenly stems～22.0%, NSC 6366 5.2 ~ 9.2%, TriMethylolPropane(TMP) 20.6 ~ 30.6%, Tetra hydro Phthalic anhydride 28.6 ~ 38.6%, the agent 0.1 ~ 0.2% of losing lustre, reflux solvent 2.5 ~ 4.5%, letdown solvent dun 10.5 ~ 20.5%.
2. wood lacquer according to claim 1 is used the saturated alcohol acid resin, it is characterized in that: the described agent of losing lustre is a Hypophosporous Acid, 50; Described reflux solvent and letdown solvent dun are YLENE.
3. one kind prepares claim 1 or 2 described wood lacquers are used the saturated alcohol acid resin, and it is characterized in that: its step does
After step 1. drops into reaction kettle with suffering mixing acid in the last of the ten Heavenly stems, NSC 6366, TriMethylolPropane(TMP), Tetra hydro Phthalic anhydride, Hypophosporous Acid, 50 and reflux solvent; Logical nitrogen in reaction kettle, and be warming up to 80 ± 10 ℃, begin to stir and continue to be warmed up to 160 ± 5 ℃; Be incubated 2 ± 0.5 hours;
Step 2. continues to be rapidly heated to 180 ± 10 ℃ then, is incubated 1 ± 0.5 hour;
Step 3. continues to be rapidly heated to 210-220 ℃ of insulation, and esterification to viscosity, acid number are qualified;
Step 4. is cooled to below 150 ℃, adds letdown solvent dun, promptly obtains required wood lacquer and uses the saturated alcohol acid resin.
4. preparation method according to claim 3 is characterized in that: the described agent of losing lustre is a Hypophosporous Acid, 50; Described reflux solvent and letdown solvent dun are YLENE.
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| CN201210070226XA CN102604054A (en) | 2012-03-16 | 2012-03-16 | Saturated alkyd resin for wood lacquer and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145961A (en) * | 2013-02-22 | 2013-06-12 | 嘉宝莉化工集团股份有限公司 | Modified alkyd resin, preparation method thereof and two-component glossy varnish |
| CN107417895A (en) * | 2017-05-19 | 2017-12-01 | 江苏三木化工股份有限公司 | A kind of low winding steel paint base alkyd resin of cost and preparation method |
| CN109593186A (en) * | 2018-11-22 | 2019-04-09 | 广东百川化工有限公司 | High solid environment-friendly alkide resin and preparation method |
| CN113136025A (en) * | 2021-04-19 | 2021-07-20 | 莱阳红安化工有限公司 | Water-soluble saturated polyester resin suitable for water-based steel drum coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557855A (en) * | 2004-02-10 | 2004-12-29 | 方学平 | Alkyd resin for floor paint |
-
2012
- 2012-03-16 CN CN201210070226XA patent/CN102604054A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557855A (en) * | 2004-02-10 | 2004-12-29 | 方学平 | Alkyd resin for floor paint |
Non-Patent Citations (1)
| Title |
|---|
| 徐达春等: "一种高性价比浅色醇酸树脂的合成及应用研究", 《现代涂料与涂装》, vol. 14, no. 7, 31 July 2011 (2011-07-31) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145961A (en) * | 2013-02-22 | 2013-06-12 | 嘉宝莉化工集团股份有限公司 | Modified alkyd resin, preparation method thereof and two-component glossy varnish |
| CN107417895A (en) * | 2017-05-19 | 2017-12-01 | 江苏三木化工股份有限公司 | A kind of low winding steel paint base alkyd resin of cost and preparation method |
| CN107417895B (en) * | 2017-05-19 | 2019-10-25 | 江苏三木化工股份有限公司 | A kind of winding steel paint base alkyd resin and preparation method at low cost |
| CN109593186A (en) * | 2018-11-22 | 2019-04-09 | 广东百川化工有限公司 | High solid environment-friendly alkide resin and preparation method |
| CN113136025A (en) * | 2021-04-19 | 2021-07-20 | 莱阳红安化工有限公司 | Water-soluble saturated polyester resin suitable for water-based steel drum coating and preparation method thereof |
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Application publication date: 20120725 |