CN101348692A - Modified raw lacquer and preparation thereof - Google Patents
Modified raw lacquer and preparation thereof Download PDFInfo
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- CN101348692A CN101348692A CNA2008101188332A CN200810118833A CN101348692A CN 101348692 A CN101348692 A CN 101348692A CN A2008101188332 A CNA2008101188332 A CN A2008101188332A CN 200810118833 A CN200810118833 A CN 200810118833A CN 101348692 A CN101348692 A CN 101348692A
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Abstract
The invention discloses a modified raw lacquer and a method for preparing the same; and the method for preparing the modified raw lacquer adopts raw lacquer and rosin to perform esterification reaction. A lacquer film of the raw lacquer prepared by the method remarkably improves the performance, obviously shortens the drying time and remarkably improves the adhesive force, impact resistance and scratch hardness.
Description
Technical field
The present invention relates to coating composition of a kind of natural resin and preparation method thereof, particularly a kind of raw lacquer and preparation method thereof.
Background technology
The economic worth of raw lacquer is very high, have corrosion resistant, wear-resisting, acidproof, anti-solvent, heat-resisting, water proof and good insulating, be rich in gloss and wait for property, be the high-quality coating of military project, industrial equipments, fundamental construction, handicraft and civilian furniture etc., also be one of valuable cargo of China's tradition outlet, and be world-famous for well to measure many matter.Raw lacquer lacquer liquid film forming is hard and be rich in gloss, is ageing-resistant, acidproof, alkaline-resisting, water-fast, high temperature resistant, organic solvent-resistant, wear-resisting, natural paint that insulating property are superior, is commonly called as " king of coating ".
But raw lacquer has serious irritated toxicity to human body, and (relative humidity is not less than 80%, 20～30 ℃) could be dry under given conditions, viscosity is big, is difficult for construction, and is bad to metal sticking power, alkali resistance is poor, thereby, seriously limited its range of application.
Mainly be to carry out modification in the present research at the laccol in the raw lacquer.Main component laccol in the raw lacquer is the pyrocatechol that has unsaturated long side chain, side chain and two hydroxyls all are to make phenyl ring activatory electron-donating group, make and on phenyl ring, easily carry out electrophilic substitution reaction, make laccol metallizing thing that redox reaction and coordination reaction take place earlier and generate inner complex, further polymerization becomes the product that has inner complex characteristics and raw lacquer proper property concurrently then.This method also can be synthesized the laccol metal polymer of different valence state such as laccol titanium, copper, tin.The method of laccol metal polymer modified raw lacquer need be made with extra care raw lacquer, makes laccol, adopts the raw lacquer direct reaction, and the laccol metal polymer film forming after drying time that obtains is long, and paint film property is poor.
The patent disclosure of publication number CN1557893 a kind of copolymerization coating that makes with the reaction of pyrocatechol modified terpene resin and raw lacquer, the compound that obtains by pyrocatechol modified terpene resin and raw lacquer copolymerization, its preparation method comprises the preparation of pyrocatechol modified terpene resin and two steps of preparation of pyrocatechol modified terpene resin-raw lacquer copolymerization coating, the preparation of terpenes pyrocatechol resin is with terpine resin and pyrocatechol, use dissolution with solvents, use anhydrous AlCl
3Catalysis, isolating the upper strata is organic layer, through washing, separates, drying obtains the pyrocatechol modified terpene resin; Again raw lacquer is dissolved in the solvent, adds the pyrocatechol modified terpene resin, add catalyst reaction and obtain pyrocatechol modified terpene resin-raw lacquer copolymerization coating, this preparation method's complex procedures, complex operation, long reaction time, production efficiency is low, the production cost height, and the rate ratio rosin of terpine resin is low, and the film-forming properties of pyrocatechol modified terpene resin own is relatively poor, and gained drying varniss speed is very slow, time of drying is long, influences the use of finished product.
Rosin is natural, the cheap Forest products of China, mainly is made up of resinous acid, and other has little fat acid and neutral substance.Rosin is soluble in various organic solvents, and easy film forming, and is glossy.
Do not find as yet at present to utilize rosin, improve the document and the patent application of raw lacquer paint film property the raw lacquer modification.
Summary of the invention
The objective of the invention is problem, a kind of modified raw lacquer and preparation method thereof is provided at above prior art existence.Paint film property by the raw lacquer of the inventive method preparation is significantly improved, and not only obviously shorten time of drying, and raw lacquer paint film adhesion, impact resistance, scratch hardness significantly improves.
For realizing purpose of the present invention, one aspect of the present invention provides a kind of preparation method of modified raw lacquer: make raw lacquer and rosin carry out esterification.
Wherein, the weight part proportioning of rosin and raw lacquer is 1-15: 100, be preferably 5-10: 100.
The present invention provides a kind of preparation method of modified raw lacquer on the other hand, comprises following step in sequence:
1) the weight part proportioning according to rosin and raw lacquer is 1-15: 100 ratio is got the raw materials ready;
2) in raw lacquer, add rosin, stir, under vacuum state, be heated to 40-70 ℃, carry out esterification 2-4h.
Wherein, the weight part proportion optimization of rosin described in the step 1) and raw lacquer is 5-10: 100; Described rosin is selected solid rosin powder or rosin solution; Described rosin solution is the rosin ethanolic soln; Step 2) esterification reaction temperature described in is preferably 45-60 ℃, and the reaction times is preferably 2.5-3.5h; The vacuum tightness of described vacuum state is-0.07～-0.10Mpa, be preferably-0.08～-0.09Mpa, be 0 promptly with a normal atmosphere, with respect to an atmospheric vacuum tightness be-0.07～-0.10MPa.
Particularly, the mass percent concentration of described rosin ethanolic soln is 20%.
Another aspect of the invention provides a kind of preparation method of modified raw lacquer, at first makes raw lacquer and metal ion reagent carry out polyreaction and generates raw lacquer metal ion polymkeric substance; Make raw lacquer metal ion polymkeric substance and rosin carry out esterification then.
Wherein, the weight part proportioning of described metal ion reagent and raw lacquer is 10-30: 100, be preferably 20: 100; The weight part proportioning of described rosin and raw lacquer is 1-15: 100, be preferably 5-10: 100.
Particularly, described metal ion reagent is FeCl
3Ethanolic soln, SnCl
2Ethanolic soln, SbCl
3In the ethanolic soln one or more, the mass percent concentration of described solution are 20%.
The present invention provides a kind of preparation method of modified raw lacquer on the other hand, comprises following step in sequence:
1) get the raw materials ready according to following weight part proportioning:
Metal ion reagent 10-30, rosin 1-15, raw lacquer 100;
2) in raw lacquer, add metal ion reagent, stir, be heated to 60-100 ℃ then, carry out polyreaction 30-60min, make raw lacquer metal ion polymkeric substance.
3) in raw lacquer metal ion polymkeric substance, add rosin, stir, under vacuum state, be heated to 40-70 ℃, carry out esterification 2-4h.
Wherein, the proportioning of weight part described in the step 1) is chosen as: metal ion reagent 20, rosin 5-10, raw lacquer 100; Described metal ion reagent is FeCl
3Ethanolic soln, SnCl
2Ethanolic soln, SbCl
3In the ethanolic soln one or more, the mass percent concentration of described solution are 20%.Described rosin is selected solid rosin powder or rosin solution; Described rosin solution is the rosin ethanolic soln.
Particularly, the mass percent concentration of described rosin ethanolic soln is 20%.
Wherein, step 2) described Heating temperature is chosen as 70-90 ℃, and polymerization reaction time is chosen as 35-50min; The temperature of reacting by heating described in the step 3) is chosen as 45-60 ℃, and the reaction times is chosen as 2.5-3.5h; The vacuum tightness of described vacuum state is-0.07～-0.10Mpa, be preferably-0.08～-0.09Mpa, promptly establishing a normal atmosphere is 0, with respect to an atmospheric vacuum tightness be-0.07～-0.10MPa
Another aspect of the invention provides a kind of modified raw lacquer that is prepared from according to the method described above.
The modified raw lacquer of the present invention's preparation has following advantage:
1, modified raw lacquer of the present invention adopts raw lacquer and rosin to carry out esterification and makes, and this preparation method's technology is simple, and working method is simple and easy to do, and production cost is low.
2, the modified raw lacquer of the inventive method preparation has good film-forming properties, and the thickness of paint film reaches 0.56mm.
3, its impact resistance of modified raw lacquer and the sticking power of the inventive method preparation significantly strengthen; Shorten the time of drying of paint film; The hardness cut reaches H or 2H rank, and the performance index of the paint film that modified raw lacquer coats all are up to state standards.
Embodiment
Natural raw lacquer, Sichuan, the place of production.
Embodiment 1
1) add solid rosin powder in the 500mL there-necked flask that raw lacquer is housed, the rosin weight that control adds is 5: 100 with the ratio of raw lacquer weight, stirs;
2) interface in the there-necked flask is connected with vacuum distillation apparatus, two other interface connects thermometer, agitator respectively, heat then, stir and decompression vacuum pumping, the vacuum tightness of control in the there-necked flask for-0.09Mpa (is 0 with a normal atmosphere promptly, with respect to an atmospheric vacuum tightness be-0.09Mpa), make rosin and raw lacquer mixed solution be heated to 50 ℃, reacted with this understanding 3 hours, promptly obtain the raw lacquer of modification.
Embodiment 2
1) add solid rosin powder in the 500mL there-necked flask that raw lacquer is housed, the solid rosiny weight that control adds is 10: 100 with the ratio of the weight of raw lacquer, stirs;
2) interface in the there-necked flask is connected with vacuum distillation apparatus, two other interface connects thermometer, agitator respectively, heat then, stir and decompression vacuum pumping, the vacuum tightness of control in the there-necked flask for-0.07Mpa (is 0 with a normal atmosphere promptly, with respect to an atmospheric vacuum tightness be-0.07Mpa), make rosin and raw lacquer mixed solution be heated to 45 ℃, reacted with this understanding 4 hours, promptly obtain the raw lacquer of modification.
Embodiment 3
1) adding mass percent concentration in the 500mL there-necked flask that raw lacquer is housed is 20% rosin ethanolic soln, and the rosiny weight that control adds is 5: 100 with the ratio of raw lacquer weight, stirs;
2) interface in the there-necked flask is connected with vacuum distillation apparatus, two other interface connects thermometer, agitator respectively, heat then, stir and decompression vacuum pumping, the vacuum tightness of control in the there-necked flask for-0.08Mpa (is 0 with a normal atmosphere promptly, with respect to an atmospheric vacuum tightness be-0.08Mpa), make rosin and raw lacquer mixed solution be heated to 70 ℃, reacted with this understanding 3 hours, promptly obtain the raw lacquer of modification.
Embodiment 4
1) adding mass percent concentration in the 500mL there-necked flask that raw lacquer is housed is 20% rosin ethanolic soln, and the rosiny weight that control adds is 1: 100 with the ratio of raw lacquer weight, stirs;
2) interface in the there-necked flask is connected with vacuum distillation apparatus, two other interface connects thermometer, agitator respectively, heat then, stir and decompression vacuum pumping, the vacuum tightness of control in the there-necked flask for-0.09Mpa (is 0 with a normal atmosphere promptly, with respect to an atmospheric vacuum tightness be-0.09Mpa), make rosin and raw lacquer mixed solution be heated to 60 ℃, reacted with this understanding 2.5 hours, promptly obtain the raw lacquer of modification.
Embodiment 5
1) adding mass percent concentration in the 500mL there-necked flask that raw lacquer is housed is 20% FeCl
3Dissolve with ethanol liquid, the FeCl that control adds
3The weight of dissolve with ethanol liquid is 20: 100 with the ratio of raw lacquer weight, stirs.Be heated to 80 ℃, the reaction of raw lacquer and iron ion is 40 minutes under this temperature, makes raw lacquer iron ion polymkeric substance.
2) after the raw lacquer iron ion polymkeric substance that step 1) is prepared is cooled to 50 ℃, add 20% rosin ethanolic soln, stir.Wherein, the rosiny weight of control adding is 5: 100 with the ratio of raw lacquer weight;
3) interface in the there-necked flask is connected with vacuum distillation apparatus, two other interface connects thermometer, agitator respectively, heat then, stir and decompression vacuum pumping, the vacuum tightness of control in the there-necked flask for-0.07Mpa (is 0 with a normal atmosphere promptly, with respect to an atmospheric vacuum tightness be-0.07Mpa), make rosin and raw lacquer mixed solution be heated to 50 ℃, reacted with this understanding 3 hours, promptly obtain the raw lacquer of modification.
Embodiment 6
1) the adding mass percent concentration is 20% SbCl in the 500mL there-necked flask that raw lacquer is housed
3Dissolve with ethanol liquid, the SbCl that control adds
3The weight of dissolve with ethanol liquid is 20: 100 with the ratio of raw lacquer weight, stirs, and is heated to 80 ℃ of reactions 40 minutes, makes raw lacquer antimony ion polymkeric substance.
2) after the raw lacquer antimony ion polymkeric substance that step 1) is prepared was cooled to 50 ℃, the adding mass percent concentration was 20% rosin ethanolic soln, stirs.Wherein, the rosiny weight of control adding is 10: 100 with the ratio of raw lacquer weight;
3) interface in the there-necked flask is connected with vacuum distillation apparatus, two other interface connects thermometer, agitator respectively, heat then, stir and decompression vacuum pumping, the vacuum tightness of control in the there-necked flask for-0.08Mpa (is 0 with a normal atmosphere promptly, with respect to an atmospheric vacuum tightness be-0.08Mpa), make rosin and raw lacquer mixed solution be heated to 50 ℃, reacted with this understanding 2.5 hours, promptly obtain the raw lacquer of modification.
Embodiment 7
1) the adding mass percent concentration is 20% SnCl in the 500mL there-necked flask that raw lacquer is housed
2Dissolve with ethanol liquid, the SnCl that control adds
2The weight of dissolve with ethanol liquid is 20: 100 with the ratio of raw lacquer weight, stirs, and is heated to 90 ℃ of reactions 50 minutes, makes raw lacquer tin ion polymkeric substance.
2) after the raw lacquer tin ion polymkeric substance that step 1) is prepared was cooled to 40 ℃, the adding mass percent concentration was 20% rosin ethanolic soln, stirs.Wherein, the rosiny weight of control adding is 15: 100 with the ratio of raw lacquer weight.
3) interface in the there-necked flask is connected with vacuum distillation apparatus, two other interface connects thermometer, agitator respectively, heat then, stir and decompression vacuum pumping, the vacuum tightness of control in the there-necked flask for-0.09Mpa (is 0 with a normal atmosphere promptly, with respect to an atmospheric vacuum tightness be-0.09Mpa), make rosin and raw lacquer mixed solution be heated to 45 ℃, reacted with this understanding 3.5 hours, promptly obtain the raw lacquer of modification.
Reference examples
Reference examples 1
Adopt above-mentioned identical with the embodiment 1-7 rosiny natural raw lacquer example 1 in contrast of not adding.
Reference examples 2
Adopt with the foregoing description 1 in identical rosin example 2 in contrast.
The test example
1) modified raw lacquer of embodiment 1-7 preparation and the raw lacquer of reference examples 1 are coated paint film according to the GB1727-1992 national standard;
The solid rosin of reference examples 2 is made into the rosin alcohol saturated solution after adopting dissolve with ethanol, and then coats paint film according to the GB1727-1992 national standard.
2) will brush paint film and place the air solvent flashing, to surface drying.
3) after the paint film plate behind the solvent flashing places 110 ℃ of baking oven baking 1.5h, measure the performance of paint film.
The thickness of paint film, impact resistance, sticking power, hardness cut, time of drying are measured according to GB/T1764-1989, GB/T1732-1993, GB/T1720-1989, GB/T6739-1996 and GB/T1728-1989 national standard respectively.Measurement result sees Table 1.
The performance index detected result of table 1 paint film
| Time of drying | Sticking power | Surging force | Cut | Film thickness | |
| Embodiment 1 | Surface drying: 31～32h does solid work: 79h | 6～7 grades | ＜15cm | H | 0.6mm |
| Embodiment 2 | Surface drying: 32～33h does solid work: 80h | 6～7 grades | ＜15cm | H | 0.63mm |
| Embodiment 3 | Surface drying: 28～29h does solid work: 72h | 6 grades | ＜15cm | H | 0.6mm |
| Embodiment 4 | Surface drying: 30～31h does solid work: 73h | 6 grades | ＜15cm | H | 0.58mm |
| Embodiment 5 | Surface drying: 1～2h does solid work: 53h | 4～5 grades | ＜30cm | 2H | 0.65mm |
| Embodiment 6 | Surface drying: 2～3h does solid work: 59h | 5～6 grades | ＜25cm | 2H | 0.63mm |
| Embodiment 7 | Surface drying: 1～2h does solid work: 58h | 3～4 grades | ＜30cm | H | 0.68mm |
| Reference examples 1 | Surface drying: 48～49h does solid work: 97h | 7 grades | ＜5cm | B | 0.7mm |
| Reference examples 2 | Surface drying: 46～47h does solid work: 83h | 7 grades | ＜5cm | HB | 0.6mm |
The detected result of table 1 shows: add rosin and all can improve the raw lacquer paint film property, every performance index of the paint film of Abietyl modified raw lacquer all are significantly increased, and meet and exceed the thickness of paint film, impact resistance, sticking power, hardness cut, time of drying etc. the national standard of GB/T1764-1989, GB/T1732-1993, GB/T1720-1989, GB/T6739-1996 and GB/T1728-1989 respectively.
The time of drying of Abietyl modified raw lacquer by surface drying 48～49h, do solid work 97h and shorten to surface drying 28～29h, do solid work 72h; The sticking power grade also rises to 6～7 grades by 7 grades; The impact resistance grade is risen to＜15cm by＜5cm, has increased 10cm; The pencil cut also rises to the H level by the B level; Film thickness reduces, and shows easier film forming.
Raw lacquer is through after the metallic iron ionic polymerization, adds Abietyl modifiedly again, and every index of film forming properties all is significantly increased, time of drying by surface drying 48～49h, do solid work 97h and shorten to surface drying 1～2h, do solid work 53h; Sticking power is brought up to 3～4 grades by 7 grades; The impact resistance grade is risen to＜30cm by＜5cm, has increased 25cm; It is 2H that cut is promoted by the B grade, and film thickness reduces, and shows easier film forming.
Claims (10)
1, a kind of preparation method of modified raw lacquer is characterized in that making raw lacquer and rosin to carry out esterification.
2, a kind of preparation method of modified raw lacquer is characterized in that, comprises following step in sequence:
1) gets the raw materials ready according to following weight part proportioning: rosin 1-15, raw lacquer 100;
2) in raw lacquer, add rosin, stir, under vacuum state, be heated to 40-70 ℃, carry out esterification 2-4h.
3, preparation method as claimed in claim 2 is characterized in that, the described rosin weight part of step 1) is chosen as 5-10.
4, preparation method as claimed in claim 2 is characterized in that, described step 2) described in temperature be 45-60 ℃, the reaction times is 2.5-3.5h.
5, a kind of preparation method of modified raw lacquer is characterized in that, at first makes raw lacquer and metal ion reagent carry out polyreaction and generates raw lacquer metal ion polymkeric substance; Make raw lacquer metal ion polymkeric substance and rosin carry out esterification then.
6, as preparation method as described in the claim 5, it is characterized in that the weight part proportioning of described metal ion reagent and raw lacquer is 10-30: 100; The weight part proportioning of described rosin and raw lacquer is 1-15: 100.
7, a kind of preparation method of modified raw lacquer is characterized in that, comprises following step in sequence:
1) get the raw materials ready according to following weight part proportioning:
Metal ion reagent 10-30, rosin 1-15, raw lacquer 100;
2) add metal ion reagent in raw lacquer, stir, be heated to 60-100 ℃ then, reaction 30-60min makes raw lacquer metal ion polymkeric substance;
3) in raw lacquer metal ion polymkeric substance, add rosin, stir, under vacuum state, be heated to 40-70 ℃, carry out esterification 2-4h.
8, preparation method as claimed in claim 7 is characterized in that, the weight part proportioning of described raw material is chosen as metal ion reagent 20, rosin 5-10, raw lacquer 100.
9, as claim 7 or 8 described preparation methods, it is characterized in that step 2) described reacting by heating selection of time is 35-50 min.
10, a kind of modified raw lacquer is characterized in that, is prepared from according to method as described in arbitrary as claim 1-9.
Priority Applications (1)
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| CN2008101188332A CN101348692B (en) | 2008-08-25 | 2008-08-25 | Modified raw lacquer and preparation thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101188332A CN101348692B (en) | 2008-08-25 | 2008-08-25 | Modified raw lacquer and preparation thereof |
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| CN101348692A true CN101348692A (en) | 2009-01-21 |
| CN101348692B CN101348692B (en) | 2011-01-12 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101586000B (en) * | 2009-05-15 | 2011-06-22 | 湖北宝石花工艺品有限公司 | Modulation method of raw lacquer |
| CN104497877A (en) * | 2014-12-26 | 2015-04-08 | 常州大学 | Quick self-drying modified raw lacquer and preparation method thereof |
| CN105062362A (en) * | 2015-07-23 | 2015-11-18 | 韦海棉 | Method for catalyzing oxidative polymerization of urushiol |
| CN105462502A (en) * | 2015-12-07 | 2016-04-06 | 中华全国供销合作总社西安生漆涂料研究所 | Light-color raw lacquer resin and preparation method thereof |
| CN113462289A (en) * | 2021-07-22 | 2021-10-01 | 闽江学院 | Method for changing raw lacquer curing speed |
-
2008
- 2008-08-25 CN CN2008101188332A patent/CN101348692B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101586000B (en) * | 2009-05-15 | 2011-06-22 | 湖北宝石花工艺品有限公司 | Modulation method of raw lacquer |
| CN104497877A (en) * | 2014-12-26 | 2015-04-08 | 常州大学 | Quick self-drying modified raw lacquer and preparation method thereof |
| CN105062362A (en) * | 2015-07-23 | 2015-11-18 | 韦海棉 | Method for catalyzing oxidative polymerization of urushiol |
| CN105462502A (en) * | 2015-12-07 | 2016-04-06 | 中华全国供销合作总社西安生漆涂料研究所 | Light-color raw lacquer resin and preparation method thereof |
| CN105462502B (en) * | 2015-12-07 | 2018-11-23 | 中华全国供销合作总社西安生漆涂料研究所 | A kind of raw lacquer light-colored resin and preparation method thereof |
| CN113462289A (en) * | 2021-07-22 | 2021-10-01 | 闽江学院 | Method for changing raw lacquer curing speed |
| CN113462289B (en) * | 2021-07-22 | 2022-06-28 | 闽江学院 | Method for changing raw lacquer curing speed |
| WO2023000504A1 (en) * | 2021-07-22 | 2023-01-26 | 闽江学院 | Method for changing curing speed of raw lacquer |
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| CN101348692B (en) | 2011-01-12 |
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