CN109749033B - Water-soluble amino resin synthesized from mixed alcohol and preparation method thereof - Google Patents
Water-soluble amino resin synthesized from mixed alcohol and preparation method thereof Download PDFInfo
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- CN109749033B CN109749033B CN201811533438.0A CN201811533438A CN109749033B CN 109749033 B CN109749033 B CN 109749033B CN 201811533438 A CN201811533438 A CN 201811533438A CN 109749033 B CN109749033 B CN 109749033B
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Abstract
The invention discloses a water-soluble amino resin synthesized by mixed alcohol and a preparation method thereof. The resin takes paraformaldehyde, melamine, a catalyst, an etherifying agent, a solvent and the like as raw materials, wherein the etherifying agent is selected from two or more of methanol, ethanol and isopropanol, and the water-soluble amino resin is synthesized from mixed alcohol by a chemical synthesis modification method according to a specific raw material ratio. The production process of the resin is simple, the production efficiency of the water-soluble amino resin is improved, and the production energy consumption and the wastewater treatment cost are reduced. Compared with common methylated amino resin, the mixed alcohol synthesized water-soluble amino resin has lower viscosity, lower molecular weight and a proper amount of reactive groups, has better miscibility with other resins, low baking temperature in paint preparation and high gloss after crosslinking.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a water-soluble amino resin synthesized by mixed alcohol and a preparation method thereof.
Background
The amino resin for the coating is a multifunctional compound containing (-NH)2) Addition condensation of functional compounds with aldehydes, mainly formaldehyde, and subsequent formation of methylol groups (-CH)2OH) and aliphatic monohydric alcohols are partially or completely etherified. Paint films using amino resins as crosslinking agents have excellent gloss, color retention, hardness, chemical resistance, water resistance, weather resistance and the like, and thus, paints using amino resins as crosslinking agents are widely used as industrial paints for automobiles, industrial and agricultural machinery, steel furniture, household appliances, metal precoating and the like.
The common amino resin coating on the market is generally a solvent-based coating and contains a large amount of VOC. At present, frequent coating construction, maintenance and the like easily cause environmental pollution and cause safety and environmental protection problems. Under the current environment-friendly situation, the environment-friendly and water-soluble amino resin coating is more suitable for social environment and personal health. At present, the conventional water-soluble amino resin in China is methylated amino resin, the adopted production process is that melamine reacts with formaldehyde aqueous solution to generate a hydroxymethyl compound, and then the hydroxymethyl compound reacts with excessive methanol through twice etherification reactions to finally generate the methylated water-soluble amino resin.
Disclosure of Invention
The invention aims to provide a method for preparing water-soluble amino resin by mixed alcohol synthesis, aiming at the problems in the prior art.
The purpose of the invention can be realized by the following technical scheme:
a mixed alcohol synthesized water-soluble amino resin is composed of the following components in parts by weight:
in some preferred embodiments: the resin consists of 25-45 parts of paraformaldehyde, 10-20 parts of melamine, 0.05-5 parts of catalyst, 30-50 parts of etherifying agent and 15-25 parts of solvent.
In some more preferred embodiments: 30-40 parts of paraformaldehyde, 13-18 parts of melamine, 0.08-3 parts of catalyst, 35-45 parts of etherifying agent and 18-22 parts of solvent in sequence.
The technical scheme of the invention is as follows: the catalyst is selected from one or more of acetic acid and phthalic anhydride.
The technical scheme of the invention is as follows: the etherifying agent is selected from two or more of methanol, ethanol and isopropanol.
The technical scheme of the invention is as follows: the solvent is selected from one or more of butanol and isobutanol.
A preparation method for synthesizing water-soluble amino resin by using the mixed alcohol comprises the following steps:
the first step is as follows: uniformly mixing paraformaldehyde and 30-60% of etherifying agent, slowly heating to 60-75 ℃, preserving heat for 1-2 hours under the temperature condition to prepare a transparent formaldehyde-etherified alcohol mixed solution, and then cooling to room temperature;
the second step is that: adding melamine, the rest etherifying agent and catalyst into the formaldehyde-etherified alcohol solution, slowly heating to 40-55 ℃, preserving the heat for 20-40min at the temperature, slowly heating to 80-100 ℃, carrying out polycondensation reaction at the temperature, adding a solvent after the reaction is finished, and diluting to obtain the mixed alcohol synthetic water-soluble amino resin.
The method of the invention comprises the following steps: the water-soluble amino resin synthesized by the mixed alcohol has the viscosity range of (2000-3000) mPa & s and the non-volatile part of 79-81 percent under the condition of 25 ℃.
The invention has the beneficial effects that:
the invention discloses a preparation method for synthesizing water-soluble amino resin by mixed alcohol. The resin takes paraformaldehyde, melamine, a catalyst, an etherifying agent, a solvent and the like as raw materials, wherein the etherifying agent is selected from two or more of methanol, ethanol and isopropanol, and the water-soluble amino resin is synthesized from mixed alcohol by a chemical synthesis modification method according to a specific raw material ratio. Compared with the common methylated amino resin, the mixed alcohol synthesized water-soluble amino resin has lower viscosity, lower molecular weight and a proper amount of reactive groups, has better miscibility with other resins, low baking temperature (120 ℃) for preparing paint, and high gloss (more than or equal to 100 and 60 ℃) of a paint film formed after crosslinking; the baking temperature of the conventional methylated amino resin is 150 ℃, and the gloss of a paint film is more than or equal to 90 and 60 degrees.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention:
the formula components and the mass percentage thereof adopted by the water-soluble amino resin synthesized by mixing alcohol are shown in the table I.
The preparation method of the mixed alcohol synthetic water-soluble amino resin of the invention from example 1 to example 3 is as follows:
the first step is as follows: uniformly mixing the paraformaldehyde and a part of etherifying agent of the components, slowly heating to 65 ℃, preserving heat for 1.5 hours under the temperature condition to prepare a transparent formaldehyde-etherified alcohol mixed solution, and then cooling to room temperature;
the second step is that: adding melamine, the rest etherifying agent and the catalyst of the components into the formaldehyde-etherified alcohol solution, slowly heating to 50 ℃, preserving the temperature for 30min, slowly heating to 90 ℃, carrying out polycondensation reaction at the temperature, and adding a solvent for diluting after the reaction is finished to obtain the mixed alcohol synthetic water-soluble amino resin. Then cooling, filtering and packaging to obtain the mixed alcohol synthesized water-soluble amino resin.
Watch 1
Compared with the conventional methanol etherified amino resin, the water-soluble amino resin synthesized by the prepared mixed alcohol has the specific product quality parameters shown in the table II.
Watch two
The comparison shows that the mixed alcohol etherified amino resin synthesized by the technical scheme has lower viscosity. 5717W methylated amino resin is an amino resin produced by Jiangsu Sanmu group Co.
The water-soluble amino resin and 5717W amino resin synthesized in the embodiments 1 to 3 of the present technical scheme are respectively matched with 362-70 water-based polyester to prepare paint, and the paint film performance comparison after baking is as shown in the following table three:
watch III
The 362-70 aqueous polyester resin is produced by Jiangsu Sanmu group Co. Compared with the conventional methylated amino resin, the paint prepared by the technical scheme has high gloss and low baking temperature.
Claims (6)
1. A preparation method for synthesizing water-soluble amino resin by mixed alcohol is characterized in that: the method comprises the following steps:
the first step is as follows: uniformly mixing paraformaldehyde and 30-65% of etherifying agent, slowly heating to 60-75 ℃, preserving heat for 1-2 hours under the temperature condition to prepare a transparent formaldehyde-etherified alcohol mixed solution, and then cooling to room temperature;
the second step is that: adding melamine, the rest etherifying agent and a catalyst into the formaldehyde-etherified alcohol mixed solution, slowly heating to 40-55 ℃, preserving the heat for 20-40min at the temperature, slowly heating to 80-100 ℃, carrying out polycondensation reaction at the temperature, and adding a solvent for diluting after the reaction is finished to obtain the mixed alcohol synthetic water-soluble amino resin;
wherein: the dosage of each component is as follows:
10-45 parts of paraformaldehyde;
1-30 parts of melamine;
0.05-5 parts of a catalyst;
10-50 parts of an etherifying agent;
1-25 parts of a solvent;
the catalyst is selected from one or more of acetic acid and phthalic anhydride.
2. The method of claim 1, wherein: the resin consists of 25-45 parts of paraformaldehyde, 10-20 parts of melamine, 0.05-5 parts of catalyst, 30-50 parts of etherifying agent and 15-25 parts of solvent.
3. The method of claim 1, wherein: 30-40 parts of paraformaldehyde, 13-18 parts of melamine, 0.08-3 parts of catalyst, 35-45 parts of etherifying agent and 18-22 parts of solvent in sequence.
4. The method according to claim 1, characterized in that: the etherifying agent is selected from two or more of methanol, ethanol and isopropanol.
5. The method according to claim 1, characterized in that: the solvent is selected from one or more of butanol and isobutanol.
6. The method of claim 1, wherein: the viscosity of the water-soluble amino resin synthesized by the mixed alcohol is measured to be (2000-3000) mPa.s and the non-volatile matter is (79-81)%, under the condition of 25 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN109749033B true CN109749033B (en) | 2022-03-15 |
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| CN114057969B (en) * | 2021-11-30 | 2024-06-18 | 江苏三木化工股份有限公司 | Amino resin for high-performance coiled material coating and preparation method thereof |
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| JP2002097243A (en) * | 2000-09-26 | 2002-04-02 | Hitachi Chem Co Ltd | Modified amino resin, its production method and water soluble resin composition |
| JP2004051696A (en) * | 2002-07-17 | 2004-02-19 | Hitachi Chem Co Ltd | Water-soluble resin composition, alkyl etherified amino resin, and its production method |
| CN102050933A (en) * | 2010-12-17 | 2011-05-11 | 上海涂料有限公司上海新华树脂厂 | Methanol and isobutanol mixed ether amino resin and preparation method thereof |
| CN102604470A (en) * | 2012-02-27 | 2012-07-25 | 长兴化学工业(中国)有限公司 | Energy-saving crosslinking agent for low-temperature baking varnish |
| CN102993394A (en) * | 2012-11-19 | 2013-03-27 | 江苏三木集团有限公司 | New process for producing methylated amino resin through multi-step etherification |
| CN105440232A (en) * | 2015-11-27 | 2016-03-30 | 河南骏化发展股份有限公司 | Preparation process of water-soluble methyl-etherified melamine formaldehyde resin |
| CN106117477A (en) * | 2016-08-27 | 2016-11-16 | 合肥普庆新材料科技有限公司 | A kind of method of methanol, isopropanol complex etherified production of melamine resin |
| CN106117478A (en) * | 2016-08-27 | 2016-11-16 | 合肥普庆新材料科技有限公司 | A kind of method of methanol, ethanol complex etherified production of melamine resin |
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- 2018-12-14 CN CN201811533438.0A patent/CN109749033B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002097243A (en) * | 2000-09-26 | 2002-04-02 | Hitachi Chem Co Ltd | Modified amino resin, its production method and water soluble resin composition |
| JP2004051696A (en) * | 2002-07-17 | 2004-02-19 | Hitachi Chem Co Ltd | Water-soluble resin composition, alkyl etherified amino resin, and its production method |
| CN102050933A (en) * | 2010-12-17 | 2011-05-11 | 上海涂料有限公司上海新华树脂厂 | Methanol and isobutanol mixed ether amino resin and preparation method thereof |
| CN102604470A (en) * | 2012-02-27 | 2012-07-25 | 长兴化学工业(中国)有限公司 | Energy-saving crosslinking agent for low-temperature baking varnish |
| CN102993394A (en) * | 2012-11-19 | 2013-03-27 | 江苏三木集团有限公司 | New process for producing methylated amino resin through multi-step etherification |
| CN105440232A (en) * | 2015-11-27 | 2016-03-30 | 河南骏化发展股份有限公司 | Preparation process of water-soluble methyl-etherified melamine formaldehyde resin |
| CN106117477A (en) * | 2016-08-27 | 2016-11-16 | 合肥普庆新材料科技有限公司 | A kind of method of methanol, isopropanol complex etherified production of melamine resin |
| CN106117478A (en) * | 2016-08-27 | 2016-11-16 | 合肥普庆新材料科技有限公司 | A kind of method of methanol, ethanol complex etherified production of melamine resin |
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