CN115198556B - Melamine resin curing agent and preparation method thereof - Google Patents
Melamine resin curing agent and preparation method thereof Download PDFInfo
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- CN115198556B CN115198556B CN202111045285.7A CN202111045285A CN115198556B CN 115198556 B CN115198556 B CN 115198556B CN 202111045285 A CN202111045285 A CN 202111045285A CN 115198556 B CN115198556 B CN 115198556B
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- acid
- melamine resin
- curing agent
- urea
- organic acid
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/47—Condensation polymers of aldehydes or ketones
- D21H17/49—Condensation polymers of aldehydes or ketones with compounds containing hydrogen bound to nitrogen
- D21H17/51—Triazines, e.g. melamine
Abstract
The invention discloses a melamine resin curing agent and a preparation method thereof, alkyl sulfonate, organic acid, inorganic acid, alcohol amine and urea are used as raw materials, the prepared curing agent has good normal-temperature latency, the curing of melamine resin at normal temperature or non-curing temperature is avoided, the usability of melamine resin and melamine resin impregnated paper is improved, and the curing agent prepared by the invention can also reduce the formaldehyde emission in the melamine resin and improve the environmental protection of the melamine resin and the melamine resin impregnated paper.
Description
Technical Field
The invention belongs to the field of C08L61/28, and particularly relates to a melamine resin curing agent and a preparation method thereof.
Background
The wide application of melamine impregnated paper in the field of home furnishings has driven the development of the melamine impregnated paper industry. The use of melamine impregnated paper can simplify the production process of the plate furniture and improve the aesthetic degree of the furniture. The quality of melamine impregnated paper has a close relationship with melamine resins, additives, etc. In order to solve the problems of excessively high curing speed, uneven resin layer, poor pollution resistance, low resin latency and the like of melamine impregnated paper, the applicant discloses a curing agent in China patent CN111592686A, which is prepared by taking ammonia water, hydrochloric acid, diethanolamine and triethanolamine as raw materials, but the curing agent can possibly reduce the curing capability of the curing agent after the raw materials react in the using process, so that the curing time of melamine resin is prolonged. Based on this, the applicant discloses a melamine resin curing agent and a method for preparing the same.
Disclosure of Invention
The first aspect of the invention provides a melamine resin curing agent, which comprises the following raw materials: alkyl sulfonate, organic acid, inorganic acid, alcohol amine and urea.
In a preferred embodiment, the organic acid is a complex of an aromatic organic acid and an aliphatic organic acid.
In a preferred embodiment, the mass ratio of the aromatic organic acid to the aliphatic organic acid is (1 to 1.6): (2.5-5).
In a preferred embodiment, the aromatic organic acid is at least one selected from the group consisting of benzoic acid, terephthalic acid, phthalic acid, isophthalic acid, sodium phenyl methane sulfonate, and p-toluene sulfonic acid.
In a preferred embodiment, the aromatic organic acid is p-toluene sulfonic acid.
In a preferred embodiment, the aliphatic organic acid is selected from at least one of formic acid, acetic acid, propionic acid, butyric acid, valeric acid, oxalic acid, glycolic acid, succinic acid, malonic acid, tartaric acid.
In a preferred embodiment, the aliphatic organic acid is oxalic acid.
In a preferred embodiment, the mass ratio of the aromatic organic acid to the aliphatic organic acid is (1.2 to 1.6): (2.8-4.6).
In a preferred embodiment, the mass ratio of the aromatic organic acid to the aliphatic organic acid is 4:15.
in a preferred embodiment, the inorganic acid is selected from at least one of hydrochloric acid, sulfuric acid, phosphoric acid, and nitric acid.
In a preferred embodiment, the mineral acid is sulfuric acid.
In a preferred embodiment, the sulfuric acid is a 50-70wt% aqueous sulfuric acid solution.
In a preferred embodiment, the sulfuric acid is a 50wt% aqueous sulfuric acid solution.
In a preferred embodiment, the mass ratio of the mineral acid to urea is (3-6): 1.
in a preferred embodiment, the mass ratio of mineral acid to urea is 3:1.
In a preferred embodiment, the alcohol amine is a secondary and/or tertiary amine alcohol.
In a preferred embodiment, the tertiary amine alcohol is selected from at least one of triethanolamine, triisopropanolamine, N-butyldiethanolamine, N-dibutylethanolamine, N-ethyldiethanolamine, N-isobutyldiethanolamine, N-butyldiisopropylethanolamine, N- (3-aminopropyl) diethanolamine.
In a preferred embodiment, the tertiary amine alcohol is a combination of triethanolamine and triisopropanolamine.
In a preferred embodiment, the mass ratio of triethanolamine to triisopropanolamine is (5-10): 1.5.
in a preferred embodiment, the mass ratio of triethanolamine to triisopropanolamine is 8:1.5.
In a preferred embodiment, the raw materials comprise the following components in percentage by mass: 10-26% of alkyl sulfonate, 14-22% of organic acid, 15-28% of inorganic acid, 4-11% of urea and the balance of alcohol amine.
In a preferred embodiment, the raw materials comprise the following components in percentage by mass: 10-20% of alkyl sulfonate, 14-18% of organic acid, 20-28% of inorganic acid, 6-11% of urea and the balance of alcohol amine.
In a preferred embodiment, the raw materials comprise 10% of alkyl sulfonate, 15% of organic acid, 24% of inorganic acid, 8% of urea and the balance of alcohol amine in percentage by mass.
In a preferred embodiment, the alkyl sulfonate is sodium dodecyl sulfonate.
The applicant finds in the experimental process that the curing agent prepared by the invention has good stability, and when the mass ratio of triethanolamine to triisopropanolamine is 8:1.5, the curing agent can interact with organic acid and other substances in the system, so that the latency of the curing agent of the system at normal temperature is improved, and the addition of inorganic acid, urea and other substances in the system can generate inorganic ammonium salt, so that the viscosity of melamine resin is improved, the usability of melamine impregnated paper is improved, and the addition of alkyl sulfonate in the curing agent of the system can improve the compatibility of the curing agent and melamine resin, and meanwhile, the addition of inorganic acid can reduce the formaldehyde emission in the melamine resin, improve the environmental protection of the melamine resin, and expand and improve the use field and environmental protection degree of the melamine impregnated paper.
The second aspect of the invention provides a preparation method of a melamine resin curing agent, which comprises the following steps: adding alcohol amine into a reaction kettle, adding urea, adding inorganic acid, organic acid and alkyl sulfonate, and uniformly stirring to obtain the curing agent.
Compared with the prior art, the invention has the beneficial effects that:
1. the curing agent prepared by the invention takes inorganic acid, organic acid, urea, alcohol amine and alkyl sulfonate as raw materials, so that the latency of the curing agent at normal temperature is improved, the curing of melamine resin at normal temperature or non-curing temperature is avoided, and the stability and surface smoothness of the melamine resin impregnated paper are improved. When the desired curing temperature is reached, the curing agent may in turn react with the melamine resin to promote curing of the melamine resin.
2. The curing agent prepared by the invention can reduce the formaldehyde emission in the melamine resin and improve the environmental protection of the melamine resin and the melamine resin impregnated paper.
3. The curing agent prepared by the invention has the advantages of simple and easily obtained raw materials, simple preparation method, strong operability and wide application field, and is particularly suitable for melamine resin for impregnated paper.
Detailed Description
The raw materials used in the invention are all commercial products, and the purchasing manufacturer does not limit the raw materials specifically.
Example 1
The first aspect of the invention provides a melamine resin curing agent, which comprises the following raw materials by mass percent, and the balance of 10% sodium dodecyl sulfate, 15% organic acid, 24% sulfuric acid, 8% urea and alcohol amine.
Wherein the organic acid is a compound substance of p-toluenesulfonic acid and oxalic acid, and the mass ratio of the p-toluenesulfonic acid to the oxalic acid is 4:15.
The alcohol amine is a compound substance of triethanolamine and triisopropanolamine, and the mass ratio of the triethanolamine to the triisopropanolamine is 8:1.5.
Sulfuric acid is a 50wt% aqueous sulfuric acid solution.
The second aspect of the invention provides a preparation method of a melamine resin curing agent, which comprises the following steps: adding alcohol amine into a reaction kettle, adding urea, sulfuric acid, organic acid and sodium dodecyl sulfate, and uniformly stirring to obtain the curing agent.
Example 2
The first aspect of the invention provides a melamine resin curing agent, which comprises the following raw materials by mass percent, and the balance of 10% sodium dodecyl sulfate, 15% organic acid, 24% sulfuric acid, 8% urea and alcohol amine.
Wherein the organic acid is a compound substance of p-toluenesulfonic acid and oxalic acid, and the mass ratio of the p-toluenesulfonic acid to the oxalic acid is 4:15.
The alcohol amine is triethanolamine.
Sulfuric acid is a 50wt% aqueous sulfuric acid solution.
The second aspect of the invention provides a preparation method of a melamine resin curing agent, which comprises the following steps: adding alcohol amine into a reaction kettle, adding urea, sulfuric acid, organic acid and sodium dodecyl sulfate, and uniformly stirring to obtain the curing agent.
Example 3
The first aspect of the invention provides a melamine resin curing agent, which comprises the following raw materials by mass percent, 10% of sodium dodecyl sulfate, 25% of organic acid, 8% of urea and the balance of alcohol amine.
Wherein the organic acid is a compound substance of p-toluenesulfonic acid and oxalic acid, and the mass ratio of the p-toluenesulfonic acid to the oxalic acid is 15:4.
The alcohol amine is a compound substance of triethanolamine and triisopropanolamine, and the mass ratio of the triethanolamine to the triisopropanolamine is 1.5:8.
The second aspect of the invention provides a preparation method of a melamine resin curing agent, which comprises the following steps: adding alcohol amine into a reaction kettle, adding urea, sulfuric acid, organic acid and sodium dodecyl sulfate, and uniformly stirring to obtain the curing agent.
Example 4
The first aspect of the invention provides a melamine resin curing agent, which comprises the following raw materials by mass percent, and the balance of 10% sodium dodecyl sulfate, 15% organic acid, 24% sulfuric acid, 8% urea and alcohol amine.
Wherein the organic acid is a compound substance of p-toluenesulfonic acid and oxalic acid, and the mass ratio of the p-toluenesulfonic acid to the oxalic acid is 4:15.
The alcohol amine is a compound substance of triethanolamine and triisopropanolamine, and the mass ratio of the triethanolamine to the triisopropanolamine is 8:1.5.
Sulfuric acid is a 50wt% aqueous sulfuric acid solution.
The second aspect of the invention provides a preparation method of a melamine resin curing agent, which comprises the following steps: adding alcohol amine into a reaction kettle, adding urea, sulfuric acid, organic acid and sodium dodecyl sulfate, and uniformly stirring to obtain the curing agent.
Performance testing
The curing agent prepared in the embodiment is compounded with the commercially available melamine resin according to the mass ratio of 1:100, and the curing time and stability of the compounded composition are tested. The data are recorded in table 1.
1. Curing time
The compounded composition is filled into a transparent glass tube, and is placed at 130 ℃ to observe the whitening condition of the composition. When the composition is fully and uniformly blushed, it is defined as the composition being fully cured. The time required for the composition to fully whiten was recorded.
2. Stability of
The compounded composition is smeared on the surface of impregnated paper, the impregnated paper is placed at room temperature, the service performance of the impregnated paper is tested once in 1 month, and the time of bubbling, uneven glossiness and the like of the impregnated paper in the use process is recorded.
TABLE 1
| Curing time(s) | Stability (moon) | |
| Example 1 | 83 | 8 |
| Example 2 | 85 | 7 |
| Example 3 | 96 | 6 |
| Example 4 | 88 | 7 |
Claims (4)
1. The melamine resin curing agent is characterized by comprising the following raw materials in percentage by mass: 10-26% of alkyl sulfonate, 14-22% of organic acid, 15-28% of inorganic acid, 4-11% of urea and the balance of alcohol amine;
the alkyl sulfonate is sodium dodecyl sulfonate;
the inorganic acid is sulfuric acid;
the alcohol amine is tertiary amine alcohol, the tertiary amine alcohol is a compound substance of triethanolamine and triisopropanolamine, and the mass ratio of the triethanolamine to the triisopropanolamine is 8:1.5;
the organic acid is the compound of p-toluenesulfonic acid and oxalic acid, and the mass ratio of the p-toluenesulfonic acid to the oxalic acid is 4:15.
2. The melamine resin curing agent according to claim 1, wherein the mass ratio of the inorganic acid to urea is (3-6): 1.
3. the melamine resin curing agent according to claim 1, wherein the raw materials comprise, in mass percent: 10-20% of alkyl sulfonate, 14-18% of organic acid, 20-28% of inorganic acid, 6-11% of urea and the balance of alcohol amine.
4. A method for producing the melamine resin curing agent according to any one of claims 1 to 3, characterized by comprising the steps of: adding alcohol amine into a reaction kettle, adding urea, adding inorganic acid, organic acid and alkyl sulfonate, and uniformly stirring to obtain the curing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111045285.7A CN115198556B (en) | 2021-09-07 | 2021-09-07 | Melamine resin curing agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111045285.7A CN115198556B (en) | 2021-09-07 | 2021-09-07 | Melamine resin curing agent and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN115198556A CN115198556A (en) | 2022-10-18 |
| CN115198556B true CN115198556B (en) | 2023-08-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202111045285.7A Active CN115198556B (en) | 2021-09-07 | 2021-09-07 | Melamine resin curing agent and preparation method thereof |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008009464A1 (en) * | 2006-07-21 | 2008-01-24 | Ami Agrolinz Melamine International Gmbh | Thermoplastically processable thermoset molding materials with improved property spectrum |
| CN102719209A (en) * | 2012-06-05 | 2012-10-10 | 滁州斯迈特复合材料有限公司 | Urea-formaldehyde glue latent curing agent for impregnated paper and preparation method thereof |
| JP2013006956A (en) * | 2011-06-24 | 2013-01-10 | Dic Corp | Amine-based curing agent, epoxy resin composition containing the amine-based curing agent, and cured product thereof |
| CN103225229A (en) * | 2013-04-07 | 2013-07-31 | 苏州市建诚装饰材料有限公司 | Preparation method of melamine resin curing agent |
| JP2014098105A (en) * | 2012-11-15 | 2014-05-29 | Mitsui Chemicals Inc | Ethylated melamine resin, method for producing the same, curing agent for coating, resin composition, coating film, and laminate |
| CN109642138A (en) * | 2016-07-27 | 2019-04-16 | 催化系统C.E.D.有限责任公司 | The hardening of bonding system |
| CN111592686A (en) * | 2020-06-01 | 2020-08-28 | 杭州临安迪恩化工有限公司 | Curing agent and melamine resin composition containing same |
| CN112029063A (en) * | 2020-09-07 | 2020-12-04 | 江苏湘园化工有限公司 | Liquid polyurethane curing agent composition and application method thereof |
-
2021
- 2021-09-07 CN CN202111045285.7A patent/CN115198556B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008009464A1 (en) * | 2006-07-21 | 2008-01-24 | Ami Agrolinz Melamine International Gmbh | Thermoplastically processable thermoset molding materials with improved property spectrum |
| JP2013006956A (en) * | 2011-06-24 | 2013-01-10 | Dic Corp | Amine-based curing agent, epoxy resin composition containing the amine-based curing agent, and cured product thereof |
| CN102719209A (en) * | 2012-06-05 | 2012-10-10 | 滁州斯迈特复合材料有限公司 | Urea-formaldehyde glue latent curing agent for impregnated paper and preparation method thereof |
| JP2014098105A (en) * | 2012-11-15 | 2014-05-29 | Mitsui Chemicals Inc | Ethylated melamine resin, method for producing the same, curing agent for coating, resin composition, coating film, and laminate |
| CN103225229A (en) * | 2013-04-07 | 2013-07-31 | 苏州市建诚装饰材料有限公司 | Preparation method of melamine resin curing agent |
| CN109642138A (en) * | 2016-07-27 | 2019-04-16 | 催化系统C.E.D.有限责任公司 | The hardening of bonding system |
| CN111592686A (en) * | 2020-06-01 | 2020-08-28 | 杭州临安迪恩化工有限公司 | Curing agent and melamine resin composition containing same |
| CN112029063A (en) * | 2020-09-07 | 2020-12-04 | 江苏湘园化工有限公司 | Liquid polyurethane curing agent composition and application method thereof |
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| CN115198556A (en) | 2022-10-18 |
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