CN111592686A - Curing agent and melamine resin composition containing same - Google Patents
Curing agent and melamine resin composition containing same Download PDFInfo
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- CN111592686A CN111592686A CN202010485214.8A CN202010485214A CN111592686A CN 111592686 A CN111592686 A CN 111592686A CN 202010485214 A CN202010485214 A CN 202010485214A CN 111592686 A CN111592686 A CN 111592686A
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- curing agent
- alcohol amine
- melamine resin
- acid
- resin composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of curing agents, and particularly provides a curing agent and a melamine resin composition containing the same. The invention provides a curing agent, which is prepared from at least alcohol amine, inorganic base and inorganic acid; the mass ratio of the alcohol amine to the inorganic base to the inorganic acid is (5-9): 1: 8.
Description
Technical Field
The invention relates to the technical field of curing agents, and particularly provides a curing agent and a melamine resin composition containing the same.
Background
At present, the quality of the melamine impregnated paper in China is uneven, the difference of the use level of the melamine resin curing agent is large, general enterprises only use the melamine resin curing agent which is simply prepared by the general enterprises, the curing agent has a curing effect on glue at a low temperature, the produced impregnated paper is cured too early, the latency is low, some high-end enterprises adopt the imported curing agent with slightly high latency, the effect is good, but the effect is not changed fundamentally, and meanwhile, the curing agent of a certain brand is imported, so that once the goods are out of stock or broken, the risk to the enterprise production is high.
With the development of society, the market demand of melamine impregnated paper is getting larger and higher, and therefore a latent curing agent with high curing activity and good stability at normal temperature needs to be researched to meet the market demand.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a curing agent, which is prepared from at least alcohol amine, inorganic base and inorganic acid; the mass ratio of the alcohol amine to the inorganic base to the inorganic acid is (5-9): 1: 8.
as a preferred technical solution of the present invention, the alcohol amine is an alkyl alcohol amine.
As a preferable technical scheme of the invention, the alkyl alcohol amine is selected from one or a combination of a plurality of monoalkyl alcohol amine, dialkyl alcohol amine and trialkyl alcohol amine.
As a preferable technical scheme of the invention, the mass ratio of the dialkyl alcohol amine to the trialkyl alcohol amine is (2-3): 1.
as a preferable technical scheme of the invention, the inorganic base is selected from one or a combination of more of ammonia water, lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium carbonate, calcium bicarbonate, sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate.
As a preferred technical scheme of the invention, the inorganic acid is selected from one or a combination of more of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid.
As a preferable technical scheme of the invention, the ammonia water is 20 wt% ammonia water solution.
The second aspect of the present invention provides a method for preparing a curing agent, which at least comprises the following steps: adding the components into a reaction kettle, and uniformly stirring to obtain the product.
The third aspect of the invention provides a melamine resin composition, and the preparation raw materials comprise a melamine resin prepolymer and the curing agent.
As a preferable technical scheme of the invention, the mass ratio of the melamine resin prepolymer to the curing agent is 100: (0.1-2).
Has the advantages that: the invention provides a curing agent and a melamine resin composition containing the same, wherein the curing agent is added with alcohol amine substances comprising dialkyl alcohol amine and trialkyl alcohol amine, inorganic acid and inorganic alkali with specific content, so that the curing agent has reaction inertia on functional groups in melamine resin at normal temperature, can perform rapid curing and crosslinking reaction with a melamine resin system under heating condition, and has better latency, long service life and high curing activity.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
In order to solve the above technical problems, a first aspect of the present invention provides a curing agent, which is prepared from at least alcohol amine, inorganic base and inorganic acid; the mass ratio of the alcohol amine to the inorganic base to the inorganic acid is (5-9): 1: 8.
in a preferred embodiment, the preparation raw materials at least comprise alcohol amine, inorganic base and inorganic acid; the mass ratio of the alcohol amine to the inorganic base to the inorganic acid is 7: 1: 8.
<alcohol amines>
The alcohol amine is alkyl alcohol amine.
In a preferred embodiment, the alkyl alcohol amine is selected from one or more of monoalkyl alcohol amine, dialkyl alcohol amine and trialkyl alcohol amine.
As specific examples of the monoalkyl alcohol amine, there are included, but not limited to, monomethyl ethanolamine, monoethyl ethanolamine, monopropyl ethanolamine, monobutyl ethanolamine, monomethyl propanolamine, monoethyl propanolamine, monopropyl propanolamine, monobutyl propanolamine, monomethyl butanolamine, monoethyl butanolamine, monopropyl butanolamine, monobutyl butanolamine.
Specific examples of the dialkanolamine include, but are not limited to, dimethylethanolamine, diethanolamine, diethylethanolamine, dipropylethanolamine, dibutylethanolamine, dimethylpropanolamine, diethylpropanolamine, dipropylpropanolamine, dibutylpropanolamine, dimethylbutanolamine, diethylbutanolamine, dipropylbutanolamine, dibutylbutanolamine.
Specific examples of the trialkylalkanolamine include, but are not limited to, trimethylethanolamine, triethanolamine, triethylethanolamine, tripropylethanolamine, tributylethanolamine, trimethylpropanolamine, triethylpropanolamine, tripropylpropanolamine, tributylpropanolamine, trimethylbutanolamine, triethylbutanolamine, tripropylbutanolamine, tributylbutanolamine.
In a preferred embodiment, the alcohol amine includes a dialkanol amine and a trialkyl alcohol amine.
In a more preferred embodiment, the mass ratio of the dialkanolamine to the trialkylalkanolamine is (2 to 3): 1; more preferably, the mass ratio of the dialkanolamine to the trialkylalkanolamine is 2.5: 1.
in a more preferred embodiment, the dialkanolamine is diethanolamine; the trialkyl alcohol amine is triethanolamine.
The diethanolamine and triethanolamine are commercially available and include, but are not limited to, those available from Jinan Guangyu chemical Co.
<Inorganic base>
The inorganic base is selected from one or a combination of more of ammonia water, lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium carbonate, calcium bicarbonate, sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate.
In a preferred embodiment, the inorganic base is ammonia.
In a more preferred embodiment, the aqueous ammonia is a 20 wt% aqueous ammonia solution.
The ammonia may be obtained from commercial sources including, but not limited to, Nantong Guangrong chemical Co.
<Inorganic acid>
The inorganic acid is selected from one or a combination of more of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid.
In a preferred embodiment, the mineral acid is hydrochloric acid.
The applicant finds that by adding an alcohol amine substance comprising dialkanol amine and trialkyl alcohol amine and further limiting the mass ratio of the dialkanol amine to the trialkyl alcohol amine to (2-3): the melamine resin curing agent can interact with inorganic base and inorganic acid in a system, has reaction inertia to functional groups in melamine resin in a normal temperature normal state, can perform rapid curing crosslinking reaction with the melamine resin system when being heated to 140 ℃, and has good latency, long service life and high curing activity.
In addition, when the inorganic base and the inorganic acid in the system are added too much or too little, the curing effect of the curing agent is influenced, and when the mass ratio of the alcohol amine to the inorganic base to the inorganic acid is controlled to be (5-9): 1: at 8, the system can keep better curing activity and latency with the melamine resin.
A second aspect of the present invention provides a method for preparing the curing agent, characterized by comprising at least the steps of: adding the components into a reaction kettle, and uniformly stirring to obtain the product.
In a preferred embodiment, the preparation method of the curing agent at least comprises the following steps: adding dialkyl hydramine into a reaction kettle, stirring, then sequentially adding trialkyl hydramine, ammonia water and hydrochloric acid, stirring, starting cooling water, cooling to room temperature, and discharging to obtain the catalyst.
The third aspect of the invention provides a melamine resin composition, which comprises a melamine resin prepolymer and the curing agent.
In a preferred embodiment, the mass ratio of the melamine resin prepolymer to the curing agent is 100: (0.1-2); preferably, the mass ratio of the melamine resin prepolymer to the curing agent is 100: 1.
the melamine resin prepolymer may be obtained from commercial sources including, but not limited to, from Kelida chemical trade, Inc., of Tianjin.
Examples
In order to better understand the above technical solutions, the following detailed descriptions will be provided with reference to specific embodiments. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention. In addition, the starting materials used are all commercially available, unless otherwise specified.
Example 1
The embodiment 1 of the invention provides a curing agent, which is prepared from the following raw materials: alcohol amine, inorganic base and inorganic acid; the mass ratio of the alcohol amine to the inorganic base to the inorganic acid is 7: 1: 8.
the alcohol amine is dialkyl alcohol amine and trialkyl alcohol amine; the mass ratio of the dialkyl alcohol amine to the trialkyl alcohol amine is 2.5: 1; the dialkanolamine is diethanolamine; the trialkyl alcohol amine is triethanolamine.
The diethanolamine and triethanolamine are purchased from Jinan Guangyu chemical Co.
The inorganic base is ammonia water, and is purchased from Nantong Guangrong chemical Co.
The inorganic acid is hydrochloric acid.
The preparation steps of the curing agent are as follows: adding dialkyl hydramine into a reaction kettle, stirring, then sequentially adding trialkyl hydramine, ammonia water and hydrochloric acid, stirring, starting cooling water, cooling to room temperature, and discharging to obtain the catalyst.
Comparative example 1
Comparative example 1 of the present invention provides a curing agent, which is the same as example 1 except that the ratio of alkyl alcohol amine to trialkyl alcohol amine by mass is 5: 1.
comparative example 2
Comparative example 2 of the present invention provides a curing agent, which is similar to example 1 except that diethanolamine is not present.
Comparative example 3
Comparative example 3 of the present invention provides a curing agent, which is the same as example 1 except that triethanolamine is not included.
Comparative example 4
Comparative example 4 of the present invention provides a curing agent, which is the same as example 1 in the embodiment except that the mass ratio of the alcohol amine, the inorganic base and the inorganic acid is 7: 3: 8.
comparative example 5
Comparative example 5 of the present invention provides a curing agent, which is the same as example 1 in the embodiment except that the mass ratio of the alcohol amine, the inorganic base and the inorganic acid is 7: 1: 13.
performance testing
1. Curing time test
The curing agents and the melamine resin prepolymers prepared in the examples and the comparative examples are uniformly stirred at room temperature to obtain a melamine resin composition (the mass ratio of the melamine resin prepolymer to the curing agent is 100: 1), the melamine resin composition is placed into a test tube, the test tube is sealed and placed in a constant-temperature water bath at 140 ℃, and the time required for curing the melamine resin composition is recorded (the end point is that the melamine resin composition is completely whitened and cured in the test tube), and the melamine resin prepolymer is purchased from Kalimada chemical trade company of Tianjin. Each set of experiments was tested in parallel three times, and finally the mean value, unit: and s.
2. Latent curability test
The curing agents and the melamine resin prepolymers prepared in the examples and the comparative examples are uniformly stirred at room temperature to obtain a melamine resin composition (the mass ratio of the melamine resin prepolymer to the curing agent is 100: 1), the melamine resin composition is put into a test tube, the test tube is sealed and stored at 20 ℃, the change condition of the melamine resin composition is observed every 2 hours, and the pot life (the time required from the addition of the curing agent to the solidification of the system) is recorded, wherein the unit is as follows: h.
TABLE 1
| Curing time(s) | Shelf life (h) | |
| Example 1 | 80 | ＞24 |
| Comparative example 1 | 90 | ＜20 |
| Comparative example 2 | 110 | ＜20 |
| Comparative example 3 | 115 | ＜20 |
| Comparative example 4 | 120 | ＜20 |
| Comparative example 5 | 125 | ＜20 |
The data show that the curing agent prepared by the invention has good latency, long working life and high curing activity when being applied to melamine resin.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The curing agent is characterized in that the preparation raw materials at least comprise alcohol amine, inorganic base and inorganic acid; the mass ratio of the alcohol amine to the inorganic base to the inorganic acid is (5-9): 1: 8.
2. the curing agent of claim 1, wherein the alcohol amine is an alkyl alcohol amine.
3. The curing agent according to claim 2, wherein the alkyl alcohol amine is selected from one or more of mono-alkyl alcohol amine, di-alkyl alcohol amine, tri-alkyl alcohol amine.
4. The curing agent according to claim 3, wherein the mass ratio of the dialkanolamine to the trialkanolamine is (2-3): 1.
5. the curing agent according to claim 1, wherein the inorganic base is selected from one or more of ammonia, lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium carbonate, calcium bicarbonate, sodium carbonate, sodium bicarbonate, potassium carbonate, and potassium bicarbonate.
6. The curing agent according to claim 1, wherein the inorganic acid is selected from one or more of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid.
7. The curing agent according to claim 5, wherein the ammonia is a 20 wt% ammonia solution.
8. A method for preparing the curing agent according to any one of claims 1 to 7, comprising at least the steps of: adding the components into a reaction kettle, and uniformly stirring to obtain the product.
9. A melamine resin composition, characterized in that the raw materials for preparation comprise a melamine resin prepolymer and the curing agent of any one of claims 1 to 7.
10. The melamine resin composition according to claim 9, wherein the mass ratio of the melamine resin prepolymer to the curing agent is 100: (0.1-2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010485214.8A CN111592686A (en) | 2020-06-01 | 2020-06-01 | Curing agent and melamine resin composition containing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010485214.8A CN111592686A (en) | 2020-06-01 | 2020-06-01 | Curing agent and melamine resin composition containing same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111592686A true CN111592686A (en) | 2020-08-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010485214.8A Withdrawn CN111592686A (en) | 2020-06-01 | 2020-06-01 | Curing agent and melamine resin composition containing same |
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| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115198556A (en) * | 2021-09-07 | 2022-10-18 | 杭州临安迪恩化工有限公司 | Melamine resin curing agent and preparation method thereof |
-
2020
- 2020-06-01 CN CN202010485214.8A patent/CN111592686A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115198556A (en) * | 2021-09-07 | 2022-10-18 | 杭州临安迪恩化工有限公司 | Melamine resin curing agent and preparation method thereof |
| CN115198556B (en) * | 2021-09-07 | 2023-08-29 | 杭州临安迪恩化工有限公司 | Melamine resin curing agent and preparation method thereof |
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Application publication date: 20200828 |