CN109897568B - Whitening-resistant curing agent for seam beautifying agent and preparation method thereof - Google Patents
Whitening-resistant curing agent for seam beautifying agent and preparation method thereof Download PDFInfo
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- CN109897568B CN109897568B CN201910179762.5A CN201910179762A CN109897568B CN 109897568 B CN109897568 B CN 109897568B CN 201910179762 A CN201910179762 A CN 201910179762A CN 109897568 B CN109897568 B CN 109897568B
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Abstract
The invention discloses a whitening-resistant curing agent for a seam beautifying agent, which is prepared by modifying m-xylylenediamine derivatives by benzyl alcohol, a phenol promoter, an auxiliary amine and a pre-reaction resin, wherein the m-xylylenediamine derivatives, the benzyl alcohol, the phenol promoter and the auxiliary amine are mixed in proportion, the pre-reaction resin is slowly dripped after the uniform stirring, the temperature is kept after the dripping of the pre-reaction resin is finished, and the temperature is reduced to room temperature after the complete reaction, so that the whitening-resistant curing agent is obtained. The whitening-resistant curing agent is prepared by modifying m-xylylenediamine derivatives, has excellent water resistance, can withstand long-term outdoor rainwater drenching without whitening and yellowing after being cured in a humid environment or constructed, and obviously improves the application effect of the seam beautifying agent.
Description
Technical Field
The invention relates to the technical field of seam beautifying agents, and particularly relates to a whitening-resistant curing agent for a seam beautifying agent and a preparation method thereof.
Background
The crack beautifying agent is epoxy resin adhesive, and has rich color, strong pollution resistance, easy construction, fast development in recent years and fast increase in market amount. Especially, in recent years, the heat of the household is not reduced. The common seam beautifying agent usually has a whitening phenomenon (the surface is partially or completely changed into white in the curing process) in a humid environment, a rainy weather or a coastal area, so that the original colorful color disappears. The whitening phenomenon seriously influences the use effect of the seam beautifying agent, greatly reduces the satisfaction degree of users and increases the construction disputes.
At present, the main scheme for solving the whitening problem on the main field is as follows: 1. adding water repellent agent, which is added phenolic compound. 2. The reaction speed is increased, and it is desired to reduce the whitening phenomenon by reducing the contact time with water. 3. The water resistance is improved by increasing the dosage of phenols. The common crack sealing agent curing agent contains phenolic compounds, such as nonyl phenol or dodecyl phenol, which has the dual effects of accelerating curing speed and resisting water.
The three existing anti-whitening methods have the following disadvantages: 1. the method of adding the water repellent agent only can locally relieve the whitening phenomenon, and the effect is not obvious. Because it does not participate in chemical reaction, the addition amount is limited, the price is higher, and the cost is increased. 2. The method for improving the reaction speed can shorten the operable time during construction, and the heat of the system is difficult to remove, so that the colloid is brittle, thereby affecting the application effect of the crack sealer. 3. Increasing the amount of phenols used results in a decrease in the yellowing resistance of the colloid and the use of phenols causes an increase in the toxicity of the colloid.
Therefore, research and development of a curing agent for a caulking agent having a good whitening resistance effect has been one of important research subjects in the field.
Disclosure of Invention
The invention aims to provide a whitening-resistant curing agent for a seam beautifying agent and a preparation method of the whitening-resistant curing agent, so as to solve the defects in the background technology.
The invention is realized by the following technical scheme:
a whitening-resistant curing agent for a seam beautifying agent is prepared by modifying m-xylylenediamine derivatives through benzyl alcohol, a phenol promoter, auxiliary amines and pre-reaction resin, wherein the m-xylylenediamine derivatives have the following structural general formula:
in the structural formula of the m-xylylenediamine derivative, R can be a functional group containing a phenyl group, and preferably, in the structural formula of the m-xylylenediamine derivative, R is selected from phenethyl (C)6H5CH2CH2-) methyl phenethyl (CH)3C6H5CH2CH2-) styrenated phenoxy.
The structural formula of the styrenated phenoxy group is shown as follows:
wherein n is 1-3.
More preferably, the m-xylylenediamine derivative is N- (3-aminomethyl) benzyl-2-phenylethane-1-amine (N- (3- (aminomethyl) benzyl) -2-phenylethane-1-amine) having the following structural formula:
the physical indexes are as follows:
further preferably, the phenolic accelerator is nonylphenol or dodecylphenol.
Further preferably, the auxiliary amine is at least one selected from alicyclic amines and polyether amines. The alicyclic amine includes but is not limited to IPDA, PACM, 1,3-BAC, the polyether amine includes but is not limited to D2000, D230, T403, and the auxiliary amine is mainly used for adjusting speed, flexibility and the like.
Further preferably, the pre-reaction resin is selected from at least one of bisphenol a type epoxy resin or polyfunctional ether compound, such as E51 type epoxy resin.
The invention also provides a preparation method of the whitening-resistant curing agent, which comprises the following steps:
mixing m-xylylenediamine derivatives, benzyl alcohol, a phenolic promoter and auxiliary amine in proportion, stirring uniformly, slowly dropwise adding pre-reaction resin, controlling the reaction temperature to be not higher than 80 ℃, preserving the temperature for 1-3 hours at 75-80 ℃ after the dropwise adding of the pre-reaction resin is finished, and cooling to room temperature to obtain the whitening-resistant curing agent.
As a preferred technical scheme, the dosage of each component is as follows:
the sum of the percentage contents of all the components is 100 percent.
The color (Gardner) of the whitening-resistant curing agent is less than 100, the viscosity (cps,25 ℃) is 2500-.
The whitening-resistant curing agent is prepared by modifying m-xylylenediamine derivatives, has excellent water resistance, can withstand long-term outdoor rainwater drenching without whitening and yellowing after being cured in a humid environment or constructed, and obviously improves the application effect of the seam beautifying agent.
Detailed Description
The invention is illustrated below by means of specific examples, without being restricted thereto.
Example 1
Adding benzyl alcohol, dodecylphenol, alicyclic amine PACM, polyetheramine T403 and m-xylylenediamine derivative into a reaction kettle with a stirrer in proportion at the rotating speed of 100-130 rpm. After stirring uniformly, the epoxy resin E51 resin is added dropwise. The dropping speed is controlled to be 1-2 KG/min, and the reaction temperature in the kettle is not higher than 80 ℃. And (3) after the dripping of the resin is finished, preserving the heat for 2 hours at the temperature of 75-80 ℃, cooling to room temperature, discharging and packaging to obtain the whitening-resistant curing agent.
The dosage of the components is as follows:
wherein the m-xylylenediamine derivative is N- (3-aminomethyl) benzyl-2-phenylethane-1-amine.
Example 2
Adding benzyl alcohol, dodecylphenol, alicyclic amine PACM, polyetheramine T403 and m-xylylenediamine derivative into a reaction kettle with a stirrer in proportion at the rotating speed of 100-130 rpm. After stirring uniformly, the epoxy resin E51 resin is added dropwise. The dropping speed is controlled to be 1-2 KG/min, and the reaction temperature in the kettle is not higher than 80 ℃. And (3) after the dripping of the resin is finished, preserving the heat for 2 hours at the temperature of 75-80 ℃, cooling to room temperature, discharging and packaging to obtain the whitening-resistant curing agent.
The dosage of the components is as follows:
wherein the m-xylylenediamine derivative is N- (3-aminomethyl) benzyl-2-p-tolylethane-1-amine.
Example 3
Adding benzyl alcohol, nonyl phenol, alicyclic amine IPDA, polyether amine D230 and m-xylylenediamine derivative into a reaction kettle with a stirrer in proportion at the rotating speed of 100-130 rpm. After stirring uniformly, the epoxy resin E51 resin is added dropwise. The dropping speed is controlled to be 1-2 KG/min, and the reaction temperature in the kettle is not higher than 80 ℃. And (3) after the dripping of the resin is finished, preserving the heat for 2 hours at the temperature of 75-80 ℃, cooling to room temperature, discharging and packaging to obtain the whitening-resistant curing agent.
The dosage of the components is as follows:
wherein the m-xylylenediamine derivative is N- (3-aminomethyl) benzyl-2-styrenated phenoxy-1-amine.
Application examples
Whitening-resistant seam beautifying agents (numbered as #1, #2 and #3 in sequence) are respectively prepared by using the whitening-resistant curing agents prepared in the examples 1 to 3, and the specific formula and the process are as follows:
material A
80 parts of E51 type epoxy resin,
10 portions of glycol,
10 parts of fumed silica.
Adding epoxy resin and diluent in proportion once in a stirring kettle with vacuum, stirring uniformly at low speed of 300rpm, increasing the rotating speed to about 800rpm, adding fumed silica (hydrophobic type, specific surface area of 200 square meters/gram) in batches, and dispersing at high speed. Stirring was continued for about 10 minutes after the fumed silica was completely dissolved. The rotation speed is reduced to about 400rpm, the vacuum is opened (the vacuum degree is minus 0.09MPa), and the vacuum defoamation is carried out for 1 hour.
And (6) discharging.
B material
Firstly adding a whitening-resistant curing agent and a toner in proportion into a vacuum stirring kettle, uniformly stirring at a low speed, then adding fumed silica (hydrophilic type, the specific surface area is 200 square meters per gram) in batches, increasing the rotating speed, dispersing at a high speed until the fumed silica is completely dissolved, decreasing the rotating speed, and finally adding a flow stopping agent. After the dispersion is uniform, vacuumizing and defoaming (vacuum degree is-0.1 MPa), finishing about 1 hour, and discharging.
And respectively filling the material A and the material B into 400ml double-tube rubber bottles by using a full-automatic or semi-automatic filling machine to obtain the whitening-resistant seam beautifying agent.
The whitening-resistant seam sealer and a comparative example (a commercially available common seam sealer without the whitening-resistant curing agent of the invention) are respectively tested for whitening under the following two working conditions:
1. placing the product outdoors for curing in rainy days;
2. placing in an indoor water tank, and continuously spraying water drops.
The test results were as follows:
the test result shows that the whitening-resistant curing agent is applied to the seam beautifying agent and has obvious whitening resistance.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The whitening-resistant curing agent for the seam beautifying agent is characterized by being prepared by modifying m-xylylenediamine derivatives through benzyl alcohol, a phenol promoter, an auxiliary amine and a pre-reaction resin, wherein the m-xylylenediamine derivatives have the following structural general formula:
r is selected from styrenated phenoxy.
2. The whitening-resistant curing agent for a caulking agent according to claim 1, wherein the phenolic accelerator is nonylphenol or dodecylphenol.
3. The whitening-resistant curing agent for a caulking agent according to claim 1, wherein the auxiliary amine is at least one selected from the group consisting of alicyclic amines and polyether amines.
4. The whitening-resistant curing agent for a caulking agent according to claim 1, wherein the pre-reaction resin is at least one selected from a bisphenol a type epoxy resin and a polyfunctional ether compound.
5. A process for producing the whitening-resistant curing agent for a cosmetic agent according to any one of claims 1 to 4, comprising the steps of:
mixing m-xylylenediamine derivatives, benzyl alcohol, a phenolic promoter and auxiliary amine in proportion, stirring uniformly, slowly dropwise adding pre-reaction resin, controlling the reaction temperature to be not higher than 80 ℃, preserving the temperature for 1-3 hours at 75-80 ℃ after the dropwise adding of the pre-reaction resin is finished, and cooling to room temperature to obtain the whitening-resistant curing agent.
6. The method of claim 5, wherein the components are used in the following amounts:
the sum of the percentage contents of all the components is 100 percent.
7. The method of claim 5, wherein the phenolic accelerator is nonylphenol or dodecylphenol, the auxiliary amine is at least one selected from alicyclic amines and polyetheramines, and the pre-reaction resin is at least one selected from bisphenol A type epoxy resins or polyfunctional ether compounds.
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| CN101338018B (en) * | 2007-07-06 | 2010-09-08 | 上海树脂厂有限公司 | Epoxy curing agent and method for preparing same |
| US8729213B2 (en) * | 2011-09-23 | 2014-05-20 | Air Products And Chemicals, Inc. | Benzylated polyamine curing agents |
| CN103554438B (en) * | 2013-10-12 | 2017-01-11 | 瑞奇化工（松滋）有限公司 | Preparation method of modified epoxy hardener for reducing bleaching |
| CN105622899A (en) * | 2016-03-16 | 2016-06-01 | 惠州市彩田化工实业有限公司 | Modified polyether amine curing agent and preparation method and application thereof |
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