Background and overview[1]
DMP-30 is the abbreviation of 2,4,6-tris(dimethylaminomethyl)phenol. As a curing catalyst for thermosetting epoxy resin adhesives, it can greatly increase the reaction speed between the curing agent and the epoxy resin and reduce the The curing temperature does not affect the physical and chemical properties of the adhesive; compared with other curing agents, it has good catalytic effect and complete reaction, and is generally suitable for low-temperature, high-temperature resistant and low-molecular-weight rubber-modified epoxy adhesives and some special Adhesives for use and special processes. DMP-30 can also be used as a catalyst for isocyanate trimerization reaction, making the reaction proceed quickly, reaching the highest reaction temperature in a short time, and producing a final product with better performance. This catalyst forms a co-oxidant with the epoxy compound and is used for The trimerization reaction of isocyanate has good compatibility with isocyanate, low toxicity, stable storage, and low price. It has great development prospects to replace some more expensive catalysts to prepare high-resilience polyurethane products. DMP-30 pure product is a colorless liquid. Since it is a phenolic compound, it is easily oxidized, especially when heated, the color is more likely to become darker. During the production process, in order to control the moisture content, vacuum heating and dehydration are generally required. The product can easily turn yellow to yellow-brown. Currently, the DMP-30 produced in China is generally yellow to yellow-brown, with poor quality. It can only be used in low-end products of epoxy resin, and its application scope is limited.
Apply[2-4]
DMP‑30 is mainly used as an epoxy resin curing agent. It can be quickly cured at room temperature or low-temperature cured epoxy resin coating, and can be used for castings, seals, etc. DMP‑30 can be used alone as an epoxy resin curing agent. For bisphenol A epoxy resin with an epoxy equivalent of 185‑195, the dosage is 10%. It can also be mixed with other epoxy curing agents to promote curing and improve For curing rate, the dosage when used as an accelerator is 0.1%-3%; when used in epoxy resin-liquid polysulfide systems, the normal temperature curing dosage is 10%-15%, and the heating curing dosage is 6%. Overall, DMP‑30 can impart unique properties to bonding systems and sealing materials when used alone. When used as an accelerator, it can greatly reduce the curing temperature and improve curing efficiency. It has a wide range of uses in the field of epoxy resin adhesives. The ring-opening mechanism of the cured epoxy group is as follows: First, the N atom in DMP-30 contains a lone pair of electrons, and the nucleophilicity of its lone pair of electrons promotes the attack on the epoxy group. After the epoxy group is opened, The formed oxygen anions can further react with epoxy groups to achieve polymerization and curing of epoxy resin. See the following reaction process:
If there is research and development of an epoxy self-leveling epoxy resin curing agent, it is composed of 45~55 parts by weight of raw materials polyetheramine (D-230), 20~24 parts of nonylphenol, and DMP-301~9 Prepare by reacting 1 to 6 parts of epoxy resin, 1 to 4 parts of benzyl alcohol, and 1 to 7 parts of 2168 curing agent. Add nonylphenol, epoxy resin, and benzyl alcohol to the reactor, stir evenly, and set aside. Add D-230 and DMP-30 to another reactor and heat it to 60°C; then the flow from the front reactor is added dropwise to the rear reactor for reaction, and the dripping speed is controlled to maintain the reaction temperature at 60~70°C. Complete the dropwise addition within ~2h; continue the reaction at 60~70°C for 1h, cool down and discharge. It has light color, high gloss and low viscosity, and is particularly suitable as a curing agent for epoxy floor topcoats.
There is also research and development of an epoxy resin photoelastic model, using four raw materials: 618# epoxy resin, methylhexahydrophthalic anhydride, accelerator DMP-30, and epoxy resin defoaming agent to prepare a mixed liquid; When adding liquid, first pour the weighed methyl hexahydrophthalic anhydride and epoxy resin defoaming agent into the epoxy resin and start stirring. During the stirring process, use a rubber tip dropper to drip in the weighed DMP-30 drop by drop. Mixed liquid; pour the mixed liquid into the mold; after the pouring is completed, put the mold into the oven and heat it to solidify the mixed liquid; after the heating process is completed, take the mold out of the oven and remove the mold to get the molded model; The model is put into the oven for quenching to obtain the epoxy resin photoelastic model. The reaction process of the mixed liquid prepared by this formula is not violent, the curing time is short, the curing process is simple, the fading effect is good after the model is formed, the internal residual stress is small, the chemical raw materials used have low toxicity, no irritating smell, and almost no harm to the body .
Preparation[5]
The traditional production process of 2,4,6-tris(dimethylaminomethyl)phenol ((DMP-30)) uses 37% formaldehyde aqueous solution, dimethylamine aqueous solution and phenol to be synthesized through Mannich condensation reaction, but this synthesis The process has many shortcomings. The shortcomings are as follows: (1) The formaldehyde content in the formaldehyde aqueous solution is low (generally 37%), the transportation cost is high, and because it is in a solution state, it is not easy to transport, and it is easy to polymerize during storage. A white pasty precipitate precipitates; (2) Using formaldehyde aqueous solution as the formaldehyde source for organic synthesis reactions, because the reaction system contains a large amount of water, the mass transfer and heat transfer efficiency is low, and energy consumption increases; (3) Due to the condensation reaction, Water is generated, and a formaldehyde aqueous solution is used for the condensation reaction. The presence of a large amount of water in the reaction system is unfavorable for the condensation reaction; (4) The formaldehyde aqueous solution is used for the reaction. After the reaction, the water must be removed in a vacuum, which further increases energy consumption and produces A large amount of sewage causes environmental pollution. If the sewage is treated, it will increase production costs.
There is research and development of a method for synthesizing 2,4,6-tris(dimethylaminomethyl)phenol ((DMP-30)), which is characterized in that the method utilizes multipleThe target product is prepared by Mannich condensation reaction of polyformaldehyde with phenol and dimethylamine aqueous solution; wherein the weight percentage of phenol, dimethylamine aqueous solution and paraformaldehyde is 13.82% to 15.72%: 68.39% to 72.21%: 13.97% to 15.89% During the reaction, first mix the phenol and dimethylamine aqueous solutions evenly at a temperature of 0 to 70°C, add a measured amount of paraformaldehyde in batches within 0.5 to 1 hour, and allow the mixture to react at a temperature of 30 to 100°C for 1 ~4h, the material is discharged and subjected to oil-water separation and vacuum distillation to obtain the 2,4,6-tris(dimethylaminomethyl)phenol ((DMP-30)).
Main reference materials
[1] CN201610332431.7 Preparation method of colorless DMP-30
[2] CN201210064580.1 A DMP-30 sealing method and its application in epoxy adhesive
[3] CN201510683964.5 An epoxy resin photoelastic model and its production method
[4] CN201310179252.0 A solvent-free self-leveling epoxy resin curing agent and its preparation method
[5] CN201210241307.1 A method of synthesizing 2,4,6-tris(dimethylaminomethyl)phenol
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