The invention belongs to a preparation method of tripropylene glycol diacrylate,(TPGDA Monomer) comprising the following steps:
(1) Putting tripropylene glycol, acrylic acid, catalyst, and solvent and polymerization inhibitor into a reaction kettle and fully mixing and stirring to form a mixed solution
(2) Open the steam valve of the reactor and slowly heat it to make the temperature at 70-90°C and maintain the reaction at this temperature for 20-40 minutes;
(3) Continue to heat up to 80-115°C and reflux for 3-5h, the reaction ends;
(4) Add soda ash aqueous solution and sodium chloride aqueous solution to the mixed solution, wash and get the upper organic phase;
(5) Remove the solvent from the upper organic phase;
(6) cool and filter to obtain the finished product. The process of the invention is simple, generates less by-products and waste water, has better activity and flexibility, lower chroma, acidity, viscosity and shrinkage rate, high yield and good quality.
Table of Contents
Description:
The preparation method of tripropylene glycol diacrylate
Technical field:
The invention belongs to the field of diluents, in particular to a preparation method of tripropylene glycol diacrylate.
Background technique:
Tripropylene glycol diacrylate (TPGDA Monomer) is a bifunctional functional monomer with a molecular formula of C15H2406 and a molecular weight of 300. It is easily soluble in organic solvents such as low-carbon alcohols and aromatic hydrocarbons, but insoluble in water. Its appearance is generally colorless or Light yellow transparent oily liquid, the tripropylene glycol diacrylate is used as a reactive diluent in the radiation crosslinking of UV and EB. Stability and strong wear and corrosion resistance. Existing production method is to adopt alkyd esterification method, with acrylic acid excess, toluene or benzene are water-carrying solvent, and sulfuric acid is catalyzer to obtain final product, but there are following deficiencies: 1. the by-product and waste water of generation are many, to The environmental pollution is serious; 2. The activity and flexibility are poor; 3. The color, acidity and viscosity are high, and it is easy to be turbid; 4. The shrinkage rate is high, the yield is low, and the quality is poor.
SUMMARY
The object of the present invention is to overcome the deficiencies of the prior art, provide a simple process, generate fewer by-products and waste water, better activity and flexibility, lower chromaticity, acidity, viscosity and shrinkage, and high yield, The preparation method of good quality tripropylene glycol diacrylate.
The present invention is achieved through the following technical solutions:
A preparation method of tripropylene glycol diacrylate, characterized in that: the steps of the preparation method are:
(1) 50-60 parts of tripropylene glycol, 40-50 parts of acrylic acid, 1-10 parts of catalyst, 40-60 parts of solvent and 50-800 ppm of polymerization inhibitor are put into the reaction kettle and fully mixed and stirred to form a mixed solution ;
(2) open the reaction kettle steam valve and heat slowly, control the heating speed and make its vapor pressure at 0.3-0.5Mpa, make temperature control at 70-90 ℃ within 1h and maintain 20-40 minute reaction at this temperature;
(3). Continue to heat the mixture until the temperature rises to 80-115. Backflow 3-5h during C, the reaction finishes;
(4) Add the soda ash aqueous solution that the concentration is 10% and the sodium chloride aqueous solution that the concentration is 20% in the mixed solution, wash 2-4 times and stand for stratification, and get the upper organic phase;
(5) . The upper organic phase is removed from the solvent, and its vacuum degree is controlled at greater than -0.09Mpa, and the temperature is controlled at 70-90 ° C;
(6). Cooling and pressure filtration to obtain tripropylene glycol diacrylate. Moreover, the catalyst is one of p-toluenesulfonic acid, methanesulfonic acid or silicic acid. Moreover, the solvent is one of toluene, benzene, n-hexane, cyclohexane, or a mixture of two or more.
