Preparation method of low-migration di (2-ethylhexyl) terephthalate plasticizer
A technology of di-terephthalic acid and terephthalic acid, which is applied in the field of preparation of low-migration terephthalate diester plasticizers, can solve the problem of affecting the appearance and feel of PVC products, increasing the complexity of the processing process, and increasing the manufacturing cost and other issues, to achieve the effect of good processability, simplified production process and good compatibility
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[0039] The preparation method of low mobility terephthalate di(2-ethylhexyl) ester plasticizer of the present invention, comprises the following steps:
[0040] 1) Use terephthalic acid (PTA) or its derivative, 2-ethylhexanol (2-EH) and 911 alcohol mixture as raw materials, wherein the equivalent molar ratio of PTA, 2EH and 911 alcohol is 1:2.2 -3.8:0.029, based on the total weight of the reactants (PTA and 2-EH weight), take 23-35wt% of terephthalic acid or its derivatives, 65-77wt% of 2-EH alcohol and 0.0014wt% of 911 alcohol for addition;
[0041] 2) based on the total amount of di(2-ethylhexyl) terephthalate with low mobility, take 0.1-6wt% metal-containing catalyst or inorganic acid catalyst as an esterification catalyst to add;
[0042] 3) Under the reaction pressure of 5-1033 mbar and the reaction temperature of 200-250 ° C, preferably the reaction pressure of 15-950 mbar and the reaction temperature of 220-240 ° C, for step 1) terephthalic acid or its derivatives, 2 et...
Embodiment 1
[0067] According to the formula in Table 1, take 120 g of terephthalic acid (PTA), 310 g of 2EH alcohol, 0.168 g of 911 alcohol (diluted with 2-EH), and the amount of catalyst TIPT (tetraisopropyl titanate) added is 0.6 g, terephthalic acid, 2EH alcohol, 911 alcohol mixture and catalyst are simultaneously fed into a four-necked flask, the reaction temperature is 225 ° C under nitrogen, the reaction time is 6 hours, and the reaction pressure is 5-1033 mbar, which must be removed during the reaction process. When the water is reacted to an acid value of 1 mgKOH / g or less, neutralize it with an aqueous solution of an alkali metal oxyhydroxide until the acid value of the synthesis reaction mixture is less than 0.07 mgKOH / g, then perform distillation to reduce the alcohol content to 300 ppm or less, and then filter After purification, low-migration bis(2-ethylhexyl) terephthalate was obtained and used as a plasticizer.
[0068] The basic physical properties and processing propertie...
Embodiment 2
[0070] As in the preparation method of Example 1, according to the formula in Table 1, the 911 alcohol therein was changed to 2-PH (2-phenylphenol). Under the same process conditions, the esterified DOTP plasticizer was obtained.
[0071] The basic physical properties and processing properties of the prepared DOTP plasticizer ester compound, the test results are shown in Table 1, wherein, the hue: 12APHA, acid value: 0.06mgKOH / g, purity: 99.8%, migration rate: 3.01% (at 80PHR), Transparency: 89.5%, and plasticization coefficient: 1.05.
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