Process for making esters
A technology of esters and triglycerides, applied in the field of biodiesel, which can solve the problems of undesirable fine particle formation and pressure drop
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Embodiment 1
[0028] A 10 mL titanium silicate tablet was prepared according to the procedure of US-A-5 053 139, in particular according to its Example 9: by adding 569.11 g of TiCl 4 Add to enough deionized water to reach 2dm 3 , making 2dm 3 1.5M titanium chloride solution (Solution A). By adding 638.2g of Na 2 SiO 3.5 ·H 2 O is dissolved in sufficient 3M NaOH to reach 2dm 3 , making 2dm 3 1.5M sodium silicate solution (solution B). Solution B was added to solution A at a rate of 16 ml / min with very vigorous stirring. After the addition was complete, the mixture was allowed to continue mixing for an additional 15 minutes. The pH of the solution should fall between 7.5 and 7.9. Adjust pH with diluted HCl or diluted NaOH if necessary. Then, the samples were allowed to age for 2-4 days. After aging, any water on top of the gel was decanted off. Then filter the sample, every dm 3 1dm for gel 3 Wash with deionized water at 4-6dm 3 Reslurry in deionized water, filter and finally ...
Embodiment 2
[0031] 10 mL of titanium silicate tablets prepared according to the procedure of US-A-5 053 139 were loaded in a fixed bed reactor. The reactor was fed with MeOH (1.73 ml / h) and rapeseed oil (3.47 ml / h) containing 5 wt.% dodecanoic acid. After 284 hours on stream at 180°C, the reaction was stopped and the product stream and catalyst were analyzed. The product stream contains only trace amounts of titanium and silicon (several or tens of ppm (w / w)).
Embodiment 3
[0033] 10 mL titanium silicate tablets with different amounts of Na were prepared by treating the tablets prepared according to Example 1 with different amounts of HCl in water. The final Na content of the tablet can be controlled by controlling the pH of the aqueous phase. After 2 hours of HCl treatment, the tablets were washed thoroughly with demi-water and dried in an oven at 110° C. overnight. This process allowed the production of titanium silicate tablets with different Na contents, namely 6.0, 3.9, 3.2, 2.4 and 0.8 wt% Na, respectively.
[0034] Treated and untreated tablets were tested in a fixed bed reactor under similar conditions as described in Example 2. figure 1 The relationship between the amount of Na in the catalyst (wt.%) versus the amount of Si (ppm) and Ti in the product stream (XRF peak height) is shown (see figure 1 , respectively, the square line and the rhombus line). When measuring the amount of titanium and silicon in the final product by XRF (X-Ra...
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