Catalyst for synthesizing tirbutyl citrate and preparation method thereof
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A technology of tributyl citrate and catalyst, which is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of poor thermal stability of the carrier, easy loss of active components, and low conversion rate of raw materials. , to achieve the effect of not easy to lose and good reuse performance
Inactive Publication Date: 2011-04-06
JIANGSU QIANGLIN BIO ENERGY +1
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[0003] In order to solve the shortcomings in the prior art that the catalyst active components are easy to lose, the conversion rate of raw materials is low, and the thermal stability of the carrier
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Embodiment 1
[0027] The mesoporous support was prepared according to Example 26. Put 5 g of mesoporous carrier, 25 mL of silane coupling agent KH-5500, and 45 mL of toluene into the reactor, reflux for 12 hours, then suction filter, wash with ethanol, and dry at 105°C. The resulting product was reacted with 5 g of 1,3-propane sultone at 80°C for 3 hours, then suction filtered, washed with ethyl acetate, and dried at 105°C. React with 1g of sulfuric acid and 20mL of water at 80°C for 3h, rotary evaporate, and dry at 105°C to obtain the finished catalyst.
Embodiment 2
[0029] Put 5g of mesoporous carrier, 15mL of silane coupling agent KH-5500, and 30mL of toluene into the reactor, reflux for 10 hours, then suction filter, wash with ethanol, and dry at 105°C. The resulting product was reacted with 5 g of 1,3-propane sultone at 80°C for 3 hours, then suction filtered, washed with ethyl acetate, and dried at 105°C. React with 1g of sulfuric acid and 20mL of water at 80°C for 3h, rotary evaporate, and dry at 105°C to obtain the finished catalyst.
Embodiment 3
[0031] Put 5g of mesoporous carrier, 10mL of silane coupling agent KH-550, and 15mL of toluene into the reactor, reflux for 8 hours, then suction filter, wash with ethanol, and dry at 105°C. The resulting product was reacted with 5 g of 1,3-propane sultone at 80°C for 3 hours, then suction filtered, washed with ethyl acetate, and dried at 105°C. React with 1g of sulfuric acid and 20mL of water at 80°C for 3h, rotary evaporate, and dry at 105°C to obtain the finished catalyst.
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Abstract
The invention discloses a catalyst for synthesizing tirbutyl citrate and a preparation method thereof. in the preparation of the catalyst, a strong acid mesoporous material prepared by a hydrothermal synthesis method is used as a carrier, and strong acid ionic liquid is bonded on the mesoporous material carrier by chemical bonds, wherein the bonding mode of the acid ionic liquid adopts surface modification, the mesoporous material is any one of mesoporous silicon, mesoporous zirconium and mesoporous titanium, and the acid ionic liquid is ionic liquid containing phosphate radicals or sulfate radicals. The preparation method comprises the following steps of: preparing the mesoporous material carrier by utilizing precursors of the zirconium, the titanium or the silicon with hexadecyl trimethyl ammonium bromide by a conventional hydrothermal method; then carrying out surface modification with the acid ionic liquid: sufficiently reacting the mesoporous material carrier with a silane coupling agent KH-550 and methylbenzene and then reacting with 1,3-propane sultone or 1,4-butane sultone; and finally, reacting with ionic liquid containing strong acid groups to obtain the mesoporous material. After the catalyst is used, the conversion rate of citric acid is 90-99 percent.
Description
technical field [0001] The invention belongs to the field of preparation of tributyl citrate, and mainly relates to a catalyst for synthesizing tributyl citrate and a preparation method thereof. Background technique [0002] Tributyl citrate is an environmentally friendly plasticizer prepared from renewable resources. It can be used as a plasticizer for polyvinyl chloride (PVC), PVC-vinyl chloride copolymer, cellulose resin, etc., with good intersecting properties and plasticizing properties. High efficiency, mildew resistance and degradability. It can also be used as an additive for medicines, chemicals and food, as a hair growth promoter, and as a defoamer for protein solutions. Traditional methods use sulfuric acid and toluenesulfonic acid as catalysts, which cause serious equipment corrosion and environmental pollution. The patent (CN 1762969A) introduces a method for mesoporous materials to catalyze tributyl citrate. The HAl-MCM-41 mesoporous molecular sieve adopted i...
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