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Catalyst for preparing acrylic acid and butyl ester using lactic acid method and preparation method thereof
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A catalyst, acrylic technology
Active Publication Date: 2009-04-29
溧阳常大技术转移中心有限公司
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[0007] (1) The reaction temperature is higher at 300-500°C, the main reason is that the activation energy of the reaction is higher, and the reaction cannot be carried out under low temperature conditions;
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Embodiment 1
[0028] Step 1: Weigh a quantitative amount of CaSO 4 , CuSO 4 , NaH 2 PO 4 , La 2 O 3 , After being fully grinded in an agate mortar and transferred to a beaker, the molar ratio of raw materials: CaSO 4 :CuSO 4 :NaH 2 PO 4 :La 2 O 3 =50:1:1:3;
[0029] Step 2: Put H 3 PO 4 Dissolved in quantitative deionized water (the amount of deionized water is CaSO 4 , CuSO 4 , NaH 2 PO 4 , La 2 O 3 The total mass of ), add it to the beaker in step 1, mix and stir thoroughly, the molar ratio of raw materials: CaSO 4 :H 3 PO 4 =50:2;
[0030] Step 3: Dry the material in step 2 in an oven at 110°C until there is no free water, grind and pulverize, sieving with a standard sieve of 18 mesh and 35 mesh to obtain a catalyst of 18 to 35 mesh;
[0031] Step 4: Roast the catalyst prepared in step 3 at 450°C for 4 hours, and place it in a desiccator for use after cooling;
[0032] Step 5: The catalyst prepared in Step 4 is used in the reaction of butyl lactatedehydration to prepare acrylic acid and its...
Embodiment 2
[0034] Step 1: Weigh a quantitative amount of CaSO 4 , CuSO 4 , NaH 2 PO 4 , La 2 O 3 , After being fully grinded in an agate mortar and transferred to a beaker, the molar ratio of raw materials: CaSO 4 :CuSO 4 :NaH 2 PO 4 :La 2 O3 =50:3:1:3;
[0035] Step 2 to Step 4: Same as Step 2 to Step 4 in Example 1.
[0036] Step 5: The catalyst prepared in Step 4 is used in the reaction of butyl lactate dehydration to prepare acrylic acid and its butyl ester, the specific reaction conditions: temperature 400℃, pressure at normal pressure, space velocity 1.8h -1 , Adopt nitrogen protection, the feed volume ratio of nitrogen and butyl lactate is: V (nitrogen): V (raw material) = 40:1, the experimental result: the molar conversion rate of butyl lactate reaches 75.7%, acrylic acid and its butyl ester The molar selectivity is 70.5%.
Embodiment 3
[0038] Step 1: Weigh a quantitative amount of CaSO 4 , MgSO 4 , NaH 2 PO 4 , La 2 O 3 , After being fully grinded in an agate mortar and transferred to a beaker, the molar ratio of raw materials: CaSO 4 :MgSO 4 :NaH 2 PO 4 :La 2 O 3 =50:1:1:3;
[0039] Step 2 to Step 4: Same as Steps 2 to 4 in Example 1.
[0040] Step 5: The catalyst prepared in step 4 is used in the dehydration reaction of butyl lactate to prepare acrylic acid and its butyl ester. The specific reaction conditions are: temperature 400℃, pressure is normal pressure, and space velocity is 1.8h -1 , Using nitrogen protection, the feed volume ratio of nitrogen and butyl lactate is: V (nitrogen): V (raw material) = 40:1, experimental results: the molar conversion rate of butyl lactate reaches 69.1%, acrylic acid and its butyl ester The molar selectivity reached 65.1%.
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Abstract
The invention discloses a catalyst used for preparing acrylic acid and butyl ester by the dehydration of butyl lactate and a preparation method thereof. The catalyst is a composite catalyst, comprising a main catalyst A and auxiliary catalysts B, C, D and E, wherein, A is calcium sulphate, B is sulphuric acid, C is phosphate, D is alkaline matter and E is promoter. The preparation method comprises the steps as follows: five compositions A, B, C, D and E are sufficiently mixed, baked for 2-10 hours at the temperature of 200-800DEG C and formed for standby. The catalyst has high catalytic activation; under the catalysis of the catalyst, the molar yield reaches 75.1 percent and the molar selectivity of the acrylic acid and butyl ester reaches 71.5 percent. The preparation method has the advantages that the crystal structure of the main catalyst can be improved so as to be beneficial for carrying out the reaction; and the introduction of different auxiliary catalysts and quantities is helpful to improve the conversion ratio of the raw material and the product selectivity and is beneficial for improving the strength of the catalyst.
Description
Technical field [0001] The invention relates to the composition and preparation method of a catalyst for preparing acrylic acid by dehydration of butyl lactate and its butyl ester. Background technique [0002] Acrylic acid and its butyl ester are basic organic chemical raw materials, and they are used in huge amounts in coatings, paints, adhesives, synthetic rubber, plastics, and water-absorbent resins. The preparation processes of acrylic acid and its butyl ester mainly include: cyanoethanol method, improved Reppe method, acrylonitrilehydrolysis method, and propylene oxidation method. The dominant one is the propylene oxidation method, which is currently used in 90% of operating devices. [0003] The propylene oxidation method uses petroleum cracked product propylene as the raw material. The process is divided into two steps: the first step is to oxidize propylene to acrolein; in the second step, acrolein is further oxidized to acrylic acid. The raw material of the process com...
Claims
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