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Molecular sieve modified catalyst, preparation method and application thereof to preparation of acrylic ester

A molecular sieve and catalyst technology, applied in the field of molecular sieve modified catalyst and its preparation, can solve problems such as no major breakthrough, and achieve the effects of promoting reaction activity, increasing specific surface area, improving conversion rate and selectivity

Active Publication Date: 2013-05-22
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above four patents use phosphate and sulfate as catalysts, the technical indicators are roughly similar, and there is no major breakthrough

Method used

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  • Molecular sieve modified catalyst, preparation method and application thereof to preparation of acrylic ester
  • Molecular sieve modified catalyst, preparation method and application thereof to preparation of acrylic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1 weighs 20g of NaX (Si / Al=10), 0.82g Ca (NO 3 ) 2 , into a round bottom flask, dissolved in deionized water.

[0028] Step 2 Stir the material in step 1 for 6 hours at 80° C. in a water bath, and soak for 4 hours.

[0029] In step 3, the catalyst prepared in step 2 is suction-filtered and washed, and no nitrate ions are detected.

[0030]Step 4 Put the filter cake in step 3 in an oven to dry at 120°C until there is no free water, roast at 300°C for 4 hours, press into tablets, grind to get 18-35 mesh catalyst, put it in a desiccator for use.

[0031] Step 5: Use the catalyst prepared in step 4 to prepare acrylic acid and its butyl ester by dehydrating butyl lactate. Specific reaction conditions: temperature 300°C, normal pressure, space velocity 1h -1 , n (methanol): n (butyl lactate)=0.5, experimental results: the conversion rate of butyl lactate reaches 92.1%, and the molar selectivity of acrylic acid and its butyl ester reaches 60.5%.

Embodiment 2

[0033] Step 1 weighs quantitative 20gNaX (Si / Al=15), 0.47gLa (NO 3 ) 3 , into a round bottom flask, dissolved in deionized water.

[0034] Steps 2-3: Same as Steps 2-3 in Example 1.

[0035] Step 4 Put the filter cake in step 3 in an oven to dry at 120°C until there is no free water, roast at 350°C for 4 hours, press into tablets, grind to get a 18-35 mesh catalyst, put it in a desiccator for use.

[0036] Step 5 The catalyst prepared in step 4 is used for the reaction of dehydrating butyl lactate to prepare acrylic acid and its butyl ester. The specific reaction conditions are: temperature 320°C, normal pressure, space velocity 1h -1 , n (methanol): n (butyl lactate)=0.5, experimental results: the conversion rate of butyl lactate reaches 93.2%, and the molar selectivity of acrylic acid and its butyl ester reaches 61.4%.

Embodiment 3

[0038] Step 1: Weigh quantitative 20gNaY (Si / Al=20), 1.04gKNO 3 , into a round bottom flask, dissolved in deionized water.

[0039] Steps 2-3: Same as Steps 2-3 in Example 1.

[0040] Step 4 Put the filter cake in step 3 in an oven to dry at 120°C until there is no free water, bake at 350°C for 5 hours, press into tablets, grind to get 18-35 mesh catalyst, put it in a desiccator for later use.

[0041] Step 5: The catalyst prepared in step 4 is used for the reaction of dehydrating butyl lactate to prepare acrylic acid and its butyl ester. Specific reaction conditions: temperature 340°C, normal pressure, space velocity 2h -1 , n (methanol): n (butyl lactate)=1, experimental results: the conversion rate of butyl lactate reaches 92.8%, and the molar selectivity of acrylic acid and its butyl ester reaches 63.5%.

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PUM

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Abstract

The invention relates to a molecular sieve modified catalyst and a preparation method. The catalyst comprises a main catalyst A and an auxiliary catalyst B, wherein the main catalyst A comprises X-type, Y-type, ZSM-6type and ZSM-8-type molecular sieves, and the auxiliary catalyst B comprises nitrates of Ca (NO3)2, La (NO3)3, KNO3, Cu(NO3)2 and Co(NO3)2; the mass ratio of metal ions in the catalyst B to the catalyst A is 1%-5%. The preparation method comprises the following steps: weighting quantitative components A and B; adding a certain amount of deionized water; acutely stirring in a waterbath at 80 DEG C for 6h; soaking for 4h; drying a filter cake in an oven at 120 DEG C until free water is dried; baking the dried catalysts in a muffle furnace at 200-600 DEG C for 4-8h; and tabletting, grinding and sieving the cooled catalysts on a standard sieve to obtain a catalyst of 18-35 meshes. The method for preparing acrylic ester by catalyzing butyl lactate and methanol with the catalysts is carried out under the conditions that the mol ratio of raw materials is 0.5: (1-4):1, the temperature is 300-400 DEG C, the reaction pressure is normal pressure, and the airspeed is 1-4h-1. The specific surface area of the catalyst is increased by load metal ions, and the amplification of pore volumes is beneficial to the operation of the reaction.

Description

technical field [0001] The invention relates to a molecular sieve modified catalyst, a preparation method thereof, and a method in which the catalyst is used to catalyze the dehydration of butyl lactate to prepare acrylate. Background technique [0002] Acrylic acid and its butyl ester are important chemical raw materials, and are widely used in coatings, paints, adhesives, synthetic rubber, plastics, and water-absorbing resins. The currently dominant process is the propylene oxidation method, which is currently used in 90% of the operating units. Propylene Oxidation Method: Petroleum cracking product propylene is used as raw material, and the process is divided into two steps: the first step is to oxidize propylene to acrolein; the second step is to further oxidize acrolein to acrylic acid. The main patented technologies are: 1) Sohio method, the catalyst is Mo-Bi, Mo-V series, the yield is 80%; 2) Japanese catalyst method, the catalyst is Mo-Bi-Co Mo-V-Cu, the yield is 8...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/70B01J29/08B01J29/40C07C69/54C07C67/327C07C57/04C07C51/00
Inventor 张跃严生虎刘建武沈介发
Owner 溧阳常大技术转移中心有限公司
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