Preparation method of modified molecular sieve catalyst and method for continuously synthesizing 3-methoxy-3-methyl butanol

A technology of molecular sieve and catalyst, which is applied in the synthesis field of 3-methoxy-3-methylbutanol, an important fine chemical raw material, can solve the problems of long reaction time, coking of catalyst, slow reaction rate, etc., and achieve the reduction of light components and high polymer formation, improved service life and stability, reliable and stable operability

Active Publication Date: 2021-03-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Regarding the preparation method of 3-methoxy-3-methylbutanol, CN102206142 adopts 3-methyl-3-butene-1-alcohol, methyl alcohol and heterogeneous catalyst to react in a closed reactor, and the reaction time is 1~ 12h, the reaction temperature is 50~200℃, the reaction pressure is 0.1~5MPa, and the heterogeneous catalyst is used in a closed reactor to obtain the highest yield of 95.2% of 3-methoxy-3-methylbutanol, but the reaction time needs 12h, and belongs to intermittent reaction; patent JP8176053 uses 4,4-dimethyl-1,3-dioxane to react with methanol under the catalysis of strong acid cationic resin, but 3-methoxy-3-methylbutanol is selected property ~ 40%, many by-products, and low atom economy; patent CN106966923A discloses a synthetic method for synthesizing 3-methoxy-N,N-dimethylpropionamide, which has a similar reaction and uses propylene Nitrile and anhydrous methanol are prepared in a closed reactor under the action of metal alkoxide, which is a batch reaction and does not have continuous operability
[0004] In summary, the currently disclosed technology uses 3-methyl-3-butene-1-alcohol as the technique for synthesizing 3-methoxyl-3-methylbutanol as a raw material, under high temperature and acidic catalyst conditions 3-Methyl-3-buten-1-ol is easy to generate too many low-boiling impurities, and at the same time, it is easy to cause coking and loss of the catalyst under high temperature conditions, which affects catalyst efficiency and life; while under low temperature conditions, the reaction rate is slow and the reaction long time problem
Moreover, the continuous operability is poor, and there is no technical advantage in terms of economy and industrial mass production.

Method used

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  • Preparation method of modified molecular sieve catalyst and method for continuously synthesizing 3-methoxy-3-methyl butanol
  • Preparation method of modified molecular sieve catalyst and method for continuously synthesizing 3-methoxy-3-methyl butanol

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Experimental program
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Effect test

Embodiment 1

[0037] Add 50g of bentonite to 116g of pure water and stir evenly to form slurry A; dissolve 30g of sodium tripolyphosphate in 90g of water and stir evenly to form solution B; add 400g of nano aluminum sol and 41.6g of solution B to slurry A, Stir for 1.5h to obtain uniformly mixed slurry C; add 750g of USY molecular sieve to slurry C, stir for 2h, put it in an oven at 80°C after stirring evenly, evaporate and remove excess water, and obtain a semi-finished catalyst ; The semi-finished catalyst was extruded into a spherical shape, washed with ethanol, sent to an oven for drying, and then transferred to a muffle furnace for calcination at 700°C for 3 hours to obtain the finished spherical catalyst CAT-1.

Embodiment 2

[0039] Add 60g of bentonite to 73.3g of pure water and stir evenly to form slurry A; dissolve 40g of sodium hexametaphosphate in 74.3g of water and stir evenly to form solution B; add 373.3g of nano aluminum sol and 26.7g of Solution B, stirred for 2 hours to obtain uniformly mixed slurry C; add 799.5g of NaY molecular sieve to slurry C, stirred for 2.5 hours, put it into an oven at 85°C after stirring, and evaporated the excess water , to obtain a semi-finished catalyst; the semi-finished catalyst was extruded into a spherical shape, washed with ethanol, sent to an oven for drying, and then transferred to a muffle furnace for calcination at 650°C for 2.5 hours to obtain a finished spherical catalyst CAT-2.

Embodiment 3

[0041]Add 45g of bentonite to 36.82g of pure water and stir evenly to form slurry A; dissolve 52g of disodium dihydrogen pyrophosphate in 63.6g of water and stir evenly to form solution B; add 210g of nano aluminum sol and 11.68 g solution B, stirred for 1.2h to obtain uniformly mixed slurry C; added 575.7g of 5A molecular sieve to slurry C, stirred for 2.2h, put it in an oven at 85°C after stirring evenly, and evaporated the excess water Removed to obtain a semi-finished catalyst; the semi-finished catalyst was extruded into a spherical shape, washed with ethanol, dried in an oven, and then transferred to a muffle furnace for 3.5 hours at 680°C to obtain a finished spherical catalyst CAT-3.

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Abstract

The invention provides preparation of a modified molecular sieve catalyst. The modified molecular sieve catalyst is a polyphosphate modified molecular sieve catalyst, bentonite is added into the molecular sieve catalyst, so that the catalyst changes acid site distribution and pore channel structure, and the modified molecular sieve prepared by the invention is used as a catalyst to prepare 3-methoxy-3-methyl butanol. The method overcomes the defects of many side reactions and short service life of the catalyst under the high temperature condition in the process of continuously preparing 3-methoxy-3-methyl butanol by taking 3-methyl-3-butylene-1-alcohol and methanol as raw materials, the conversion rate and selectivity of 3-methyl-3-butylene-1-alcohol are improved, and the yield of 3-methoxy-3-methyl butanol reaches 97% or above. The method has the advantages of high continuous operability, low cost and simple process.

Description

technical field [0001] The invention relates to a method for synthesizing 3-methoxy-3-methylbutanol, an important fine chemical raw material, and belongs to the technical field of organic chemical synthesis. Background technique [0002] 3-Methoxy-3-methylbutanol has good hydrophilicity, lipophilicity, low toxicity and biodegradability, and is widely used in cosmetics, printer inks, air fresheners, detergents, pesticides and insecticides It is an important fine chemical raw material. [0003] Regarding the preparation method of 3-methoxy-3-methylbutanol, CN102206142 adopts 3-methyl-3-butene-1-alcohol, methyl alcohol and heterogeneous catalyst to react in a closed reactor, and the reaction time is 1~ 12h, the reaction temperature is 50~200℃, the reaction pressure is 0.1~5MPa, and the heterogeneous catalyst is used in a closed reactor to obtain the highest yield of 95.2% of 3-methoxy-3-methylbutanol, but the reaction time needs 12h, and belongs to intermittent reaction; pate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/08B01J29/70B01J35/08B01J37/00B01J37/08C07C41/06C07C43/13
CPCB01J29/084B01J29/7003B01J29/088B01J37/0009B01J37/08C07C41/06B01J2229/186B01J35/51C07C43/13
Inventor 庞计昌刘英俊张红涛朱小瑞杨在刚张永振黎源
Owner WANHUA CHEM GRP CO LTD
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