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A kind of preparation method of 3-methyl-1,3-butanediol

A technology of butanediol and methyl, applied in the field of preparation of 3-methyl-1,3-butanediol, can solve the problems of difficult separation of products and catalysts, difficulty in recycling and the like, and achieves controllable and easy operation of the reaction process , the effect of simple reaction process and simple separation process

Active Publication Date: 2021-06-01
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Except some homogeneous inorganic acids such as phosphoric acid (RU2330007), sulfuric acid, and acidic ionic liquid (CN101665409-A) can catalyze this process, but such catalysts are not easy to recycle, and it is difficult to separate the product from the catalyst

Method used

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  • A kind of preparation method of 3-methyl-1,3-butanediol
  • A kind of preparation method of 3-methyl-1,3-butanediol
  • A kind of preparation method of 3-methyl-1,3-butanediol

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Experimental program
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Embodiment 1

[0039] Dissolve cerium nitrate and praseodymium nitrate in water at a molar ratio of 99:1 to obtain an aqueous solution of cerium nitrate and praseodymium nitrate. The sum of the concentrations of the two metal ions in the aqueous solution is 1mol / L. Then, under stirring conditions, at 25°C, Add 38wt% ammonia water dropwise thereto, the molar ratio of ammonia water to the sum of the moles of the two metal ions is 10:1, then stand, separate, wash with water and ethanol, dry, and then roast at 300°C for 2h to obtain Pr Doped ceria catalyst (Pr doping amount 0.8wt%) is denoted as Pr-CeO 2 -99.

[0040] 2g of formaldehyde solution with a mass concentration of 38wt% was added to the autoclave, and 0.3g of the Pr-doped ceria prepared above was added, and the catalyst consumption was 0.01g (mmol HCHO) -1 , and then filled with 3g isobutene (the isobutene gas placed in the high-pressure bottle was filled into the autoclave at one time), and the isobutene accounted for 60wt% of the su...

Embodiment 2

[0042] Dissolve cerium nitrate and praseodymium nitrate in water at a molar ratio of 49:1 to obtain an aqueous solution of cerium nitrate and praseodymium nitrate. The sum of the concentrations of the two metal ions in the aqueous solution is 0.1mol / L. Add sodium hydroxide to it, the molar ratio of sodium hydroxide to the sum of the moles of the two metal ions is 5:1, then let it stand, separate, wash with water and ethanol, dry, and then roast at 500 °C for 4h, Available Pr-doped ceria catalyst (Pr doping amount 1.6wt%), denoted as Pr-CeO 2 -49.

[0043] Add 1g of formaldehyde solution with a mass concentration of 38wt% and 1g of deionized water into the autoclave. At this time, the mass concentration of the formaldehyde solution is 19wt%. Add 0.3g of the Pr-doped ceria prepared above, and the catalyst consumption is 0.02 g (mmol HCHO) -1 , and then filled with 2g of isobutene (the isobutene gas placed in the high-pressure bottle was filled into the autoclave at one time), ...

Embodiment 3

[0045] Dissolve cerium nitrate and praseodymium nitrate in water at a molar ratio of 19:1 to obtain an aqueous solution of cerium nitrate and praseodymium nitrate. The concentration of the two metal ions in the aqueous solution is 0.05mol / L. Then, under stirring conditions, at 85°C, Add potassium hydroxide dropwise to it, the molar ratio of potassium hydroxide to metal ions is 3:1, then let stand, separate, wash with water and ethanol, dry, and then roast at 800°C for 8h to obtain Pr-doped dioxide The cerium catalyst (the doping amount of Pr is 4wt%) is denoted as Pr-CeO 2 -19.

[0046] 0.5g of formaldehyde solution with a mass concentration of 38wt% and 1.5g of deionized water were added to the autoclave. At this time, the mass concentration of the formaldehyde solution was 10wt%, and 0.75g of the above-mentioned prepared Pr-doped ceria was added. 0.1g (mmol HCHO) -1 , and then filled with 1g of isobutene (the isobutene gas placed in the high-pressure bottle was filled into...

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Abstract

The invention relates to a preparation method of 3-methyl-1,3-butanediol. In this method, isobutylene, formaldehyde aqueous solution and Pr-doped ceria catalyst are mixed, put into a pressure-resistant container and sealed, stirred and reacted, and 3-methyl-1,3-butane is prepared through Prins condensation and hydrolysis reaction. diol. The separation process of the product and the catalyst is simple, the catalyst can be recycled, the reaction process is simple, controllable and easy to operate, and the yield of 3-methyl-1,3-butanediol can reach up to 98%.

Description

technical field [0001] The invention relates to a preparation method of 3-methyl-1,3-butanediol, in particular to the preparation of 3-methyl-1,3-butanediol by catalyzing the reaction of isobutene and formaldehyde aqueous solution with Pr-doped ceria. Background technique [0002] 3-Methyl-1,3-butanediol is an important pharmaceutical intermediate, chemical intermediate, and material intermediate, mainly used in the production of polymers and surfactants. For example, 3-methyl-1,3-butanediol can be dehydrated to prepare the monomer isoprene of synthetic rubber. Schneider et al. used p-nitrobenzenesulfonic acid catalyst to catalyze the selective hydroxylation of isoamyl alcohol to prepare 3-methyl-1,3-butanediol, but the yield was not as high as 5%. (Schneider, H.J.; Müller, W.Angew.Chem.1982,94,153-154.) FeMCM-41 can catalyze the reaction of isobutene and formaldehyde, but 3-methyl-1,3-butanediol is produced as a side reaction, and the yield is not Super 10%. (Yashima, T....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/38C07C31/20B01J23/10
CPCB01J23/10B01J37/03C07C29/38C07C31/20Y02P20/584
Inventor 王峰张志鑫王业红王敏张超锋侯婷婷安静华张健李利花
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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