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Synthetic method of 3-methyl-3-buten-1-ol, catalyst and preparation method of catalyst

A synthesis method and catalyst technology, applied in the field of synthesis of 3-methyl-3-buten-1-ol, can solve the problems of high price of isoprene raw materials, unsuitability for industrial production, and high investment costs, and achieve Improve catalytic efficiency and selectivity, suitable acidity and high selectivity

Active Publication Date: 2018-04-20
SHANDONG YUHUANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN105541544A discloses a method for synthesizing MBOH with isoprene and hydrogen chloride as raw materials. Due to the existence of hydrogen chloride, this process route is highly corrosive to equipment, and the price of isoprene raw materials is relatively expensive, and the investment cost is obvious. Higher than isobutylene and paraformaldehyde methods, not suitable for industrial production

Method used

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preparation example Construction

[0031] The present invention also provides a method for synthesizing 3-methyl-3-butene-1-ol, comprising:

[0032] The paraformaldehyde and isobutylene are reacted under the catalysis of the above catalysts.

[0033] Specifically, the synthetic method includes:

[0034] S1. Mix the solvent and paraformaldehyde with the catalyst prepared by the present invention to obtain a first mixed solution.

[0035] Among them, the solvent is tert-butanol, methanol, ethanol, isopropanol or toluene, preferably isopropanol. For dissolving paraformaldehyde and isobutylene, the reaction becomes a homogeneous reaction.

[0036] Preferably, the mass ratio of the added amount of the solvent to the added amount of paraformaldehyde is 5-10:1.

[0037] Paraformaldehyde is paraformaldehyde with a degree of polymerization of 10-100 and a low degree of polymerization; wherein, 95wt%≤paraformaldehyde purity≤99wt%. The selectivity of the catalyst within this range is better.

[0038] S2. Mix the isob...

Embodiment 1

[0045] A synthetic method of 3-methyl-3-butene-1-ol, comprising:

[0046] In a 100 mL autoclave, 2.5 g of paraformaldehyde, 20 g of isopropanol, and 0.1 g of catalyst were weighed and sealed. After feeding nitrogen to remove the air in the kettle, 30 g of isobutene was fed. Under the conditions of 150°C and 6.8MPa, react for 3h, remove the remaining isobutene and catalyst, rectify, and collect 120-130°C fractions.

[0047] Wherein, the catalyst is prepared by the following method:

[0048] After calcining the phosphosilicate aluminum molecular sieve at 550 °C for 4 h, in NaH 2 PO 4 After the solution is immersed in a medium volume, it is aged for 5 hours, dried at 100 °C for 5 hours, and calcined at 200-550 °C for 4 hours.

[0049] Among them, the phosphorus-aluminum ratio of the phosphorus-silicon-aluminum molecular sieve is 1, the pore size of the phosphorus-silicon-aluminum molecular sieve is 0.4 nm, the average grain size of the phosphorus-silicon-aluminum molecular si...

Embodiment 2

[0052] A synthetic method of 3-methyl-3-butene-1-ol, comprising:

[0053] In a 100 mL autoclave, 2.5 g of paraformaldehyde, 20 g of isopropanol, and 0.1 g of catalyst were weighed and sealed. After feeding nitrogen to remove the air in the kettle, 30 g of isobutene was fed. Then react at 170°C and 7.4MPa for 3h, remove the remaining isobutene and catalyst, rectify, and collect 120-130°C fractions.

[0054] Wherein, the catalyst adopts the catalyst provided in Example 1. After the reaction, the yield of the obtained 3-methyl-3-buten-1-ol relative to formaldehyde was 85%, and the selectivity was 97%.

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Abstract

The invention relates to a synthetic method of 3-methyl-3-buten-1-ol, a catalyst and a preparation method of the catalyst, and relates to the technical field of catalyst synthesis. The preparation method of the catalyst for synthesis of 3-methyl-3-buten-1-ol includes the steps: baking a phosphorus-silicon-aluminum molecular sieve at the temperature of 300-600 DEG C for 3.5-5 h, carrying out equivalent-volume impregnation in an alkaline phosphate solution, then aging, drying, and baking. The preparation method is simple to operate and prone to industrialized production; the 3-methyl-3-buten-1-ol catalyst prepared by the method has good catalytic effect; when the catalyst is applied in the synthesis of 3-methyl-3-buten-1-ol, the yield of 3-methyl-3-buten-1-ol is effectively improved, the production efficiency is effectively improved and the preparation cost is reduced.

Description

technical field [0001] The invention relates to the technical field of catalyst synthesis, in particular to a synthesis method of 3-methyl-3-buten-1-ol, a catalyst and a preparation method thereof. Background technique [0002] 3-Methyl-3-buten-1-ol (MBOH) is a very important chemical intermediate, mainly used for the synthesis of high-efficiency and low-toxicity pesticides pyrethroids, polycarboxylate water reducer raw materials TPEG, vitamins E, vitamin A and fragrance products such as citral. Another use of MBOH is to produce the main intermediate of polycarboxylate water reducer raw material TPEG. The use of this high-performance cement water reducer in concrete production and construction can reduce water consumption by more than 30% and enhance the strength of concrete by 30%. % or more, and the amount of cement can be reduced accordingly. [0003] Patent US2335027A first disclosed the method of synthesizing MBOH from isobutene and formaldehyde. Brace N.0. (Journal ...

Claims

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Application Information

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IPC IPC(8): B01J29/84B01J35/10C07C29/44C07C33/025
CPCC07C29/44B01J29/84B01J2229/18B01J35/617B01J35/643B01J35/633C07C33/025
Inventor 赵存胜常俊丽景文侯红霞王建伟王胜伟
Owner SHANDONG YUHUANG CHEM CO LTD
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