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Method for preparing 1,4-butanediol

A technology of butanediol and diacetoxybutene is applied in the field of preparing 1,4-butanediol and can solve the problems of low yield and selectivity of 4-butanediol

Active Publication Date: 2018-03-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is the problem of low yield and selectivity of 1,4-butanediol, and a new method for preparing 1,4-butanediol is provided, which has 1,4-butanediol Features of high alcohol yield and high selectivity

Method used

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  • Method for preparing 1,4-butanediol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Preparation of hydrogenation catalyst:

[0044] ① Ammonium chloroplatinite ((NH 4 ) 2 PtCl 4 ) is dissolved in the hydrochloric acid aqueous solution that concentration is 8wt%, obtains impregnation solution 200ml, and 1L diameter 3mm, length 2cm, pore volume are 0.80cm 3 / g, the specific surface area is 1200cm 2 The coal-based cylindrical activated carbon carrier of / g is impregnated in the above-mentioned impregnating liquid, obtains catalyst precursor I;

[0045] ② Standing and aging for 24 hours to obtain catalyst precursor II;

[0046] ③ with a concentration of 8% (in N 2 h 4 ·H 2 The 500ml hydrazine hydrate of (2 weight ratio) reduces catalyst precursor II for 3h, obtains catalyst precursor III;

[0047] ④ washed with water to no chloride ion, dried at 50°C for 4 hours to obtain catalyst precursor IV;

[0048] ⑤Stannous nitrate (Sn(NO) containing 1.85g Sn 3 ) 2 ) 180ml of aqueous solution was impregnated on the catalyst precursor IV, and dried at 110° C...

Embodiment 2

[0054] Preparation of hydrogenation catalyst:

[0055] ① Ammonium chloroplatinite ((NH 4 ) 2 PtCl 4 ) is dissolved in the hydrochloric acid aqueous solution that concentration is 8wt%, obtains impregnation solution 200ml, and 1L diameter 3mm, length 2cm, pore volume are 0.80cm 3 / g, the specific surface area is 1200cm 2 The coal-based cylindrical activated carbon carrier of / g is impregnated in the above-mentioned impregnating liquid, obtains catalyst precursor I;

[0056] ② Standing and aging for 24 hours to obtain catalyst precursor II;

[0057] ③ with a concentration of 8% (in N 2 h 4 ·H 2 The 500ml hydrazine hydrate of (2 weight ratio) reduces catalyst precursor II for 3h, obtains catalyst precursor III;

[0058] ④ washed with water to no chloride ion, dried at 50°C for 4 hours to obtain catalyst precursor IV;

[0059] ⑤ Ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) 180ml of aqueous solution was impregnated on the catalyst precursor IV, and dried at 110° C....

Embodiment 3

[0089] Preparation of hydrogenation catalyst:

[0090] ① Ammonium chloroplatinite ((NH 4 ) 2 PtCl 4 ) is dissolved in the hydrochloric acid aqueous solution that concentration is 8wt%, obtains impregnation solution 200ml, and 1L diameter 3mm, length 2cm, pore volume are 0.80cm 3 / g, the specific surface area is 1200cm 2 The coal-based cylindrical activated carbon carrier of / g is impregnated in the above-mentioned impregnating liquid, obtains catalyst precursor I;

[0091] ② Standing and aging for 24 hours to obtain catalyst precursor II;

[0092] ③ with a concentration of 8% (in N 2 h 4 ·H 2 The 500ml hydrazine hydrate of (2 weight ratio) reduces catalyst precursor II for 3h, obtains catalyst precursor III;

[0093] ④ washed with water to no chloride ion, dried at 50°C for 4 hours to obtain catalyst precursor IV;

[0094] ⑤ Chromium acetate (Cr(OAc) containing 1.85g Cr 3 ·6H 2 O) Dissolved in hot water to obtain 180 ml of impregnating solution, impregnated on the c...

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Abstract

The invention relates to a method for preparing 1,4-butanediol, and mainly solves the problems that in the prior art, the yield and the selectivity are poor after 1,4-diacetoxy butylene hydrogenation,so that the yield and the selectivity of the 1,4-butanediol are low after 1,4-diacetoxy butane is hydrolyzed. The method for preparing the 1,4-butanediol comprises the following steps that acetoxylation reaction is performed by using butadiene, acetic acid and oxygen as raw materials under the existence of an acetoxylation catalyst to obtain the 1,4-diacetoxy butylene; under the existence of a hydrogenation catalyst, hydrogen gas and the 1,4-diacetoxy butylene react to obtain the 1,4-diacetoxy butane; the 1,4-diacetoxy butane is hydrolyzed to obtain the 1,4-butanediol, wherein the hydrogenation catalyst uses active carbon as a carrier; active ingredients include a Pt element and cocatalyst elements; the cocatalyst elements include at least one metal element selected from IVA group metal and VIB group metal.

Description

technical field [0001] The present invention relates to a process for the preparation of 1,4-butanediol. Background technique [0002] 1,4-Butanediol (1,4-BDO) is an important organic and fine chemical raw material, which is widely used in the fields of medicine, chemical industry, textile, papermaking, automobile and daily chemical industry. It can derive a series of high value-added fine chemical products. For example, tetrahydrofuran (THF), polybutylene terephthalate (PBT), γ-butyrolactone (GBL) and polyurethane resin (PU Resin) can be produced from 1,4-BDO, especially as the production of PBT engineering The basic raw material of plastic and PBT fiber has received extensive attention from research institutions. [0003] There are many process routes for the preparation of 1,4-butanediol. From the raw materials used, there are acetylene, ethylene, propylene, butadiene and maleic anhydride and other raw material routes. The same raw materials also have different synthesi...

Claims

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Application Information

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IPC IPC(8): C07C27/02B01J23/62B01J23/652B01J31/04B01J31/26B01J31/34C07C29/09C07C31/20
Inventor 查晓钟杨运信
Owner CHINA PETROLEUM & CHEM CORP
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