Preparation method of synthetic 1,4-butynediol catalyst

The technology of butynediol and catalyst is applied in the field of preparation of catalyst for producing 1,4-butynediol, and can solve the problems of poor wear resistance and stability of catalyst, unsuitable particle size of catalyst, complicated preparation process of carrier and the like, To achieve the effect of easy separation, concentrated distribution and uniform catalyst particles

Inactive Publication Date: 2017-05-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In summary, the catalysts for producing 1,4-butynediol in the prior art generally have the following deficiencies: unsuitable catalyst particle size, poor wear resistance and stability of the catalyst, easy loss of active components and the use of carriers Technical problems such as complex preparation process and high cost

Method used

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  • Preparation method of synthetic 1,4-butynediol catalyst
  • Preparation method of synthetic 1,4-butynediol catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Weigh 96.64g Cu(NO 3 ) 2 .3H 2 O and 229.6g 30% silica sol, prepare 400ml copper-silicon mixed solution; Take by weighing 144.96g Cu(NO 3 ) 2 .3H 2 O and 10.24g Bi(NO 3 ) 3 .5H 2 O, prepare 600ml copper-bismuth mixed solution, adjust the pH of the solution to be 2 with nitric acid to fully dissolve the bismuth salt; prepare 3mol / L and 1mol / L Na 2 CO 3 The solution is ready for use.

[0035] (2) Heat 400ml of copper-silicon mixed solution prepared in step (1) to 60°C, add 3mol / L Na 2 CO 3 The solution was dropped into the copper-silicon mixed solution, the reaction temperature was controlled to be 60° C., and the pH at the end of the reaction was 6. After the reaction was completed, the reaction temperature and pH were maintained, and stirring was continued for 30 min.

[0036] (3) Add 600ml of the copper-bismuth mixed solution prepared in step (1) to the copper-silicon precipitate slurry obtained in step (2).

[0037] (4) The 1mol / L Na prepared in step ...

Embodiment 2

[0041] (1) Weigh 120.8g Cu(NO 3 ) 2 .3H 2 O and 348.8g 30% silica sol, prepare 500ml copper-silicon mixed solution; Take by weighing 120.8g Cu(NO 3 ) 2 .3H 2 O and 12.49g Bi(NO 3 ) 3 .5H 2 O, prepare 500ml copper-bismuth mixed solution, adjust the pH of the solution to be 2 with nitric acid to fully dissolve the bismuth salt; prepare 4mol / L NaOH solution and 1mol / L NaOH solution 2 CO 3 The solution is ready for use.

[0042] (2) Heat 500ml of the copper-silicon mixed solution prepared in step (1) to 65°C, drop 4mol / L NaOH solution into the copper-silicon mixed solution, control the reaction temperature to 65°C, and the pH at the end of the reaction to be 5.5. After the reaction was completed, the reaction temperature and pH were maintained, and stirring was continued for 30 min.

[0043] (3) Add 500ml of the copper-bismuth mixed solution prepared in step (1) to the copper-silicon precipitate slurry obtained in step (2).

[0044] (4) The 1mol / L Na prepared in step (1...

Embodiment 3

[0048] (1) Weigh 144.96g Cu(NO 3 ) 2 .3H 2 O and 304.7g 30% silica sol, prepare 600ml copper-silicon mixed solution; Take by weighing 96.64g Cu(NO 3 ) 2 .3H 2 O and 13.71g Bi(NO 3 ) 3 .5H 2 O, prepare 500ml of copper-bismuth mixed solution, adjust the pH of the solution to be 2 with nitric acid to fully dissolve the bismuth salt; prepare 4.4mol / L ammonia solution and 1.5mol / L Na 2 CO 3 The solution is ready for use.

[0049] (2) Heat 600ml of the copper-silicon mixed solution prepared in step (1) to 70°C, drop 4.4mol / L ammonia solution into the copper-silicon mixed solution, control the reaction temperature to 70°C, and the pH at the end of the reaction to be 5.5 . After the reaction was completed, the reaction temperature and pH were maintained, and stirring was continued for 30 min.

[0050] (3) Add 500ml of the copper-bismuth mixed solution prepared in step (1) to the copper-silicon precipitate slurry obtained in step (2).

[0051] (4) Add 1.5mol / L of Na prepare...

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Abstract

The invention discloses a preparation method of a synthetic 1,4-butynediol catalyst. The preparation method comprises the following preparation steps of (1) preparing a copper and silicon mixed solution, a copper and bismuth mixed solution, a precipitant solution I and a precipitant solution II; (2) dripping the precipitant solution I into the copper and silicon mixed solution, so as to obtain copper and silicon precipitate slurry; (3) adding the copper and bismuth mixed solution into the copper and silicon precipitate slurry, wherein the usage amount of copper is the left copper amount; (4) compared with a precipitation condition in step (2), under the condition of lowering the reaction temperature by 5 to 30 DEG C, dripping the copper and bismuth mixed solution containing the copper and silicon precipitate into the precipitant solution II; (5) filtering a material, and adding a proper amount of distilled water; (6) spraying and drying the slurry, and calcining, so as to obtain the catalyst for producing synthetic 1,4-butynediol. The preparation method has the advantages that the particles of the catalyst are uniform, and the loss possibility in a use process is small; the preparation method of the catalyst is simple, the implementing is easy, and the repeatability is good.

Description

technical field [0001] The invention relates to a preparation method for producing 1,4-butynediol catalyst, belonging to the technical field of chemical catalysts. Background technique [0002] 1,4-butynediol (BD) is an important organic chemical intermediate, and its hydrogenation product 1,4-butanediol (BDO) can be used to produce γ-butyrolactone (GBL), tetrahydrofuran ( THF), polybutylene diphthalate (PBT), etc. In recent years, due to the sudden increase in the demand for PBT and other derivatives, the demand for BDO in my country has increased significantly. In industry, the production of 1,4-butynediol is mainly formed by the combination of formaldehyde and acetylene produced in coal chemical industry. my country has abundant coal resources, which makes it possible to produce 1,4-butynediol with coal chemical route acetylene as raw material It has unique conditions and advantages. [0003] In the 1940s, Reppe invented the process of synthesizing 1,4-butynediol from f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/843C07C33/046C07C29/42
Inventor 关月明包洪洲王永林张艳侠袁胜华
Owner CHINA PETROLEUM & CHEM CORP
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