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Preparation method of low-mercury compound catalyst for producing vinyl chloride

A composite catalyst, vinyl chloride technology, applied in catalyst activation/preparation, chemical instruments and methods, hydrogen halide addition preparation, etc., can solve the problems of low mercury catalyst activity, stability and selectivity reduction, etc., to improve metal dispersion degree and active sites, improving activity and stability, reducing utilization and emissions

Active Publication Date: 2012-06-20
内蒙古海驰高科新材有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the manganese chloride solution used to impregnate the coal-based carbon has a high boiling point. After the manganese chloride is modified, the surface of the coal-based carbon carrier will evenly absorb manganese chloride, which changes the properties of the surface of the coal-based carbon carrier. , the result is that the activity, stability and selectivity of the prepared low-mercury catalyst are reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The first step, pretreatment of coal-based carbon carrier

[0028]At room temperature, soak 100g of coal-based carbon in 300mL of aqua regia and stir for 1 hour, then filter it with suction and wash the filter cake with deionized water until the pH value of the filtrate is 5, then bake the filter cake at 120°C Drying, the resulting dried filter cake was added to 300mL of 10% triethylamine aqueous solution at 120°C while refluxing and stirring for 3 hours, then it was suction filtered and the filter cake was dried at 120°C, Prepare the pretreated coal-based carbon carrier;

[0029] The second step is to prepare low-mercury composite catalyst

[0030] 2.1 Addition of surfactant cetyltrimethylammonium chloride

[0031] Weigh 2.85g cetyltrimethylammonium chloride and 4g HgCl respectively 2 , under the state of stirring in an ultrasonic water bath with a power of 80W at 50°C, add 2.85g of cetyltrimethylammonium chloride to 214g of deionized water, and then add 4g of HgCl ...

Embodiment 2

[0036] In addition to adopting an ultrasonic water bath with a power of 99W and cetyltrimethylammonium chloride by mass ratio: HgCl 2 =7.65:4 Weigh cetyltrimethylammonium chloride and HgCl respectively 2 Except, other is with embodiment 1, makes low mercury composite catalyst, in this low mercury composite catalyst, HgCl 2 The percentage of the total mass of the catalyst is 4%, NiCl 2 The percentage accounting for the overall mass of the catalyst is 4%, the percentage of cetyltrimethylammonium chloride accounting for the overall mass of the catalyst is 7.65%, and the rest is C. At 130°C and acetylene space velocity 80h -1 Under the evaluation conditions, the low-mercury composite catalyst prepared in this example has an acetylene conversion rate of 99.4% and a vinyl chloride selectivity of 99% in the acetylene hydrochlorination reaction.

Embodiment 3

[0038] The first step, pretreatment of coal-based carbon carrier

[0039] At room temperature, soak 100g of coal-based carbon in 300mL of aqua regia and stir for 1 hour, then filter it with suction and wash the filter cake with deionized water until the pH value of the filtrate is 6, then bake the filter cake at 120°C Drying, the resulting dried filter cake was added to 300mL of 10% triethylamine aqueous solution at 120°C and stirred for 3 hours at 120°C, then suction filtered and the filter cake was dried at 120°C to prepare Obtain the pretreated coal-based carbon carrier;

[0040] The second step is to prepare low-mercury composite catalyst

[0041] 2.1 Addition of surfactant cetyltrimethylammonium chloride

[0042] Weigh 5.25g cetyltrimethylammonium chloride and 5.25g HgCl respectively 2 , at 50°C with 90W ultrasonic water bath stirring, add 5.25g of cetyltrimethylammonium chloride to 205g of deionized water, then add 5.25g of HgCl 2 And after stirring for 30 minutes, t...

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Abstract

The invention discloses a preparation method of a low-mercury compound catalyst for producing vinyl chloride, which relates to the catalyst which contains metallic mercury and nickel, and comprises the steps that: firstly a coaly carbon carrier is soaked in aqua regia, and simultaneously flows back in the aqueous solution of triethylamine, is stirred and pre-treated; then surfactant hexadecyltrimethylammonium chloride and additive nickel chloride are added by the mass ratio that hexadecyltrimethylammonium chloride: HgCl2 is 2.85 to 7.65: 4 to 6.5 and NiCl2: HgC12 is 4:4 to 6.5, and impregnated in a vacuum rotary evaporation way, wherein the prepared HgCl2 accounts for 4 percent to 6.5 percent of the total mass of the catalyst and NiCl2 accounts for 4 percent of the total mass of the catalyst, the hexadecyltrimethylammonium chlorid accounts for 2.85 percent to 7.65 percent of the total mass of the catalyst, and the balance is the low-mercury compound catalyst of C, so that the activity, stability and selectivity of the low-mercury compound catalyst are also significantly improved while the mercury content is reduced.

Description

technical field [0001] The technical scheme of the invention relates to a catalyst containing metallic mercury and nickel, in particular to a preparation method for a low-mercury composite catalyst used in the production of vinyl chloride. Background technique [0002] The demand for vinyl chloride as a monomer of polyvinyl chloride is increasing day by day. So far, the main process for domestic production of vinyl chloride is acetylene hydrochlorination. Most of the catalysts used in this reaction are high-mercury catalysts supported by activated carbon, and the mass percentage of mercuric chloride is as high as 12%. The serious shortage of mercury resources in China today has made high-mercury catalysts to the point where there is no rice to cook. In addition, the international community's policies on mercury resources such as restrictions on mining and export restrictions have also made high-mercury catalysts face unprecedented difficulties. There are two ways to get rid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/30B01J37/02C07C21/06C07C17/08
Inventor 董轶望高吉轩雷新胜朱雨良
Owner 内蒙古海驰高科新材有限公司
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