Method for preparing iridium chloride solid-phase mercury-free catalyst

A mercury catalyst, iridium chloride technology, applied in the field of fine chemistry, can solve problems such as low selectivity

Inactive Publication Date: 2018-05-15
NINGXIA JINHAI CHUANGKE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the research of using iridium chloride to catalyze the hydrochlorination of acetylene, the low selec

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1 A kind of preparation method of iridium chloride solid-phase mercury-free catalyst

[0024] Step 1, preparation of activated carbon

[0025] (1) Raw material pretreatment

[0026] The selected raw material is red mud, said red mud: particle diameter 0.155~0.187 mm, specific gravity 2.82~2.86, bulk density 0.92~0.97, containing 35-38% CaO, SiO 2 28-31%, Al 2 o 3 5.5-6.2%, Fe 2 o 3 8.2-8.7%, TiO 2 3.8-4.4%.

[0027] The above-mentioned red mud is ground at 88°C to a particle size of 3.5-4.2 μm, and then mixed with wood vinegar and coal tar. The mixing mass ratio of red mud, wood vinegar and coal tar is 1:1.8:1.5; The pitch content of coal tar is 48-50%.

[0028] Heat the mixture of red mud, wood vinegar, and coal tar to 89-92°C, add MCM-41, sodium thiocyanate, tapioca flour, and graphene, and stir evenly to obtain a mixture;

[0029] The additions of the MCM-41, sodium thiocyanate, cassava flour and graphene are respectively 22%, 5.5%, 8.5% and 4...

Embodiment 2

[0046] Embodiment 2 above-mentioned catalyst is used for synthetic reaction of vinyl chloride

[0047] (1) Filling with mercury-free catalyst

[0048] Before filling the mercury-free catalyst, check that there are no leaks inside and outside the reactor, and the inner wall of the tubes is clean, dry, and free of foreign matter; the catalyst of the present invention is immediately packed into each tube of the reactor after opening the package, and the catalyst should be filled at 0.5 Complete within h, beware of moisture.

[0049] (2) Pretreatment

[0050] Pass through dry HCl at 96°C, control rate 33.5m 3 / h, continuous 1h, release acid from the bottom of the reactor.

[0051] (3) Synthesis of vinyl chloride reaction

[0052] The molar ratio of acetylene and hydrogen chloride is controlled at 1:1.3 (100% purity), and the mixed gas with a preheated temperature above 90°C is passed into the reactor, and the reaction temperature is controlled between 125-130°C; the space veloci...

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Abstract

The invention provides a method for preparing an iridium chloride solid-phase mercury-free catalyst. The iridium chloride solid-phase mercury-free catalyst contains, by weight, 3.69% of iridium chloride and is 1651m<2>/g in specific surface area and 4.3-4.6nm in average pore size. The preparation method includes activated carbon preparation, adsorbent preparation and adsorption treatment. Activated carbon preparation includes steps: mixing red mud, pyroligneous liquor and coal tar according to a mass ratio of 1:1.8:1.5, heating to 89-92 DEG C, adding MCM-41, sodium thiocyanate, cassava meal and graphene, and well stirring to obtain a mixture. By adoption of the method, the acetylene conversion rate of the iridium chloride solid-phase mercury-free catalyst in vinyl chloride synthesis reaction is greatly increased.

Description

technical field [0001] The invention relates to a preparation method of an iridium chloride solid-phase mercury-free catalyst, which belongs to the technical field of fine chemistry. Background technique [0002] At present, the hydrochlorination of acetylene in industrial production accounts for about 60% of the domestic mercury consumption, and causes serious harm to the environment and human health. High-mercury catalysts with 12%-15% mercuric chloride loading are mainly used, followed by low-mercury catalysts with 4%-6% mercuric chloride loading. In view of the scarcity of mercury resources and environmental pollution, as well as the increasingly stringent domestic and foreign policies on the prevention and control of mercury pollution, it is urgent to develop high-performance and environmentally friendly catalysts for the synthesis of vinyl chloride. [0003] Iridium chloride, the English name is Iridium(III) chloride hydrate, and the CAS number is 14996-61-3. It is st...

Claims

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Application Information

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IPC IPC(8): B01J31/38C07C17/08C07C21/06
CPCB01J31/38C07C17/08C07C21/06
Inventor 常炳恩李玉强李庆李通
Owner NINGXIA JINHAI CHUANGKE CHEM TECH
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