CN105214730A - A kind of method preparing modified catalyst supports - Google Patents
A kind of method preparing modified catalyst supports Download PDFInfo
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- CN105214730A CN105214730A CN201510665691.1A CN201510665691A CN105214730A CN 105214730 A CN105214730 A CN 105214730A CN 201510665691 A CN201510665691 A CN 201510665691A CN 105214730 A CN105214730 A CN 105214730A
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Abstract
The invention provides a kind of method preparing modified catalyst supports, be dissolved in by modifier in organic solvent, under the condition of 40-90 DEG C, agitating heating 1h-4h, evaporates, until evaporation becomes thick liquid; Impregnated in catalyst carrier by the thick liquid obtained, described catalyst carrier takes by the 50%-90% accounting for final mass mark, and dip time is 12-48h; Catalyst carrier after dipping transferred in drying box and carry out drying under 90 DEG C of conditions, drying time is 12h; Be transferred in Muffle furnace by the desciccate obtained in step (3), under 300-400 DEG C of condition, roasting 3h, takes out and is cooled to room temperature.The invention has the beneficial effects as follows that the catalyst activity obtained is high, simple convenient operation, be suitable for being applied to industrial production.
Description
Technical field
The invention belongs to catalyst technical field, especially relate to a kind of method preparing modified catalyst supports.
Background technology
Along with the raising of the development of national economy, raising and the environmental protection consciousness day by day of living standards of the people, the demand of PVC (polyvinyl chloride) is increasing.PVC is obtained by VCM (VCM) polymerization, and the production method of VCM mainly contains ethylene process technique, ethane method technique and acetylene method technique.
China is due to resource distribution situation, unstripped gas ethene does not enrich, and lacks all very much and price is very high always, and along with the exhaustion of fossil resources, the coal that China has a large amount of low cost provides raw material and price advantage, so China is applicable to acetylene method route for main production VCM.Therefore in west area, as the area of the rich coal resources such as Xinjiang, Inner Mongol, it is rapid that carbide that is newly-built or enlarging produces Corvic project development.But the fatal bottleneck problem that restriction acetylene method becomes Green Chemistry is catalyst problem, the principle active component of industrial its catalyst used at present is mercury chloride, and mercury easily distils loss, is the severe contamination source in carbide production polyvinyl chloride.
Therefore urgently to be resolved hurrily is at present the pollution problem that mercury catalyst causes, research replaces the non-mercury catalyst of mercuric chleride catalyst to the existence of the enterprise of acetylene method production PVC, to environmental problem, and economic development, the raising of living standards of the people, builds a harmonious society and plays huge effect.
A kind of modified catalyst supports provided by the invention, through the catalyst carrier that triphenylphosphine is modified, can the sulfate of supported copper or tin or chloride, avoid the use of mercury chloride, the method by environmental friendliness formula produces VCM.
Summary of the invention
The object of this invention is to provide a kind of method preparing modified catalyst supports that structure is simple, simple to operate, production efficiency is high, be especially suitable for P Modification catalyst carrier used in VCM production.
Technical scheme of the present invention is:
Prepare a method for modified catalyst supports, comprise the following steps
(1) be dissolved in organic solvent by modifier, under the condition of 40-90 DEG C, agitating heating 1h-4h, evaporates, until evaporation becomes thick liquid;
(2) impregnated in catalyst carrier by the thick liquid that step (1) obtains, described catalyst carrier takes by the 50%-90% accounting for final mass mark, and dip time is 12-48h;
(3) catalyst carrier after dipping step (2) obtained is transferred in drying box and is carried out drying under 90 DEG C of conditions, and drying time is 12h;
(4) be transferred in Muffle furnace by the desciccate obtained in step (3), under 300-400 DEG C of condition, roasting 3h, takes out and is cooled to room temperature.
Preferably, described catalyst carrier is active carbon, CNT, alundum (Al2O3), silica, titanium dioxide, carborundum or molecular sieve.
Preferably, described modifier is P Modification agent or oxygen modifier.
Preferably, described P Modification agent is triphenylphosphine.
Another aspect of the present invention, also comprises the P Modification catalyst obtained by a kind of described method preparing modified catalyst supports.
The advantage that the present invention has and good effect are:
1, preparation method's operating process of the present invention is simple, raw material is inexpensive, reaction temperature is low, has advantages such as being easy to large-scale production, for the production preparing P Modification catalyst provides reference frame.
2, prepare the process environmental protection of modified catalyst, obtained catalyst activity is high.
Detailed description of the invention
Embodiment 1:
A kind of method preparing modified catalyst supports of the present embodiment, comprises the following steps:
(1) be dissolved in anhydrous ethanol solvent by triphenylphosphine, under the condition of water-bath 80 DEG C, agitating heating 2h, evaporates, until evaporation becomes thick liquid;
(2) impregnated on active carbon by thick liquid, described absorbent charcoal carrier takes by account for final mass mark 80%, and dip time is 24h;
(3) absorbent charcoal carrier after dipping step (2) obtained is transferred in drying box and is carried out drying under 90 DEG C of conditions, and drying time is 12h;
(4) desciccate obtained in step (3) is transferred in Muffle furnace, under nitrogen purge, heats up gradually with the speed of 5 DEG C per minute, until temperature reaches 400 DEG C, with this understanding, roasting 3h, taking-up is cooled to room temperature, obtains the catalyst carrier of modification.
In the catalyst carrier that above-mentioned steps obtains, load copper sulphate, can be prepared into the catalyst without mercury of catalyzing acetylene hydrochlorination, this catalyst 200 DEG C, acetylene air speed is 210h
-1, raw material acetylene, hydrogen chloride automobile fitting ratio be catalyzing acetylene hydrochlorination under the condition of 1: 1.2, the initial conversion obtaining acetylene is 50%, and the selective of vinyl chloride is greater than 90%.
Embodiment 2:
A kind of method preparing modified catalyst supports of the present embodiment, comprises the following steps:
(1) be dissolved in anhydrous ethanol solvent by triphenylphosphine, under the condition of 90 DEG C, agitating heating 1h, evaporates, until evaporation becomes thick liquid;
(2) impregnated on ZTCMS-185 type molecular sieve by the thick liquid that step (1) obtains, described catalyst carrier takes by account for final mass mark 80%, and dip time is 48h;
(3) catalyst carrier after dipping step (2) obtained is transferred in drying box and is carried out drying under 90 DEG C of conditions, and drying time is 12h;
(4) desciccate obtained in step (3) is transferred in Muffle furnace, under nitrogen purge, heats up gradually with the speed of 5 DEG C per minute, until temperature reaches 350 DEG C, with this understanding, roasting 3h, taking-up is cooled to room temperature, obtains the catalyst carrier of modification.
In the catalyst carrier that above-mentioned steps obtains, load copper chloride, can be prepared into the catalyst without mercury of catalyzing acetylene hydrochlorination, this catalyst 180 DEG C, acetylene air speed is 190h
-1, raw material acetylene, hydrogen chloride automobile fitting ratio be catalyzing acetylene hydrochlorination under the condition of 1: 1.1, the initial conversion obtaining acetylene is 76%, and the selective of vinyl chloride is greater than 95%.
Embodiment 3:
A kind of method preparing modified catalyst supports of the present embodiment, comprises the following steps:
(1) be dissolved in anhydrous ethanol solvent by triphenylphosphine, under the condition of 90 DEG C, agitating heating 1h, evaporates, until evaporation becomes thick liquid;
(2) impregnated on ZTCMS-185 type molecular sieve by the thick liquid that step (1) obtains, described catalyst carrier takes by account for final mass mark 85%, and dip time is 24h;
(3) catalyst carrier after dipping step (2) obtained is transferred in drying box and is carried out drying under 90 DEG C of conditions, and drying time is 12h;
(4) be transferred in Muffle furnace by the desciccate obtained in step (3), under about 400 DEG C conditions, roasting 3h, takes out and is cooled to room temperature.
In the catalyst carrier that above-mentioned steps obtains, load stannic chloride, can be prepared into the catalyst without mercury of catalyzing acetylene hydrochlorination, this catalyst 160 DEG C, acetylene air speed is 200h
-1, raw material acetylene, hydrogen chloride automobile fitting ratio be catalyzing acetylene hydrochlorination under the condition of 1: 1.15, the initial conversion obtaining acetylene is 80%, and the selective of vinyl chloride is greater than 96%.
Embodiment 4:
A kind of method preparing modified catalyst supports of the present embodiment, comprises the following steps:
(1) be dissolved in anhydrous ethanol solvent by triphenylphosphine, under the condition of 90 DEG C, agitating heating 1h, evaporates, until evaporation becomes thick liquid;
(2) impregnated on alundum (Al2O3) powder carrier by the thick liquid that step (1) obtains, described catalyst carrier takes by account for final mass mark 85%, and dip time is 12h;
(3) catalyst carrier after dipping step (2) obtained is transferred in drying box and is carried out drying under 90 DEG C of conditions, and drying time is 12h;
(4) be transferred in Muffle furnace by the desciccate obtained in step (3), under 400 DEG C of conditions, roasting 3h, takes out and is cooled to room temperature.
In the catalyst carrier that above-mentioned steps obtains, load stannic chloride, can be prepared into the catalyst without mercury of catalyzing acetylene hydrochlorination, this catalyst 180 DEG C, acetylene air speed is 210h
-1, raw material acetylene, hydrogen chloride automobile fitting ratio be catalyzing acetylene hydrochlorination under the condition of 1: 1.1, the initial conversion obtaining acetylene is 80%, and the selective of vinyl chloride is greater than 93%.
Embodiment 5:
A kind of method preparing modified catalyst supports of the present embodiment, comprises the following steps:
(1) be dissolved in anhydrous ethanol solvent by triphenylphosphine, under the condition of 90 DEG C, agitating heating 1h, evaporates, until evaporation becomes thick liquid;
(2) impregnated on titania support by the thick liquid that step (1) obtains, described catalyst carrier takes by account for final mass mark 80%, and dip time is 48h;
(3) catalyst carrier after dipping step (2) obtained is transferred in drying box and is carried out drying under 90 DEG C of conditions, and drying time is 12h;
(4) be transferred in Muffle furnace by the desciccate obtained in step (3), under 400 DEG C of conditions, roasting 3h, takes out and is cooled to room temperature.
In the catalyst carrier that above-mentioned steps obtains, load STANNOUS SULPHATE CRYSTALLINE, can be prepared into the catalyst without mercury of catalyzing acetylene hydrochlorination, this catalyst 160 DEG C, acetylene air speed is 180h
-1, raw material acetylene, hydrogen chloride automobile fitting ratio be catalyzing acetylene hydrochlorination under the condition of 1: 1.2, the initial conversion obtaining acetylene is 75%, and the selective of vinyl chloride is greater than 89%.
Above five embodiments of the present invention have been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the present patent application scope change and improve, and all should still belong within patent covering scope of the present invention.
Claims (5)
1. prepare a method for modified catalyst supports, it is characterized in that: comprise the following steps
(1) be dissolved in organic solvent by modifier, under the condition of 40-90 DEG C, agitating heating 1h-4h, evaporates, until evaporation becomes thick liquid;
(2) impregnated in catalyst carrier by the thick liquid that step (1) obtains, described catalyst carrier takes by the 50%-90% accounting for final mass mark, and dip time is 12-48h;
(3) catalyst carrier after dipping step (2) obtained is transferred in drying box and is carried out drying under 90 DEG C of conditions, and drying time is 12h;
(4) be transferred in Muffle furnace by the desciccate obtained in step (3), under 300-400 DEG C of condition, roasting 3h, takes out and is cooled to room temperature.
2. a kind of method preparing modified catalyst supports according to claim 1, is characterized in that: described catalyst carrier is active carbon, CNT, alundum (Al2O3), silica, titanium dioxide, carborundum or molecular sieve.
3. a kind of method preparing modified catalyst supports according to claim 1, is characterized in that: described modifier is P Modification agent or oxygen modifier.
4. a kind of method preparing modified catalyst supports according to claim 3, is characterized in that: described P Modification agent is triphenylphosphine.
5. the P Modification catalyst obtained by the arbitrary a kind of described method preparing modified catalyst supports of claim 1-4.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104415794A (en) * | 2013-08-27 | 2015-03-18 | 天津大学 | Phosphorus modified catalyst carrier, preparation method and application of phosphorus modified catalyst carrier |
| CN104415793A (en) * | 2013-08-27 | 2015-03-18 | 天津大学 | Oxygen-modified catalyst carrier, and preparation method and application thereof |
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2015
- 2015-10-10 CN CN201510665691.1A patent/CN105214730A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104415794A (en) * | 2013-08-27 | 2015-03-18 | 天津大学 | Phosphorus modified catalyst carrier, preparation method and application of phosphorus modified catalyst carrier |
| CN104415793A (en) * | 2013-08-27 | 2015-03-18 | 天津大学 | Oxygen-modified catalyst carrier, and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| NIKOLAOS KAROUSIS ET AL.: ""Current Progress on the Chemical Modification of Carbon Nanotubes"", 《CHEMICAL REVIEWS》 * |
| 葛鑫等: ""多壁碳纳米管载体的改性及应用"", 《材料导报》 * |
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Application publication date: 20160106 |