CN106914277A - A kind of ultralow mercuric chloride catalyst and preparation method for adding hcl reaction for acetylene - Google Patents
A kind of ultralow mercuric chloride catalyst and preparation method for adding hcl reaction for acetylene Download PDFInfo
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Abstract
The present invention proposes a kind of for acetylene plus the ultralow mercuric chloride catalyst and preparation method of hcl reaction, ultralow mercuric chloride catalyst includes carrier, major catalyst, co-catalyst and auxiliary agent, carrier is activated carbon, major catalyst is mercury chloride, and co-catalyst is at least one in bismuth chloride, cerium chloride, stannous chloride, copper chloride, potassium chloride, lanthanum chloride, manganese chloride, stannic chloride, zinc chloride, silver chlorate and iron chloride；Auxiliary agent is ionic liquid, including disubstituted imidazole class ionic liquid, tri-substituted imidazole class ionic liquid, pyridine ionic liquid, sulfonic acid funtionalized class ionic liquid, hydroxy functionalized class ionic liquid, alkenyl functionalization class ionic liquid, benzyl functionalization class ionic liquid, carboxyl-functional class ionic liquid, ester group functionalization class ionic liquid or guanidine ionic liquid.The reaction temperature of the ultralow mercuric chloride catalyst of the present invention is low, and mercury chloride is non-volatile, long lifespan, and high conversion rate, selectivity are high, simple production process, cycle is short.
Description
Technical field
The present invention relates to a kind of mercuric chloride catalyst of super low loading and preparation method thereof, the catalyst adds hcl reaction for acetylene.The invention belongs to the technology of preparing and range of application of catalyst.
Technical background
Mercuric chloride catalyst is acetylene plus the most frequently used catalyst of hcl reaction.The Hg chloride content of existing catalyst is typically 10.5%~12.5%, and when synthesis vinyl chloride thereof is completed, the Hg chloride content of the useless mercury catalyst of recovery is 3% or so.Illustrate to be consumed in acetylene adds hcl reaction about 7.5% mercury chloride.
Heavy metal pollution is global problem, mercury paces is prohibited in the world and is accelerated.The Chinese government pays much attention to mercury pollution preventing and treating, propose the direction and goal of reduction mercury pollution, relevant departments are required to the end of the year 2015, and acetylene from calcium carbide adds the enterprise of hydrogen chloride synthesis vinyl chloride thereof all using low mercury catalyst (4%~6.5%), and to take various ways to reduce mercury loss.
The present invention is the continuity on the working foundation of China Patent No. ZL 200910236255.7 and patent No. ZL201010185916.0.
The content of the invention
It is an object of the invention to provide a kind of ultralow mercuric chloride catalyst for adding hcl reaction for acetylene, the ultralow mercuric chloride catalyst includes carrier, major catalyst, co-catalyst and ionic liquid, the carrier is activated carbon, the major catalyst is mercury chloride, and the co-catalyst is at least one in bismuth chloride, cerium chloride, stannous chloride, copper chloride, potassium chloride, lanthanum chloride, manganese chloride, stannic chloride, zinc chloride, silver chlorate and iron chloride；The ionic liquid is disubstituted imidazole class ionic liquid, tri-substituted imidazole class ionic liquid, pyridine ionic liquid, sulfonic acid funtionalized class ionic liquid, hydroxy functionalized class ionic liquid, alkenyl functionalization class ionic liquid, benzyl functionalization class ionic liquid, carboxyl-functional class ionic liquid, ester group functionalization class ionic liquid or guanidine ionic liquid.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, preferably, the content 40%-98wt.% of the carrier, the content of the major catalyst is in 2~4wt.%, the content of the co-catalyst is 1~45wt.%, the content 1%-40wt.% of the ionic liquid
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, it is preferable that the activated carbon is coconut husk activated carbon, coal mass active carbon, wood activated charcoal, MCM-41 or MCM-13X.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, preferably, the co-catalyst is one or more in bismuth chloride, cerium chloride, stannous chloride, copper chloride, potassium chloride, lanthanum chloride, manganese chloride, stannic chloride, silver chlorate and zinc chloride.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention,Preferably,The disubstituted imidazole class ionic liquid is 1- ethyl-3-methylimidazole bromides,1- ethyl-3-methylimidazole salt compounded of iodine,1- ethyl-3-methylimidazole tetrafluoroborates,1- ethyl-3-methylimidazole hexafluorophosphates,1- ethyl-3-methylimidazole ethyl-sulfate salt,1- ethyl-3-methylimidazole diethyl phosphate salt,1- ethyl-3-methylimidazole perchlorate,1- ethyl-3-methylimidazole rhodanates,1- ethyl-3-methylimidazole toluenesulfonates,1- propyl group -3- methylimidazole villaumites,1- propyl group -3- methylimidazole bromides,1- propyl group -3- methylimidazole salt compounded of iodine,1- propyl group -3- methyl imidazolium tetrafluoroborates,1- propyl group -3- methylimidazole hexafluorophosphates,1- butyl -3- methylimidazole villaumites,1- butyl -3- methylimidazole bromides,1- butyl -3- methylimidazole salt compounded of iodine,1- butyl -3- methyl imidazolium tetrafluoroborates,1- butyl -3- methylimidazole hexafluorophosphates,1- butyl -3- methylimidazolium nitrates,1- butyl -3- methylimidazole perchlorates,1- butyl -3- methylimidazole toluenesulfonates,1- butyl -3- methylimidazole dihydric phosphates,1- butyl -3- methylimidazolium hydrogen sulphate salt,1- butyl -3- methylimidazole rhodanates,1- butyl -3- methylimidazole acetate,1- amyl group -3- methylimidazole villaumites,1- amyl group -3- methylimidazole bromides,1- amyl group -3- methyl imidazolium tetrafluoroborates,1- amyl group -3- methylimidazole hexafluorophosphates,1- amyl group -3- methylimidazole perchlorates,1- hexyl -3- methylimidazole villaumites,1- hexyl -3- methylimidazole bromides,1- hexyl -3- methyl imidazolium tetrafluoroborates,1- hexyl -3- methylimidazole hexafluorophosphates,1- hexyl -3- methylimidazole perchlorates,1- hexyl -3- methylimidazole toluenesulfonates,1- hexyl -3- methylimidazolium hydrogen sulphate salt,1- octyl group -3- methylimidazole bromides,1- octyl group -3- methylimidazole villaumites,1- octyl group -3- methyl imidazolium tetrafluoroborates,1- octyl group -3- methylimidazole hexafluorophosphates,1- octyl group -3- methylimidazolium hydrogen sulphate salt,1- octyl group -3- methylimidazole perchlorates,1- octyl group -3- methylimidazole toluenesulfonates,1- decyl -3- methylimidazole villaumites,1- decyl -3- methylimidazole bromides,1- decyl -3- methyl imidazolium tetrafluoroborates,1- decyl -3- methylimidazole hexafluorophosphates,1- decyl -3- methylimidazole perchlorates,1- decyl -3- methylimidazole toluenesulfonates,1- dodecyl -3- methylimidazole villaumites,1- dodecyl -3- methylimidazole bromides,1- dodecyl -3- methyl imidazolium tetrafluoroborates,1- dodecyl -3- methylimidazole hexafluorophosphates,1- dodecyl -3- methylimidazole perchlorates,1- myristyl -3- methylimidazole bromides,1- myristyl -3- methyl imidazolium tetrafluoroborates,1- myristyl -3- methylimidazole hexafluorophosphates,1- myristyl -3- methylimidazole perchlorates,1- cetyl -3- methylimidazole bromides,1- cetyl -3- methylimidazole hexafluorophosphates,1- cetyl -3- methylimidazole perchlorates,1- cetyl -3- methyl imidazolium tetrafluoroborates.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention,Preferably,The tri-substituted imidazole class ionic liquid is 1- butyl -2,3- methylimidazole villaumites,1- butyl -2,3- methylimidazole bromides,1- butyl -2,3- methylimidazole tetrafluoroborates,1- butyl -2,3- methylimidazole hexafluorophosphates,1- butyl -2,3- methylimidazole nitrate,1- butyl -2,3- methylimidazole perchlorate,1- butyl -2,3- methylimidazole toluenesulfonates,1- butyl -2,3- methylimidazole disulfates,1- butyl -2,3- methylimidazole dihydric phosphates,1- hexyls -2,3- methylimidazole villaumites,1- hexyls -2,3- methylimidazole bromides,1- hexyls -2,3- methylimidazole tetrafluoroborates,1- hexyls -2,3- methylimidazole hexafluorophosphates,1- hexyls -2,3- methylimidazole perchlorate.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, preferably, the pyridine ionic liquid is N- butyl-pyridinium bromides, N- butyl-pyridinium tetrafluoroborates, N- butyl-pyridinium hexafluorophosphates, N- butyl-pyridinium perchlorate, N- butyl-pyridinium toluenesulfonates, N- hexyl pyridine bromides, N- hexyl pyridinium tetrafluoroborate salt, N- hexyl pyridine hexafluorophosphates, N- octylpyridinium bromides, N- octylpyridinium tetrafluoroborates, N- octylpyridinium hexafluorophosphates, pyrrolidines, N- butyl-N- crassitude bromides, N- butyl-N- crassitude tetrafluoroborates, N- butyl-N- crassitude hexafluorophosphates.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, preferably, the sulfonic acid funtionalized class ionic liquid is 1- propyl sulfonic acid -3- methylimidazoles inner salt, 1- propyl sulfonic acid -3- methylimidazolium hydrogen sulphates salt, pyridine-sulfonic acid propiolactone, N- propyl sulfonic acid pyridines disulfate, N- propyl sulfonic acid -3- picoline tosilate.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention,Preferably,The hydroxy functionalized class ionic liquid is trimethyl hydroxyethylammonium ammonium tetrafluoroborate,1- ethoxy -3- methylimidazole villaumites,1- ethoxy -3- methyl imidazolium tetrafluoroborates,1- ethoxy -3- methylimidazole hexafluorophosphates,1- ethoxy -3- methylimidazole toluenesulfonates,1- ethoxy -3- methylimidazolium hydrogen sulphate salt,1- ethoxys -2,3- methylimidazole villaumites,1,2- dimethyl -3- hydroxyethyl imidazole tetrafluoroborates,1,2- dimethyl -3- hydroxyethyl imidazole hexafluorophosphates,1,2- dimethyl -3- hydroxyethyl imidazole perchlorate,1,2- dimethyl -3- hydroxyethyl imidazole toluenesulfonates,1,2- dimethyl -3- hydroxyethyl imidazole disulfates.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, preferably, the alkenyl functionalization class ionic liquid is 1- pi-allyl -3- methylimidazole villaumites, 1- pi-allyl -3- methyl imidazolium tetrafluoroborates, 1- pi-allyl -3- methylimidazole hexafluorophosphates, 1- pi-allyl -3- methylimidazole tosilate, 1- vinyl -3- ethyl imidazol(e) bromides, 1- vinyl -3- ethyl imidazol(e) tetrafluoroborates, 1- vinyl -3- ethyl imidazol(e) hexafluorophosphates, 1- vinyl -3- butyl imidazole villaumites, 1- vinyl -3- butyl imidazole bromides, 1- vinyl -3- butyl imidazole tetrafluoroborates, 1- vinyl -3- butyl imidazole hexafluorophosphates.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, preferably, the benzyl functionalization class ionic liquid is 1- benzyl -3- methylimidazole villaumites, 1- benzyl -3- methyl imidazolium tetrafluoroborates, 1- benzyl -3- methylimidazoles hexafluorophosphate, 1- benzyl -3- methylimidazole tosilate.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, it is preferable that the carboxyl-functional class ionic liquid is 1- carboxymethyl -3- methylimidazole villaumites, 1- carboxymethyl -3- methylimidazolium hydrogen sulphates salt, 1- carboxyethyl -3- methylimidazole villaumites.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, preferably, the ester group functionalization class ionic liquid is 1- ethyl acetate base -3- methylimidazole villaumites, 1- ethyl acetate base -3- methyl imidazolium tetrafluoroborates, 1- ethyl acetate base -3- methylimidazoles hexafluorophosphate, 1- ethyl acetate base -3- methylimidazolium hydrogen sulphates salt, 1- ethylacrylate methyl -3- methylimidazole villaumites, 1- ethylacrylate methyl -3- methyl imidazolium tetrafluoroborates, 1- ethylacrylate methyl -3- methylimidazole hexafluorophosphates.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, preferably, the guanidine ionic liquid is TMG hydrochloride, TMG disulfate, TMG nitrate, TMG borofluoride, TMG acetate, TMG lactate, TMG dihydric phosphate.
Further illustrated as to the ultralow mercuric chloride catalyst of the invention, it is preferable that the water for major catalyst, co-catalyst and auxiliary agent is 1~5 times of carrier water absorption rate.
Another object of the present invention is to provide a kind of method for preparing the ultralow mercuric chloride catalyst for acetylene plus hcl reaction, methods described comprises the following steps：1) appropriate major catalyst, co-catalyst and auxiliary agent are weighed；2) at a temperature of 40-90 DEG C, major catalyst, co-catalyst and auxiliary agent are dissolved and in deionized water and is stirred, obtain mixed solution；And 3) be sufficiently impregnated on carrier with the mixed solution, then the carrier after dipping is dried；Wherein, the carrier is activated carbon, and the major catalyst is mercury chloride, and the co-catalyst is one or more in bismuth chloride, cerium chloride, stannous chloride, copper chloride, potassium chloride, lanthanum chloride, manganese chloride, stannic chloride, zinc chloride, silver chlorate and iron chloride；The auxiliary agent is disubstituted imidazole class ionic liquid, tri-substituted imidazole class ionic liquid, pyridine ionic liquid, sulfonic acid funtionalized class ionic liquid, hydroxy functionalized class ionic liquid, alkenyl functionalization class ionic liquid, benzyl functionalization class ionic liquid, carboxyl-functional class ionic liquid, ester group functionalization class ionic liquid or guanidine ionic liquid.
Further illustrated as to methods described of the invention, it is preferable that the temperature of the drying is 80-150 DEG C.
Further illustrated as to methods described of the invention, it is preferable that the 40~98wt.% of content of the carrier.In 2~4wt.%, the content of the co-catalyst is 1~45wt.%, the 1~40wt.% of content of the ionic liquid to the content of the major catalyst.
Further illustrated as to methods described of the invention, it is preferable that the activated carbon is coconut husk activated carbon, coal mass active carbon, wood activated charcoal, MCM-41 or MCM-13X；The disubstituted imidazole class ionic liquid is 1- ethyl-3-methylimidazole bromides,1- ethyl-3-methylimidazole salt compounded of iodine,1- ethyl-3-methylimidazole tetrafluoroborates,1- ethyl-3-methylimidazole hexafluorophosphates,1- ethyl-3-methylimidazole ethyl-sulfate salt,1- ethyl-3-methylimidazole diethyl phosphate salt,1- ethyl-3-methylimidazole perchlorate,1- ethyl-3-methylimidazole rhodanates,1- ethyl-3-methylimidazole toluenesulfonates,1- propyl group -3- methylimidazole villaumites,1- propyl group -3- methylimidazole bromides,1- propyl group -3- methylimidazole salt compounded of iodine,1- propyl group -3- methyl imidazolium tetrafluoroborates,1- propyl group -3- methylimidazole hexafluorophosphates,1- butyl -3- methylimidazole villaumites,1- butyl -3- methylimidazole bromides,1- butyl -3- methylimidazole salt compounded of iodine,1- butyl -3- methyl imidazolium tetrafluoroborates,1- butyl -3- methylimidazole hexafluorophosphates,1- butyl -3- methylimidazolium nitrates,1- butyl -3- methylimidazole perchlorates,1- butyl -3- methylimidazole toluenesulfonates,1- butyl -3- methylimidazole dihydric phosphates,1- butyl -3- methylimidazolium hydrogen sulphate salt,1- butyl -3- methylimidazole rhodanates,1- butyl -3- methylimidazole acetate,1- amyl group -3- methylimidazole villaumites,1- amyl group -3- methylimidazole bromides,1- amyl group -3- methyl imidazolium tetrafluoroborates,1- amyl group -3- methylimidazole hexafluorophosphates,1- amyl group -3- methylimidazole perchlorates,1- hexyl -3- methylimidazole villaumites,1- hexyl -3- methylimidazole bromides,1- hexyl -3- methyl imidazolium tetrafluoroborates,1- hexyl -3- methylimidazole hexafluorophosphates,1- hexyl -3- methylimidazole perchlorates,1- hexyl -3- methylimidazole toluenesulfonates,1- hexyl -3- methylimidazolium hydrogen sulphate salt,1- octyl group -3- methylimidazole bromides,1- octyl group -3- methylimidazole villaumites,1- octyl group -3- methyl imidazolium tetrafluoroborates,1- octyl group -3- methylimidazole hexafluorophosphates,1- octyl group -3- methylimidazolium hydrogen sulphate salt,1- octyl group -3- methylimidazole perchlorates,1- octyl group -3- methylimidazole toluenesulfonates,1- decyl -3- methylimidazole villaumites,1- decyl -3- methylimidazole bromides,1- decyl -3- methyl imidazolium tetrafluoroborates,1- decyl -3- methylimidazole hexafluorophosphates,1- decyl -3- methylimidazole perchlorates,1- decyl -3- methylimidazole toluenesulfonates,1- dodecyl -3- methylimidazole villaumites,1- dodecyl -3- methylimidazole bromides,1- dodecyl -3- methyl imidazolium tetrafluoroborates,1- dodecyl -3- methylimidazole hexafluorophosphates,1- dodecyl -3- methylimidazole perchlorates,1- myristyl -3- methylimidazole bromides,1- myristyl -3- methyl imidazolium tetrafluoroborates,1- myristyl -3- methylimidazole hexafluorophosphates,1- myristyl -3- methylimidazole perchlorates,1- cetyl -3- methylimidazole bromides,1- cetyl -3- methylimidazole hexafluorophosphates,1- cetyl -3- methylimidazole perchlorates,1- cetyl -3- methyl imidazolium tetrafluoroborates；The tri-substituted imidazole class ionic liquid is 1- butyl -2,3- methylimidazole villaumites,1- butyl -2,3- methylimidazole bromides,1- butyl -2,3- methylimidazole tetrafluoroborates,1- butyl -2,3- methylimidazole hexafluorophosphates,1- butyl -2,3- methylimidazole nitrate,1- butyl -2,3- methylimidazole perchlorate,1- butyl -2,3- methylimidazole toluenesulfonates,1- butyl -2,3- methylimidazole disulfates,1- butyl -2,3- methylimidazole dihydric phosphates,1- hexyls -2,3- methylimidazole villaumites,1- hexyls -2,3- methylimidazole bromides,1- hexyls -2,3- methylimidazole tetrafluoroborates,1- hexyls -2,3- methylimidazole hexafluorophosphates,1- hexyls -2,3- methylimidazole perchlorate；The pyridine ionic liquid is N- butyl-pyridinium bromides, N- butyl-pyridinium tetrafluoroborates, N- butyl-pyridinium hexafluorophosphates, N- butyl-pyridinium perchlorate, N- butyl-pyridinium toluenesulfonates, N- hexyl pyridine bromides, N- hexyl pyridinium tetrafluoroborate salt, N- hexyl pyridine hexafluorophosphates, N- octylpyridinium bromides, N- octylpyridinium tetrafluoroborates, N- octylpyridinium hexafluorophosphates, pyrrolidines, N- butyl-N- crassitude bromides, N- butyl-N- crassitude tetrafluoroborates, N- butyl-N- crassitude hexafluorophosphates；The sulfonic acid funtionalized class ionic liquid is 1- propyl sulfonic acid -3- methylimidazoles inner salt, 1- propyl sulfonic acid -3- methylimidazolium hydrogen sulphates salt, pyridine-sulfonic acid propiolactone, N- propyl sulfonic acid pyridines disulfate, N- propyl sulfonic acid -3- picoline tosilate；The hydroxy functionalized class ionic liquid is trimethyl hydroxyethylammonium ammonium tetrafluoroborate, 1- ethoxy -3- methylimidazole villaumites, 1- ethoxy -3- methyl imidazolium tetrafluoroborates, 1- ethoxy -3- methylimidazole hexafluorophosphates, 1- ethoxy -3- methylimidazole toluenesulfonates, 1- ethoxy -3- methylimidazolium hydrogen sulphate salt, 1- ethoxys -2, 3- methylimidazole villaumites, 1, 2- dimethyl -3- hydroxyethyl imidazole tetrafluoroborates, 1, 2- dimethyl -3- hydroxyethyl imidazole hexafluorophosphates, 1, 2- dimethyl -3- hydroxyethyl imidazole perchlorate, 1, 2- dimethyl -3- hydroxyethyl imidazole toluenesulfonates, 1, 2- dimethyl -3- hydroxyethyl imidazole disulfates；The alkenyl functionalization class ionic liquid is 1- pi-allyl -3- methylimidazole villaumites, 1- pi-allyl -3- methyl imidazolium tetrafluoroborates, 1- pi-allyl -3- methylimidazole hexafluorophosphates, 1- pi-allyl -3- methylimidazole tosilate, 1- vinyl -3- ethyl imidazol(e) bromides, 1- vinyl -3- ethyl imidazol(e) tetrafluoroborates, 1- vinyl -3- ethyl imidazol(e) hexafluorophosphates, 1- vinyl -3- butyl imidazole villaumites, 1- vinyl -3- butyl imidazole bromides, 1- vinyl -3- butyl imidazole tetrafluoroborates, 1- vinyl -3- butyl imidazole hexafluorophosphates；The benzyl functionalization class ionic liquid is 1- benzyl -3- methylimidazole villaumites, 1- benzyl -3- methyl imidazolium tetrafluoroborates, 1- benzyl -3- methylimidazoles hexafluorophosphate, 1- benzyl -3- methylimidazole tosilate；The carboxyl-functional class ionic liquid is 1- carboxymethyl -3- methylimidazole villaumites, 1- carboxymethyl -3- methylimidazolium hydrogen sulphates salt, 1- carboxyethyl -3- methylimidazole villaumites；The ester group functionalization class ionic liquid is 1- ethyl acetate base -3- methylimidazole villaumites, 1- ethyl acetate base -3- methyl imidazolium tetrafluoroborates, 1- ethyl acetate base -3- methylimidazoles hexafluorophosphate, 1- ethyl acetate base -3- methylimidazolium hydrogen sulphates salt, 1- ethylacrylate methyl -3- methylimidazole villaumites, 1- ethylacrylate methyl -3- methyl imidazolium tetrafluoroborates, 1- ethylacrylate methyl -3- methylimidazole hexafluorophosphates；The guanidine ionic liquid is TMG hydrochloride, TMG disulfate, TMG nitrate, TMG borofluoride, TMG acetate, TMG lactate, TMG dihydric phosphate.
It is therefore seen that, it is carrier that catalyst of the invention uses activated carbon, and it is auxiliary agent to be done major catalyst and add one or more metallic compound to be done co-catalyst, ionic liquid with the mercury chloride of 2%~4% super low loading, and new catalyst is obtained after high temperature drying.The characteristics of catalyst of the present invention is that mercury chloride consumption is few, and the content than traditional mercury catalyst mercury reduces 80%, and the low mercury catalyst than promoting the use of at present also reduces half or so, is more beneficial for environmental protection.Reaction temperature is low, and mercury chloride is non-volatile, the long lifespan for using, and high conversion rate, selectivity are high.Catalyst makes simple production process, cycle is short.Catalyst uses the converter for not changing original acetylene plus hcl reaction.
Specific embodiment
In order that auditor can further appreciate that structure of the invention, feature and other purposes, as follows in conjunction with appended preferred embodiment detailed description, the present embodiment is merely to illustrate technical scheme, and the non-limiting present invention.
Embodiment 1：
Mercury chloride 0.63g, bismuth chloride 2g, 1- ethyl-3-methylimidazole tetrafluoroborate 4g is weighed to be put into the deionized water of 60g.After fully being dissolved under 60 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 2.91%, bismuth chloride 9.29%, the catalyst of 1- ethyl-3-methylimidazoles tetrafluoroborate 18.49%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 78%, selectivity is more than 99%.
Embodiment 2：
Mercury chloride 0.68g, cerium chloride 1.6g, 1- propyl group -3- methylimidazole villaumites 4.5g is weighed to be put into the deionized water of 80g.After fully being dissolved under 80 degree, the coal mass active carbon of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 3.12%, cerium chloride 7.35%, the catalyst of 1- propyl group -3- methylimidazole villaumites 20.66%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 160 degree, HCl：C2H2=1.05:1, conversion ratio 79%, selectivity is more than 99%.
Embodiment 3：
Mercury chloride 0.66g, stannous chloride 1.8g, 1- hexyl -3- methyl imidazolium tetrafluoroborates 3.6g is weighed to be put into the deionized water of 60g.After fully being dissolved under 60 degree, the wood activated charcoal of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 3.13%, stannous chloride 8.55%, the catalyst of 1- hexyl -3- methyl imidazolium tetrafluoroborates 17.09%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 165 degree, HCl：C2H2=1.05:1, conversion ratio 85%, selectivity is more than 99%.
Embodiment 4：
Mercury chloride 0.65g, copper chloride 1g, 1- octyl group -3- methylimidazole toluenesulfonates 3.2g is weighed to be put into the deionized water of 35g.After fully being dissolved under 60 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 3.27%, copper chloride 5.04%, the catalyst of 1- octyl group -3- methylimidazoles toluenesulfonate 16.12%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 165 degree, HCl：C2H2=1.05:1, conversion ratio 65%, selectivity is more than 99%.
Embodiment 5：
Mercury chloride 0.62g, potassium chloride 1.5g, 1- butyl -2,3- methylimidazole villaumites 6.5g is weighed to be put into the deionized water of 35g.After fully being dissolved under 80 degree, the coal mass active carbon of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 2.62%, potassium chloride 6.359%, 1- butyl -2, the catalyst of 3- methylimidazoles villaumite 27.52%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 150 degree, HCl：C2H2=1.05:1, conversion ratio 78%, selectivity is more than 99%.
Embodiment 6：
Mercury chloride 0.66g, lanthanum chloride 1.6g, 1- butyl -2,3- methylimidazole nitrate 2g is weighed to be put into the deionized water of 35g.After fully being dissolved under 70 degree, the wood activated charcoal of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 3.43%, lanthanum chloride 8.31%, 1- butyl -2, the catalyst of 3- methylimidazoles nitrate 10.38%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 160 degree, HCl：C2H2=1.05:1, conversion ratio 32%, selectivity is more than 99%.
Embodiment 7：
Mercury chloride 0.62g, manganese chloride 2g, 1- butyl -2,3- methylimidazole dihydric phosphates 7.1g is weighed to be put into the deionized water of 35g.After fully being dissolved under 80 degree, the wood activated charcoal of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 2.51%, manganese chloride 8.09%, 1- butyl -2, the catalyst of 3- methylimidazoles dihydric phosphate 28.72%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 150 degree, HCl：C2H2=1.05:1, conversion ratio 86%, selectivity is more than 99%.
Embodiment 8：
Mercury chloride 0.5g, stannic chloride 3g, 1- hexyl -2,3- methylimidazole hexafluorophosphates 3g is weighed to be put into the deionized water of 00g.After fully being dissolved under 70 degree, the MCM-41 of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 2.33%, stannic chloride 13.95%, 1- hexyl -2, the catalyst of 3- methylimidazoles hexafluorophosphate 13.95%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 160 degree, HCl：C2H2=1.05:1, conversion ratio 88%, selectivity is more than 99%.
Embodiment 9：
Mercury chloride 0.55g, silver chlorate 0.4g, N- butyl-pyridinium bromide 3.6g is weighed to be put into the deionized water of 20g.After fully being dissolved under 80 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 2.38%, silver chlorate 2.05%, the catalyst of N- butyl-pyridiniums bromide 18.49%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 170 degree, HCl：C2H2=1.05:1, conversion ratio 96%, selectivity is more than 99%.
Embodiment 10：
Mercury chloride 0.55g, zinc chloride 2.5g, N- butyl-pyridinium hexafluorophosphate 4.25g is weighed to be put into the deionized water of 35g.After fully being dissolved under 70 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 3.47%, zinc chloride 11.21%, the catalyst of N- butyl-pyridiniums hexafluorophosphate 19.06%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 165 degree, HCl：C2H2=1.05:1, conversion ratio 95%, selectivity is more than 99%.
Embodiment 11：
Mercury chloride 0.63g, bismuth chloride 2g, copper chloride 1g, N- butyl-pyridinium toluenesulfonate 4g is weighed to be put into the deionized water of 30g.After fully being dissolved under 60 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 2.78%, bismuth chloride 8.84%, copper chloride 4.42%, the catalyst of N- butyl-pyridiniums toluenesulfonate 17.68%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 165 degree, HCl：C2H2=1.05:1, conversion ratio 89%, selectivity is more than 99%.
Embodiment 12：
Mercury chloride 0.68g, cerium chloride 1.6g, potassium chloride 1.5g, N- hexyl pyridinium tetrafluoroborate salt 4.5g is weighed to be put into the deionized water of 20g.After fully being dissolved under 60 degree, the MCM-41 of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 2.92%, cerium chloride 6.879%, potassium chloride 6.44%, the catalyst of N- hexyl pyridinium tetrafluoroborates salt 19.33%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 170 degree, HCl：C2H2=1.05:1, conversion ratio 93%, selectivity is more than 99%.
Embodiment 13：
Mercury chloride 0.66g, stannous chloride 1.8g, lanthanum chloride 1.6g, N- octylpyridinium bromide 3.6g is weighed to be put into the deionized water of 60g.After fully being dissolved under 60 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 2.91%, stannous chloride 7.94%, lanthanum chloride 7.06%, the catalyst of N- octylpyridiniums bromide 15.89%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 160 degree, HCl：C2H2=1.05:1, conversion ratio 89%, selectivity is more than 99%.
Embodiment 14：
Mercury chloride 0.65g, cerium chloride 2g, copper chloride 1g, N- octylpyridinium hexafluorophosphate 3.2g is weighed to be put into the deionized water of 35g.After fully being dissolved under 60 degree, the coal mass active carbon of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 2.97%, cerium chloride 9.15%, copper chloride 4.85%, the catalyst of N- octylpyridiniums hexafluorophosphate 14.65%.The catalyst adds the reaction of hydrogen chloride for acetylene, under 140 degree, HCl：C2H2=1.05:1, conversion ratio 94%, selectivity is more than 99%.
Embodiment 15：
Mercury chloride 0.62g, potassium chloride 1.5g, stannic chloride 2g, N- butyl-N- crassitude bromides 6.3g is weighed to be put into the deionized water of 35g.After fully being dissolved under 60 degree, the wood activated charcoal of 15g is added.Dipping is dried after 2 hours in 160 degree of baking oven, is made chloride containing mercury 2.42%, potassium chloride 5.85%, stannic chloride 7.81%, the catalyst of N- butyl-N- crassitudes bromide 25.37%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 85%, selectivity is more than 99%.
Embodiment 16：
Mercury chloride 0.66g, lanthanum chloride 1.6g, silver chlorate 1.6g, N- butyl-N- crassitude hexafluorophosphates 2g is weighed to be put into the deionized water of 35g.After fully being dissolved under 70 degree, the MCM-13X of 15g is added.Dipping is dried after 2 hours in 120 degree of baking oven, is made chloride containing mercury 3.16%, lanthanum chloride 7.67%, silver chlorate 7.67%, the catalyst of N- butyl-N- crassitudes hexafluorophosphate 9.59%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 94%, selectivity is more than 99%.
Embodiment 17：
Mercury chloride 0.62g, manganese chloride 2g, zinc chloride 1.8g, 1- propyl sulfonic acid -3- methylimidazolium hydrogen sulphate salt 7.1g is weighed to be put into the deionized water of 30g.After fully being dissolved under 95 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 4 hours in 120 degree of baking oven, is made chloride containing mercury 2.34%, manganese chloride 7.45%, zinc chloride 6.79%, the catalyst of 1- propyl sulfonic acid -3- methylimidazolium hydrogen sulphates salt 26.77%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 68%, selectivity is more than 99%.
Embodiment 18：
Mercury chloride 0.68g, zinc chloride 3g, stannic chloride 1g, trimethyl hydroxyethylammonium ammonium tetrafluoroborate 3g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 3%, zinc chloride 13%, stannic chloride 4.41%, the catalyst of trimethyl hydroxyethylammonium ammonium tetrafluoroborate 13.32%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 84%, selectivity is more than 99%.
Embodiment 19：
Mercury chloride 0.66g, silver chlorate 4g, bismuth chloride 1.6g, 1- ethoxy -3- methylimidazolium hydrogen sulphate salt 3.6g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 2.65%, silver chlorate 16.09%, bismuth chloride 6.44%, the catalyst of 1- ethoxy -3- methylimidazolium hydrogen sulphates salt 14.48%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 91%, selectivity is more than 99%.
Embodiment 20：
Mercury chloride 0.55g, zinc chloride 2.5g, cerium chloride 2g, 1- pi-allyl -3- methylimidazole villaumites 4.25g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the coal mass active carbon of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 2.26%, zinc chloride 10.29%, cerium chloride 8.23%, the catalyst of 1- pi-allyl -3- methylimidazole villaumites 17.49%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 67%, selectivity is more than 99%.
Embodiment 21：
Mercury chloride 0.62g, potassium chloride 1.5g, stannic chloride 2g, zinc chloride 1.6g, 1- benzyl -3- methylimidazole villaumites 4.3g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the wood activated charcoal of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 2.48%, potassium chloride 6.0%, stannic chloride 7.99%, zinc chloride 6.39%, the catalyst of 1- benzyl -3- methylimidazole villaumites 17.19%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 78%, selectivity is more than 99%.
Embodiment 22：
Mercury chloride 0.66g, lanthanum chloride 1.6g, silver chlorate 1.6g, stannic chloride 2g, 1- benzyl -3- methylimidazole hexafluorophosphates 4.25g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the MCM-41 of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 2.63%, lanthanum chloride 6.37%, silver chlorate 6.37%, stannic chloride 7.96%, the catalyst of 1- benzyl -3- methylimidazoles hexafluorophosphate 16.93%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 72%, selectivity is more than 99%.
Embodiment 23：
Mercury chloride 0.62g, manganese chloride 2g, zinc chloride 1.8g, stannic chloride 2g, 1- ethyl acetate base -3- methylimidazole villaumites 4.6g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the MCM-13X of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 2.38%, manganese chloride 7.69%, zinc chloride 6.92%, stannic chloride 7.69%, the catalyst of 1- ethyl acetate base -3- methylimidazole villaumites 17.68%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 77%, selectivity is more than 99%.
Embodiment 24：
Mercury chloride 0.66g zinc chloride 3.5g silver chlorate 3g stannic chloride 2.6g stannous chloride 1.6g, 1- ethylacrylate methyl -3- methyl imidazolium tetrafluoroborates 2.6g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 1.89%, zinc chloride 10.04%, silver chlorate 8.61%, stannic chloride 7.46%, stannous chloride 4.59%, the catalyst of 1- ethylacrylate methyl -3- methyl imidazolium tetrafluoroborates 24.83%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 84%, selectivity is more than 99%.
Embodiment 25：
Mercury chloride 1.3g zinc chloride 4.5g lanthanum chloride 4g silver chlorate 3.6g manganese chlorides 2.6g, TMG hydrochloride 4.5g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 3.29%, zinc chloride 11.39%, lanthanum chloride 10.13%, silver chlorate 9.11%, manganese chloride 6.58%, the catalyst of TMG hydrochloride 21.52%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 97%, selectivity is more than 99%.
Embodiment 26：
Mercury chloride 1.1g zinc chloride 5.5g potassium chloride 5g manganese chloride 4.6g stannous chlorides 2.6g, TMG dihydric phosphate 5.5g is weighed to be put into the deionized water of 30g.After fully being dissolved under 75 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 2 hours in 130 degree of baking oven, is made chloride containing mercury 3.29%, zinc chloride 11.39%, lanthanum chloride 10.13%, silver chlorate 9.11%, manganese chloride 6.58%, the catalyst of TMG dihydric phosphate 21.52%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 97%, selectivity is more than 99%.
Embodiment 27：
Mercury chloride 0.62g, iron chloride 2g, zinc chloride 1.8g, 1- carboxyethyl -3- methylimidazole chlorine 7.1g is weighed to be put into the deionized water of 30g.After fully being dissolved under 95 degree, the coconut husk preparing active carbon of 15g is added.Dipping is dried after 4 hours in 120 degree of baking oven, is made chloride containing mercury 2.34%, iron chloride 7.45%, zinc chloride 6.79%, the catalyst of 1- carboxyethyl -3- methylimidazoles chlorine 26.77%.The catalyst adds the reaction of hydrogen chloride, under 180 degree, HCl for acetylene：C2H2=1.05:1, conversion ratio 68%, selectivity is more than 99%.
Example described above is only the preferred embodiment lifted to absolutely prove the present invention, protection scope of the present invention not limited to this.Equivalent substitute or conversion that those skilled in the art are done on the basis of the present invention, within protection scope of the present invention.Protection scope of the present invention is defined by claims.
Claims (10)
1. a kind of ultralow mercuric chloride catalyst for adding hcl reaction for acetylene, it is characterised in that
The ultralow mercuric chloride catalyst includes carrier, major catalyst, co-catalyst and auxiliary agent, the load
Body is activated carbon, and the major catalyst is mercury chloride, and the co-catalyst is bismuth chloride, chlorination
Cerium, stannous chloride, copper chloride, potassium chloride, lanthanum chloride, manganese chloride, stannic chloride, zinc chloride,
At least one in silver chlorate and iron chloride；The auxiliary agent is ionic liquid, including two substitution miaows
Azole ionic liquid, tri-substituted imidazole class ionic liquid, pyridine ionic liquid, sulfonate functional
Change class ionic liquid, hydroxy functionalized class ionic liquid, alkenyl functionalization class ionic liquid, benzyl
Base functionalization class ionic liquid, carboxyl-functional class ionic liquid, ester group functionalization class ionic liquid
Body or guanidine ionic liquid.
2. ultralow mercuric chloride catalyst according to claim 1, it is characterised in that the load
40~the 98wt.% of content of body.The content of the major catalyst in 2~4wt.%, the co-catalyst
Content be 1~45wt.%, the 1~40wt.% of content of the ionic liquid.
3. ultralow mercuric chloride catalyst according to claim 1 and 2, it is characterised in that institute
Activated carbon is stated for coconut husk activated carbon, coal mass active carbon, wood activated charcoal, MCM-41 or
MCM-13X。
4. ultralow mercuric chloride catalyst according to claim 1 and 2, it is characterised in that institute
State co-catalyst for bismuth chloride, cerium chloride, stannous chloride, copper chloride, potassium chloride, lanthanum chloride,
One or more in manganese chloride, stannic chloride, silver chlorate and zinc chloride.
5. ultralow mercuric chloride catalyst according to claim 1 and 2, it is characterised in that institute
Disubstituted imidazole class ionic liquid is stated for 1- ethyl-3-methylimidazoles bromide, 1- ethyl -3- methyl miaows
Azoles salt compounded of iodine, 1- ethyl-3-methylimidazoles tetrafluoroborate, 1- ethyl-3-methylimidazole hexafluorophosphoric acids
Salt, 1- ethyl-3-methylimidazole ethyl-sulfates salt, 1- ethyl-3-methylimidazole diethyl phosphates salt,
1- ethyl-3-methylimidazoles perchlorate, 1- ethyl-3-methylimidazoles rhodanate, 1- ethyls -3-
Methylimidazole toluenesulfonate, 1- propyl group -3- methylimidazole villaumites, 1- propyl group -3- methyl miaows
Azoles bromide, 1- propyl group -3- methylimidazoles salt compounded of iodine, 1- propyl group -3- methyl imidazolium tetrafluoroborates, 1-
Propyl group -3- methylimidazoles hexafluorophosphate, 1- butyl -3- methylimidazole villaumites, 1- butyl -3- methyl
Imidazoles bromide, 1- butyl -3- methylimidazoles salt compounded of iodine, 1- butyl -3- methyl imidazolium tetrafluoroborates,
1- butyl -3- methylimidazoles hexafluorophosphate, 1- butyl -3- methylimidazolium nitrates, 1- butyl -3-
Methylimidazole perchlorate, 1- butyl -3- methylimidazoles toluenesulfonate, 1- butyl -3- first
Base imidazoles dihydric phosphate, 1- butyl -3- methylimidazolium hydrogen sulphates salt, 1- butyl -3- methylimidazoles
Rhodanate, 1- butyl -3- methylimidazoles acetate, 1- amyl group -3- methylimidazole villaumites, 1- amyl groups
- 3- methylimidazoles bromide, 1- amyl group -3- methyl imidazolium tetrafluoroborates, 1- amyl group -3- methylimidazoles
Hexafluorophosphate, 1- amyl group -3- methylimidazole perchlorates, 1- hexyl -3- methylimidazole villaumites,
1- hexyl -3- methylimidazoles bromide, 1- hexyl -3- methyl imidazolium tetrafluoroborates, 1- hexyl -3- first
Base limidazolium hexafluorophosphate, 1- hexyl -3- methylimidazole perchlorates, 1- hexyl -3- methylimidazoles
Toluenesulfonate, 1- hexyl -3- methylimidazolium hydrogen sulphates salt, 1- octyl group -3- methylimidazole bromines
Salt, 1- octyl group -3- methylimidazole villaumites, 1- octyl group -3- methyl imidazolium tetrafluoroborates, 1- octyl groups -3-
Methylimidazole hexafluorophosphate, 1- octyl group -3- methylimidazolium hydrogen sulphates salt, 1- octyl group -3- methyl miaows
Azoles perchlorate, 1- octyl group -3- methylimidazoles toluenesulfonate, 1- decyl -3- methylimidazoles
Villaumite, 1- decyl -3- methylimidazoles bromide, 1- decyl -3- methyl imidazolium tetrafluoroborates, 1- decyls
- 3- methylimidazoles hexafluorophosphate, 1- decyl -3- methylimidazole perchlorates, 1- decyl -3- methyl
Imidazoles toluenesulfonate, 1- dodecyl -3- methylimidazole villaumites, 1- dodecyl -3- first
Base imidazoles bromide, 1- dodecyl -3- methyl imidazolium tetrafluoroborates, 1- dodecyl -3- methyl
Limidazolium hexafluorophosphate, 1- dodecyl -3- methylimidazole perchlorates, 1- myristyl -3- first
Base imidazoles bromide, 1- myristyl -3- methyl imidazolium tetrafluoroborates, 1- myristyl -3- methyl
Limidazolium hexafluorophosphate, 1- myristyl -3- methylimidazole perchlorates, 1- cetyl -3- first
Base imidazoles bromide, 1- cetyl -3- methylimidazoles hexafluorophosphate, 1- cetyl -3- methyl
Imidazoles perchlorate, 1- cetyl -3- methyl imidazolium tetrafluoroborates；
The tri-substituted imidazole class ionic liquid is 1- butyl -2,3- methylimidazoles villaumite, 1- butyl
- 2,3- methylimidazoles bromide, 1- butyl -2,3- methylimidazoles tetrafluoroborate, 1- butyl -2,3-
Methylimidazole hexafluorophosphate, 1- butyl -2,3- methylimidazoles nitrate, 1- butyl -2,3- two
Methylimidazole perchlorate, 1- butyl -2,3- methylimidazoles toluenesulfonate, 1- butyl
- 2,3- methylimidazoles disulfate, 1- butyl -2,3- methylimidazoles dihydric phosphate, 1- hexyls
- 2,3- methylimidazoles villaumite, 1- hexyl -2,3- methylimidazoles bromide, 1- hexyl -2,3- dimethyl
Tetrafluoroborate, 1- hexyl -2,3- methylimidazoles hexafluorophosphate, 1- hexyl -2,3- diformazans
Base imidazoles perchlorate；
The pyridine ionic liquid be N- butyl-pyridiniums bromide, N- butyl-pyridiniums tetrafluoroborate,
N- butyl-pyridiniums hexafluorophosphate, N- butyl-pyridiniums perchlorate, N- butyl-pyridiniums are to methylbenzene
Sulfonate, N- hexyl pyridines bromide, N- hexyl pyridinium tetrafluoroborates salt, N- hexyl pyridine hexafluoros
Phosphate, N- octylpyridiniums bromide, N- octylpyridiniums tetrafluoroborate, N- octylpyridinium hexafluoros
Phosphate, pyrrolidines, N- butyl-N- crassitudes bromide, N- butyl-N- methylpyrroles
Alkane tetrafluoroborate, N- butyl-N- crassitude hexafluorophosphates；
The sulfonic acid funtionalized class ionic liquid is 1- propyl sulfonic acid -3- methylimidazoles inner salt, 1- third
Base sulfonic acid -3- methylimidazolium hydrogen sulphates salt, pyridine-sulfonic acid propiolactone, N- propyl sulfonic acid pyridine sulfuric acid
Hydrogen salt, N- propyl sulfonic acid -3- picoline tosilate；
The hydroxy functionalized class ionic liquid is trimethyl hydroxyethylammonium ammonium tetrafluoroborate, 1- hydroxyl second
Base -3- methylimidazole villaumites, 1- ethoxy -3- methyl imidazolium tetrafluoroborates, 1- ethoxy -3- first
Base limidazolium hexafluorophosphate, 1- ethoxy -3- methylimidazoles toluenesulfonate, 1- ethoxys -3-
Methylimidazolium hydrogen sulphate salt, 1- ethoxy -2,3- methylimidazoles villaumite, 1,2- dimethyl -3- hydroxyl second
Base tetrafluoroborate, 1,2- dimethyl -3- hydroxyethyl imidazoles hexafluorophosphate, 1,2- dimethyl
- 3- hydroxyethyl imidazoles perchlorate, 1,2- dimethyl -3- hydroxyethyl imidazoles toluenesulfonate,
1,2- dimethyl -3- hydroxyethyl imidazole disulfates；
The alkenyl functionalization class ionic liquid is 1- pi-allyl -3- methylimidazole villaumites, 1- allyls
Base -3- methyl imidazolium tetrafluoroborates, 1- pi-allyl -3- methylimidazoles hexafluorophosphate, 1- allyls
Base -3- methylimidazoles tosilate, 1- vinyl -3- ethyl imidazol(e)s bromide, 1- vinyl -3-
Ethyl imidazol(e) tetrafluoroborate, 1- vinyl -3- ethyl imidazol(e)s hexafluorophosphate, 1- vinyl -3-
Butyl imidazole villaumite, 1- vinyl -3- butyl imidazoles bromide, 1- vinyl -3- butyl imidazole tetrafluoros
Borate, 1- vinyl -3- butyl imidazole hexafluorophosphates；
The benzyl functionalization class ionic liquid is 1- benzyl -3- methylimidazole villaumites, 1- benzyls -3-
Methyl imidazolium tetrafluoroborate, 1- benzyl -3- methylimidazoles hexafluorophosphate, 1- benzyl -3- methyl
Imidazoles tosilate；
The carboxyl-functional class ionic liquid is 1- carboxymethyl -3- methylimidazole villaumites, 1- carboxylic first
Base -3- methylimidazolium hydrogen sulphates salt, 1- carboxyethyl -3- methylimidazole villaumites；
The ester group functionalization class ionic liquid is 1- ethyl acetate base -3- methylimidazole villaumites, 1-
Ethyl acetate base -3- methyl imidazolium tetrafluoroborates, 1- ethyl acetate base -3- methylimidazole hexafluoro phosphorus
Hydrochlorate, 1- ethyl acetate base -3- methylimidazolium hydrogen sulphates salt, 1- ethylacrylate methyl -3- methylimidazole chlorine
Salt, 1- ethylacrylate methyl -3- methyl imidazolium tetrafluoroborates, 1- ethylacrylate methyl -3- methylimidazole hexafluoros
Phosphate；
The guanidine ionic liquid is TMG hydrochloride, TMG disulfate, tetramethyl
Base guanidine nitrate, TMG borofluoride, TMG acetate, TMG lactate,
TMG dihydric phosphate.
6. ultralow mercuric chloride catalyst according to claim 1 and 2, it is characterised in that use
In 1~5 times that the water of dissolving major catalyst, co-catalyst and auxiliary agent is carrier water absorption rate.
7. a kind of method of the ultralow mercuric chloride catalyst prepared as described in claim 1~6 is any,
Methods described comprises the following steps：
1) appropriate major catalyst, co-catalyst and auxiliary agent are weighed.
2) at a temperature of 40-90 DEG C, major catalyst, co-catalyst and auxiliary agent are dissolved and is being gone
In ionized water and stir, obtain mixed solution；And
3) it is sufficiently impregnated on carrier with the mixed solution, then the carrier after dipping is dried；
Wherein, the carrier is activated carbon, and the major catalyst is mercury chloride, the co-catalysis
Agent be bismuth chloride, cerium chloride, stannous chloride, copper chloride, potassium chloride, lanthanum chloride, manganese chloride,
One or more in stannic chloride, zinc chloride, silver chlorate and iron chloride；The auxiliary agent is ion
Liquid, including disubstituted imidazole class ionic liquid, tri-substituted imidazole class ionic liquid, pyridines
Ionic liquid, sulfonic acid funtionalized class ionic liquid, hydroxy functionalized class ionic liquid, alkenyl work(
Can change class ionic liquid, benzyl functionalization class ionic liquid, carboxyl-functional class ionic liquid,
Ester group functionalization class ionic liquid or guanidine ionic liquid.
8. method according to claim 7, it is characterised in that the temperature of the drying is
80-150℃。
9. method according to claim 7, it is characterised in that the content of the carrier
40~98wt.%.The content of the major catalyst is in 2~4wt.%, the content of the co-catalyst
1~45wt.%, the 1~40wt.% of content of the ionic liquid.
10. the method according to claim 7,8 or 9, it is characterised in that the activity
Charcoal is coconut husk activated carbon, coal mass active carbon, wood activated charcoal, MCM-41 or MCM-13X；
The disubstituted imidazole class ionic liquid is 1- ethyl-3-methylimidazoles bromide, 1- ethyls -3-
Methylimidazole salt compounded of iodine, 1- ethyl-3-methylimidazoles tetrafluoroborate, 1- ethyl-3-methylimidazoles six
Fluorophosphate, 1- ethyl-3-methylimidazole ethyl-sulfates salt, 1- ethyl-3-methylimidazole di(2-ethylhexyl)phosphates
Ethyl ester salt, 1- ethyl-3-methylimidazoles perchlorate, 1- ethyl-3-methylimidazoles rhodanate,
1- ethyl-3-methylimidazoles toluenesulfonate, 1- propyl group -3- methylimidazole villaumites, 1- propyl group -3-
Methylimidazole bromide, 1- propyl group -3- methylimidazoles salt compounded of iodine, 1- propyl group -3- methylimidazole tetrafluoro boric acids
Salt, 1- propyl group -3- methylimidazoles hexafluorophosphate, 1- butyl -3- methylimidazole villaumites, 1- butyl -3-
Methylimidazole bromide, 1- butyl -3- methylimidazoles salt compounded of iodine, 1- butyl -3- methylimidazole tetrafluoro boric acids
Salt, 1- butyl -3- methylimidazoles hexafluorophosphate, 1- butyl -3- methylimidazolium nitrates, 1- butyl
- 3- methylimidazole perchlorates, 1- butyl -3- methylimidazoles toluenesulfonate, 1- butyl -3-
Methylimidazole dihydric phosphate, 1- butyl -3- methylimidazolium hydrogen sulphates salt, 1- butyl -3- methyl miaows
Azoles rhodanate, 1- butyl -3- methylimidazoles acetate, 1- amyl group -3- methylimidazole villaumites, 1-
Amyl group -3- methylimidazoles bromide, 1- amyl group -3- methyl imidazolium tetrafluoroborates, 1- amyl group -3- methyl
Limidazolium hexafluorophosphate, 1- amyl group -3- methylimidazole perchlorates, 1- hexyl -3- methylimidazole chlorine
Salt, 1- hexyl -3- methylimidazoles bromide, 1- hexyl -3- methyl imidazolium tetrafluoroborates, 1- hexyls -3-
Methylimidazole hexafluorophosphate, 1- hexyl -3- methylimidazole perchlorates, 1- hexyl -3- methyl miaows
Azoles toluenesulfonate, 1- hexyl -3- methylimidazolium hydrogen sulphates salt, 1- octyl group -3- methylimidazoles
Bromide, 1- octyl group -3- methylimidazole villaumites, 1- octyl group -3- methyl imidazolium tetrafluoroborates, 1- octyl groups
- 3- methylimidazoles hexafluorophosphate, 1- octyl group -3- methylimidazolium hydrogen sulphates salt, 1- octyl group -3- methyl
Imidazoles perchlorate, 1- octyl group -3- methylimidazoles toluenesulfonate, 1- decyl -3- methyl miaows
Azoles villaumite, 1- decyl -3- methylimidazoles bromide, 1- decyl -3- methyl imidazolium tetrafluoroborates, 1-
Decyl -3- methylimidazoles hexafluorophosphate, 1- decyl -3- methylimidazole perchlorates, 1- decyls -3-
Methylimidazole toluenesulfonate, 1- dodecyl -3- methylimidazole villaumites, 1- dodecyls -3-
Methylimidazole bromide, 1- dodecyl -3- methyl imidazolium tetrafluoroborates, 1- dodecyl -3- first
Base limidazolium hexafluorophosphate, 1- dodecyl -3- methylimidazole perchlorates, 1- myristyls -3-
Methylimidazole bromide, 1- myristyl -3- methyl imidazolium tetrafluoroborates, 1- myristyl -3- first
Base limidazolium hexafluorophosphate, 1- myristyl -3- methylimidazole perchlorates, 1- cetyls -3-
Methylimidazole bromide, 1- cetyl -3- methylimidazoles hexafluorophosphate, 1- cetyl -3- first
Base imidazoles perchlorate, 1- cetyl -3- methyl imidazolium tetrafluoroborates；
The tri-substituted imidazole class ionic liquid is 1- butyl -2,3- methylimidazoles villaumite, 1- butyl
- 2,3- methylimidazoles bromide, 1- butyl -2,3- methylimidazoles tetrafluoroborate, 1- butyl -2,3-
Methylimidazole hexafluorophosphate, 1- butyl -2,3- methylimidazoles nitrate, 1- butyl -2,3- two
Methylimidazole perchlorate, 1- butyl -2,3- methylimidazoles toluenesulfonate, 1- butyl
- 2,3- methylimidazoles disulfate, 1- butyl -2,3- methylimidazoles dihydric phosphate, 1- hexyls
- 2,3- methylimidazoles villaumite, 1- hexyl -2,3- methylimidazoles bromide, 1- hexyl -2,3- dimethyl
Tetrafluoroborate, 1- hexyl -2,3- methylimidazoles hexafluorophosphate, 1- hexyl -2,3- diformazans
Base imidazoles perchlorate；
The pyridine ionic liquid be N- butyl-pyridiniums bromide, N- butyl-pyridiniums tetrafluoroborate,
N- butyl-pyridiniums hexafluorophosphate, N- butyl-pyridiniums perchlorate, N- butyl-pyridiniums are to methylbenzene
Sulfonate, N- hexyl pyridines bromide, N- hexyl pyridinium tetrafluoroborates salt, N- hexyl pyridine hexafluoros
Phosphate, N- octylpyridiniums bromide, N- octylpyridiniums tetrafluoroborate, N- octylpyridinium hexafluoros
Phosphate, pyrrolidines, N- butyl-N- crassitudes bromide, N- butyl-N- methylpyrroles
Alkane tetrafluoroborate, N- butyl-N- crassitude hexafluorophosphates；
The sulfonic acid funtionalized class ionic liquid is 1- propyl sulfonic acid -3- methylimidazoles inner salt, 1- third
Base sulfonic acid -3- methylimidazolium hydrogen sulphates salt, pyridine-sulfonic acid propiolactone, N- propyl sulfonic acid pyridine sulfuric acid
Hydrogen salt, N- propyl sulfonic acid -3- picoline tosilate；
The hydroxy functionalized class ionic liquid is trimethyl hydroxyethylammonium ammonium tetrafluoroborate, 1- hydroxyl second
Base -3- methylimidazole villaumites, 1- ethoxy -3- methyl imidazolium tetrafluoroborates, 1- ethoxy -3- first
Base limidazolium hexafluorophosphate, 1- ethoxy -3- methylimidazoles toluenesulfonate, 1- ethoxys -3-
Methylimidazolium hydrogen sulphate salt, 1- ethoxy -2,3- methylimidazoles villaumite, 1,2- dimethyl -3- hydroxyl second
Base tetrafluoroborate, 1,2- dimethyl -3- hydroxyethyl imidazoles hexafluorophosphate, 1,2- dimethyl
- 3- hydroxyethyl imidazoles perchlorate, 1,2- dimethyl -3- hydroxyethyl imidazoles toluenesulfonate,
1,2- dimethyl -3- hydroxyethyl imidazole disulfates；
The alkenyl functionalization class ionic liquid is 1- pi-allyl -3- methylimidazole villaumites, 1- allyls
Base -3- methyl imidazolium tetrafluoroborates, 1- pi-allyl -3- methylimidazoles hexafluorophosphate, 1- allyls
Base -3- methylimidazoles tosilate, 1- vinyl -3- ethyl imidazol(e)s bromide, 1- vinyl -3-
Ethyl imidazol(e) tetrafluoroborate, 1- vinyl -3- ethyl imidazol(e)s hexafluorophosphate, 1- vinyl -3-
Butyl imidazole villaumite, 1- vinyl -3- butyl imidazoles bromide, 1- vinyl -3- butyl imidazole tetrafluoros
Borate, 1- vinyl -3- butyl imidazole hexafluorophosphates；
The benzyl functionalization class ionic liquid is 1- benzyl -3- methylimidazole villaumites, 1- benzyls -3-
Methyl imidazolium tetrafluoroborate, 1- benzyl -3- methylimidazoles hexafluorophosphate, 1- benzyl -3- methyl
Imidazoles tosilate；
The carboxyl-functional class ionic liquid is 1- carboxymethyl -3- methylimidazole villaumites, 1- carboxylic first
Base -3- methylimidazolium hydrogen sulphates salt, 1- carboxyethyl -3- methylimidazole villaumites；
The ester group functionalization class ionic liquid is 1- ethyl acetate base -3- methylimidazole villaumites, 1-
Ethyl acetate base -3- methyl imidazolium tetrafluoroborates, 1- ethyl acetate base -3- methylimidazole hexafluoro phosphorus
Hydrochlorate, 1- ethyl acetate base -3- methylimidazolium hydrogen sulphates salt, 1- ethylacrylate methyl -3- methylimidazole chlorine
Salt, 1- ethylacrylate methyl -3- methyl imidazolium tetrafluoroborates, 1- ethylacrylate methyl -3- methylimidazole hexafluoros
Phosphate；
The guanidine ionic liquid is TMG hydrochloride, TMG disulfate, tetramethyl
Base guanidine nitrate, TMG borofluoride, TMG acetate, TMG lactate,
TMG dihydric phosphate.
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| CN109499617A (en) * | 2018-12-05 | 2019-03-22 | 安徽华塑股份有限公司 | A kind of no mercury catalyst and its production method |
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| CN101716528A (en) * | 2009-10-30 | 2010-06-02 | 于志勇 | Catalyst system of chloroethylene prepared by hydrochlorinating acetylene and preparation method and application thereof |
| CN102671701A (en) * | 2011-12-08 | 2012-09-19 | 河南科技大学 | Catalyst for synthesizing vinyl chloride monomer and preparation method thereof |
| CN105148989A (en) * | 2015-07-28 | 2015-12-16 | 浙江工业大学 | Porous solid material supported ionic liquid-gold catalyst, as well as preparation and application thereof |
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| CN101716528A (en) * | 2009-10-30 | 2010-06-02 | 于志勇 | Catalyst system of chloroethylene prepared by hydrochlorinating acetylene and preparation method and application thereof |
| CN102671701A (en) * | 2011-12-08 | 2012-09-19 | 河南科技大学 | Catalyst for synthesizing vinyl chloride monomer and preparation method thereof |
| CN105148989A (en) * | 2015-07-28 | 2015-12-16 | 浙江工业大学 | Porous solid material supported ionic liquid-gold catalyst, as well as preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109499617A (en) * | 2018-12-05 | 2019-03-22 | 安徽华塑股份有限公司 | A kind of no mercury catalyst and its production method |
| CN114849791A (en) * | 2022-04-18 | 2022-08-05 | 内蒙古圣龙大地科技有限公司 | Process system of mercury-free catalyst for synthesizing chloroethylene |
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