CN103551139B - Ultralow mercury catalyst and production technology thereof - Google Patents
Ultralow mercury catalyst and production technology thereof Download PDFInfo
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Abstract
A kind of ultralow mercury catalyst is with carbon tetrachloride absorption>=70%, iodine number>=1000mg/g, moisture content≤5%, ash≤7%, mechanical strength>=95%, bulk density 360 ~ 420g/l, granularity 2.5 ~ 4.0mm, specific area 1000 ~ 1800m
2the wood activated charcoal of/g is carrier, the adsorbing chlorinated mercury in center, collaborative promoter zinc chloride, barium chloride, potassium chloride, bismuth chloride are made, though Hg chloride content only 0.5 ~ 4.0%, but because it occupies in activated carbon adsorptive capacity and the stronger center of reactivity, and due to the wood activated charcoal that the active carbon adding active component bismuth chloride and employing is superelevation voidage, also add collaborative promoter makes active carbon and mercury chloride give play to huge synergy simultaneously, and thus this catalyst has longer service life and higher activity.
Description
Technical field
The present invention relates to mercury catalyst and production technology thereof, particularly a kind of ultralow mercury catalyst and production technology thereof that a kind of acetylene gas and hydrogen chloride gas carry out addition reaction synthesizing chloroethylene.
Background technology
Polyvinyl chloride (PVC) is a kind of superior performance, broad-spectrum synthetic resin, the aggregated capacity of China PVC in 2012 is 2,300 ten thousand tons, but the national conditions of oil-poor, weak breath and coal resource relative abundance, determine China PVC produce raw material---vinyl chloride is so far still based on carbide acetylene method production, and current calcium carbide process PVC accounts for more than 80% of China PVC aggregated capacity.Calcium carbide process PVC investment of production is few, technique relative maturity, thus we believe within the quite a long time from now on it will is the prevailing technology that China's PVC Industry develops, but calcium carbide process PVC production technology also also exists many deficiencies, the most fatal be exactly as PVC raw materials for production---vinyl chloride produces necessary mercury catalyst (mercury catalyst), one is produce mercury catalyst need consume a large amount of mercury chloride, and as the mercury of mercury chloride raw materials for production, Domestic Resources is day by day deficient; Two is in use, and mercury chloride pollution on the environment is very serious.
It take active carbon as carrier that above-mentioned vinyl chloride produces necessary mercury catalyst, soak with mercuric chloride solution and make, be commonly called as " mercury catalyst ", its Hg chloride content is up to 10 ~ 15%, and in actual production, often produce one ton of polyvinyl chloride high mercury catalyst 1.2 ~ 1.5kg of wanting mean consumption such, within 2012, China's calcium carbide process PVC produces consumption 1200 ~ 1500 tons, mercury chloride, this wherein 50% mercury chloride cannot reclaim.China was once third place in the world great Chan Gong state, but mercury resource is exhausted now, can adopt without mercury, maintained supply reluctantly every year by import and recovery.Mercury or a global pollutant, by the Medium Propagation such as air, water, mobility is very strong, after settling, be further converted to methyl mercury, the harm caused human health and environment is very serious, and thus international community all pays close attention: the annual mercury emission of the U.S. will control in the scope of 10 ~ 15 tons through legislation; European Union forbade that mercury exported from 2011; In February, 2009 holds United Nations Environment Programme's conference at ministerial level in Nairobi, Kenya capital, and the nearly all country in the whole world has all participated in current meeting, and signs the global treaty of an alleviation mercury pollution; " instruction about strengthening the control of PVC Industry mercury pollution " that at the end of 2009, association of Sinopec, Chinese chlorine industry association, China Chemical Industry Epa draft jointly formulates target " China's PVC Industry all used low mercury catalyst in 2015; the useless mercury catalyst rate of recovery reaches 100% ", as above-mentioned target can not be realized as scheduled, under the pressure of international convention and Domestic Environment policy, there is the calcium carbide process PVC production industry of China's characteristic cannot continue survival.The final outlet of calcium carbide process PVC production industry is in the appearance without mercury catalyst, but even to this day, research and development without mercury catalyst not yet make great progress, the use amount of mercury can only be lowered at present, control in the scope required by policy, and the mercury reclaimed as much as possible in useless mercury catalyst, while minimizing mercury pollution, ensure the raw material supply of mercury, change space with the time, like this, the life of calcium carbide process PVC production industry just can continue, but up to the present, have not yet to see the progress report of industrial value.
We are according to the experience of long-term production mercuric chloride catalyst, and learn through concentrating on studies on this basis: the active carbon of superelevation voidage carries out addition reaction synthesizing chloroethylene to acetylene gas and hydrogen chloride gas inherently higher activity and selectivity, huge synergy will have been given play to together with zinc chloride again with a small amount of mercury chloride, play the effect that high Hg chloride content catalyst can play, and add a small amount of other compound barium chloride and potassium chloride again, can also greatly improve its mechanical performance, extend its service life.By a large amount of experiments with update, we develop Hg chloride content only 0.5 ~ 4.0% ultralow mercury catalyst, through on probation on commercial plant, have received good result.
Summary of the invention
Technical problem to be solved by this invention overcomes above-mentioned the deficiencies in the prior art, and the ultralow mercury catalyst providing a kind of acetylene gas and hydrogen chloride gas to carry out addition reaction synthesizing chloroethylene and production technology thereof.
The present invention solves the technical scheme that its technical problem takes: a kind of acetylene gas and hydrogen chloride gas carry out the ultralow mercury catalyst of addition reaction synthesizing chloroethylene, and it is with carbon tetrachloride absorption>=70%, iodine number>=1000mg/g, moisture content≤5%, ash≤7%, mechanical strength>=95%, bulk density 360 ~ 420g/l, granularity 2.5 ~ 4.0mm, specific area 1000 ~ 1800m
2the wood activated charcoal of/g is carrier, and the adsorbing chlorinated mercury in center, collaborative promoter zinc chloride, barium chloride, potassium chloride, bismuth chloride are made, and by weight percentage, its chloride containing mercury 0.5 ~ 4.0%, is preferably 2.5 ~ 3.7%; Containing Zinc Chloride 2 ~ 10%, barium chloride 2 ~ 10%, potassium chloride 2 ~ 10%, bismuth chloride 2 ~ 10%, concrete production technology is:
1, preparing mass fraction with high purity hydrochloric acid and desalted water is the hydrochloric acid solution of 0.1 ~ 5%, for subsequent use;
2, put into by selected wood activated charcoal in the hydrochloric acid solution that step 1 prepares and soak, preferably soak 20 ~ 60 minutes, period makes hydrochloric acid solution constantly flow, and then takes out to be filtered dry, to be dried to moisture less than 3%;
3, with mercury chloride, hydrochloric acid and desalted water preparation mass fraction be 2 ~ 5%, the mercury chloride hydrochloric acid solution of pH≤3, and the weight ratio of the ultralow mercury catalyst pressing preparation other material contained and mercury chloride contained by it, add appropriate collaborative promoter zinc chloride, barium chloride, potassium chloride, bismuth chloride, for subsequent use;
4, the active carbon being finally dried to moisture less than 3% by soaking through step 2 is put in the mercury chloride hydrochloric acid solution that step 3 prepares, soak 4 ~ 10 hours under the temperature conditions of 50 ~ 98 DEG C, period makes mercury chloride hydrochloric acid solution constantly flow, then take out and be filtered dry, put into baking oven, moisture less than 0.3% is dried under the temperature conditions of 100 ~ 140 DEG C, namely selected wood activated charcoal first time adsorbing chlorinated mercury work is completed, then the active carbon having adsorbed a mercury chloride is put into again in the mercury chloride hydrochloric acid solution that step 3 prepares, soak 2 ~ 5 hours under the temperature conditions of 50 ~ 98 DEG C, and other operation repeated in first time adsorbing chlorinated mercury process, the selected adsorbing chlorinated mercury work of wood activated charcoal second time can be completed, then again the active carbon third time of having adsorbed secondary mercury chloride is put in the mercury chloride hydrochloric acid solution that step 3 prepares, soak 2 ~ 5 hours under the temperature conditions of 50 ~ 98 DEG C, and other operation repeated in the adsorbing chlorinated mercury process of second time, namely three the adsorbing chlorinated mercury work of selected wood activated charcoal is completed, make the selected adsorbing chlorinated mercury in wood activated charcoal center, obtained ultralow mercury catalyst by weight percentage, chloride containing mercury 0.5 ~ 4.0%, zinc chloride 2 ~ 10%, barium chloride 2 ~ 10%, potassium chloride 2 ~ 10%, bismuth chloride 2 ~ 10%.
This acetylene gas provided by the present invention and hydrogen chloride gas carry out the mercury catalyst of addition reaction synthesizing chloroethylene, Hg chloride content is ultralow, though only 0.5 ~ 4.0%, but because it occupies in activated carbon adsorptive capacity and the stronger center of reactivity, and due to the wood activated charcoal that the active carbon adding active component bismuth chloride and employing is superelevation voidage, also add collaborative promoter makes active carbon and mercury chloride give play to huge synergy simultaneously, catalytic activity is very high, thus this catalyst has longer service life and higher activity, the high mercury catalyst being 10.5 ~ 12.5% with Hg chloride content carries out the VCM synthesis Experimental Comparison under equal operating condition: the two does not have difference in serviceability, but mercury catalyst mercury chloride consumption provided by the present invention is very low, because catalyst Hg chloride content is low and long service life and cause catalyst amount and reduce and then reduce the effect of mercury chloride consumption and vinyl chloride production cost clearly.
Detailed description of the invention
In order to better the present invention is described, enumerate following instance, but scope of the present invention is not limited only to this, its claimed scope is recorded in the claim of claim.
The embodiment of the present invention provides a kind of acetylene gas and hydrogen chloride gas to carry out the ultralow mercury catalyst of addition reaction synthesizing chloroethylene, and it is with 100 kilograms of carbon tetrachloride absorption 110% (GB/T12496-1999), iodine number 1200mg/g (GB/T12496-1999), moisture content 2% (GB/T12496-1999), ash 3% (GB/T12496-1999), mechanical strength 97% (ASTM racket method), bulk density 365g/l (GB/T12496-1999), granularity 2.5 ~ 3.8mm (GB/T12496-1999), specific area 1450m
2/ g(BET method) wood activated charcoal be carrier, the adsorbing chlorinated mercury in center, collaborative promoter zinc chloride, barium chloride, potassium chloride, bismuth chloride are made, by weight percentage, its chloride containing mercury 2.6%, zinc chloride 4%, barium chloride 3.5%, potassium chloride 3.5%, bismuth chloride 3.5%, water 0.27%, mechanical strength 95.6%, granularity 3 ~ 6mm(95%), bulk density 450g/l, mercury chloride burn tinctuer 0.89%, concrete production technology is:
1, prepare with high purity hydrochloric acid and desalted water the hydrochloric acid solution 500 kilograms that mass fraction is 0.1 ~ 5%, normal temperature is placed, for subsequent use;
2, selected 100 kilograms of wood activated charcoals are put in the hydrochloric acid solution that step 1 prepares and soak 20 ~ 60 minutes, period uses circulating pump that hydrochloric acid solution is constantly flowed, and then takes out and filters or be filtered dry with centrifuge drying dehydration, under the temperature conditions of 200 DEG C, be dried to moisture less than 3%;
3, with mercury chloride, hydrochloric acid and desalted water preparation mass fraction be 2 ~ 5%, the mercury chloride hydrochloric acid solution 500 kilograms of pH=3, and the weight ratio of the ultralow mercury catalyst pressing preparation other material contained and mercury chloride contained by it, add appropriate collaborative promoter zinc chloride, barium chloride, potassium chloride, bismuth chloride, for subsequent use;
4, the active carbon being finally dried to moisture less than 3% by soaking through step 2 is put in the mercury chloride hydrochloric acid solution that step 3 prepares, soak 4 ~ 10 hours under the temperature conditions of 50 ~ 98 DEG C, period uses circulating pump that mercury chloride hydrochloric acid solution is constantly flowed, then take out and filter or be filtered dry with centrifuge drying dehydration, put into baking oven, moisture less than 0.3% is dried under the temperature conditions of 100 ~ 140 DEG C, namely selected wood activated charcoal first time adsorbing chlorinated mercury work is completed, then the active carbon having adsorbed a mercury chloride is put into again in the mercury chloride hydrochloric acid solution that step 3 prepares, soak 2 ~ 5 hours under the temperature conditions of 50 ~ 98 DEG C, and other operation repeated in first time adsorbing chlorinated mercury process, the selected adsorbing chlorinated mercury work of wood activated charcoal second time can be completed, then again the active carbon third time of having adsorbed secondary mercury chloride is put in the mercury chloride hydrochloric acid solution that step 3 prepares, soak 2 ~ 5 hours under the temperature conditions of 50 ~ 98 DEG C, and other operation repeated in the adsorbing chlorinated mercury process of second time, namely three the adsorbing chlorinated mercury work of selected wood activated charcoal is completed, make the selected adsorbing chlorinated mercury in wood activated charcoal center, obtained ultralow mercury catalyst by weight percentage, chloride containing mercury 2.6%, zinc chloride 4%, barium chloride 3.5%, potassium chloride 3.5%, bismuth chloride 3.5%, water 0.27%, mechanical strength 95.6%, granularity 3 ~ 6mm(95%), bulk density 450g/l.
This Hg chloride content that the embodiment of the present invention provides be 2.6% ultralow mercury catalyst and existing Hg chloride content be 11.3% high mercury catalyst carry out under equal operating condition VCM synthesis contrast test:
1, test material: the Hg chloride content that the embodiment of the present invention provides be 2.6% the Hg chloride content that obtains of the existing commonsense method of ultralow mercury catalyst be 11.3% high mercury catalyst
2, testing equipment: two shell-and-tube reactors be made up by triangular arranged of 15 φ 50 × 3500 tubulations (between pipe logical water quench)
3, test method:
(1) catalyst is loaded
Check before filling catalyst that reactor is inside and outside without leak source, tubulation inwall is clean, dry, no-sundries; Be encased in immediately after opening catalyst packaging bag in each tubulation of reactor, filling catalyst will complete in 0.5h, guard against damp.
(2) preheating
Pass into the dry HCl of 90 ~ 100 DEG C, speed control 7 ~ 8m
3/ h, continuous 8 ~ 10h, period puts acid once every 2h by reactor bottom.
(3) ratio is controlled in 1:1.1 ~ 1:1.3(100% purity), the chlorination of acetylene hydrogen mixed gas that to reach more than 90 DEG C through preheat temperature passes into reactor, culture period 1 month, regulate acetylene gas intake according to reactor cooling capacity, control temperature is between 110 ~ 125 DEG C; After culture period terminates, regulate acetylene gas intake (30 ~ 50h according to reactor cooling capacity
-1), reaction temperature is controlled at 130 DEG C.Use the Hg chloride content that provides of the embodiment of the present invention be 2.6% each operating procedure of ultralow mercury catalyst and the Hg chloride content that the existing commonsense method of use obtains be 11.3% high mercury catalyst identical, result of the test is in table 1.
Table 1:
From the test data of table 1, although the amount of the ultralow mercury catalyst chloride containing mercury that the embodiment of the present invention provides is ultralow, but test the various performance that reflects with existing high mercury catalyst and indifference, embody that mercury chloride occupies in activated carbon adsorptive capacity and the stronger center of reactivity, the wood activated charcoal of employing high voidage and add zinc chloride and make active carbon and mercury chloride give play to the measures such as huge synergy to carry out the strong concerted catalysis effect of addition reaction synthesizing chloroethylene to acetylene gas and hydrogen chloride gas; The improvement added catalytic mechanical performance of stabilizing agent barium chloride, anti-coking agent potassium chloride.
Claims (3)
1. a ultralow mercury catalyst, is characterized in that: it is with carbon tetrachloride absorption>=70%, iodine number>=1000mg/g, moisture content≤5%, ash≤7%, mechanical strength>=95%, bulk density 360 ~ 420g/l, granularity 2.5 ~ 4.0mm, specific area 1000 ~ 1800m
2the wood activated charcoal of/g is carrier, the adsorbing chlorinated mercury in center, collaborative promoter zinc chloride, barium chloride, potassium chloride, bismuth chloride are made, by weight percentage, its chloride containing mercury 0.5 ~ 4.0%, zinc chloride 2 ~ 10%, barium chloride 2 ~ 10%, potassium chloride 2 ~ 10%, bismuth chloride 2 ~ 10%;
Its production technology is:
(1), with high purity hydrochloric acid and desalted water preparation mass fraction be the hydrochloric acid solution of 0.1 ~ 5%, for subsequent use;
(2), by selected wood activated charcoal put in the hydrochloric acid solution that step (1) prepares and soak, period makes hydrochloric acid solution constantly flow, and then takes out to be filtered dry, to be dried to moisture less than 3%;
(3), with mercury chloride, hydrochloric acid and desalted water preparation mass fraction be 2 ~ 5%, the mercury chloride hydrochloric acid solution of pH≤3, and the weight ratio of the ultralow mercury catalyst pressing preparation other material contained and mercury chloride contained by it, add appropriate collaborative promoter zinc chloride, barium chloride, potassium chloride, bismuth chloride, for subsequent use;
(4), the active carbon being finally dried to moisture less than 3% by soaking through step (2) is put in the mercury chloride hydrochloric acid solution that step (3) prepares, soak 4 ~ 10 hours under the temperature conditions of 50 ~ 98 DEG C, period makes mercury chloride hydrochloric acid solution constantly flow, then take out and be filtered dry, put into baking oven, moisture less than 0.3% is dried under the temperature conditions of 100 ~ 140 DEG C, namely selected wood activated charcoal first time adsorbing chlorinated mercury work is completed, then the active carbon having adsorbed a mercury chloride is put into again in the mercury chloride hydrochloric acid solution that step (3) prepares, soak 2 ~ 5 hours under the temperature conditions of 50 ~ 98 DEG C, and other operation repeated in first time adsorbing chlorinated mercury process, the selected adsorbing chlorinated mercury work of wood activated charcoal second time can be completed, then again the active carbon third time of having adsorbed secondary mercury chloride is put in the mercury chloride hydrochloric acid solution that step (3) prepares, soak 2 ~ 5 hours under the temperature conditions of 50 ~ 98 DEG C, and other operation repeated in the adsorbing chlorinated mercury process of second time, namely three the adsorbing chlorinated mercury work of selected wood activated charcoal is completed, make the selected adsorbing chlorinated mercury in wood activated charcoal center, obtained ultralow mercury catalyst by weight percentage, chloride containing mercury 0.5 ~ 4.0%, zinc chloride 2 ~ 10%, barium chloride 2 ~ 10%, potassium chloride 2 ~ 10%, bismuth chloride 2 ~ 10%.
2. ultralow mercury catalyst according to claim 1, is characterized in that: by weight percentage, its chloride containing mercury 2.5 ~ 3.7%.
3. produce a technique for the ultralow mercury catalyst described in claim 1, it is characterized in that: it is
(1), with high purity hydrochloric acid and desalted water preparation mass fraction be the hydrochloric acid solution of 0.1 ~ 5%, for subsequent use;
(2), by selected wood activated charcoal put in the hydrochloric acid solution that step (1) prepares and soak, period makes hydrochloric acid solution constantly flow, and then takes out to be filtered dry, to be dried to moisture less than 3%;
(3), with mercury chloride, hydrochloric acid and desalted water preparation mass fraction be 2 ~ 5%, the mercury chloride hydrochloric acid solution of pH≤3, and the weight ratio of the ultralow mercury catalyst pressing preparation other material contained and mercury chloride contained by it, add appropriate collaborative promoter zinc chloride, barium chloride, potassium chloride, bismuth chloride, for subsequent use;
(4), the active carbon being finally dried to moisture less than 3% by soaking through step (2) is put in the mercury chloride hydrochloric acid solution that step (3) prepares, soak 4 ~ 10 hours under the temperature conditions of 50 ~ 98 DEG C, period makes mercury chloride hydrochloric acid solution constantly flow, then take out and be filtered dry, put into baking oven, moisture less than 0.3% is dried under the temperature conditions of 100 ~ 140 DEG C, namely selected wood activated charcoal first time adsorbing chlorinated mercury work is completed, then the active carbon having adsorbed a mercury chloride is put into again in the mercury chloride hydrochloric acid solution that step (3) prepares, soak 2 ~ 5 hours under the temperature conditions of 50 ~ 98 DEG C, and other operation repeated in first time adsorbing chlorinated mercury process, the selected adsorbing chlorinated mercury work of wood activated charcoal second time can be completed, then again the active carbon third time of having adsorbed secondary mercury chloride is put in the mercury chloride hydrochloric acid solution that step (3) prepares, soak 2 ~ 5 hours under the temperature conditions of 50 ~ 98 DEG C, and other operation repeated in the adsorbing chlorinated mercury process of second time, namely three the adsorbing chlorinated mercury work of selected wood activated charcoal is completed, make the selected adsorbing chlorinated mercury in wood activated charcoal center, obtained ultralow mercury catalyst by weight percentage, chloride containing mercury 0.5 ~ 4.0%, zinc chloride 2 ~ 10%, barium chloride 2 ~ 10%, potassium chloride 2 ~ 10%, bismuth chloride 2 ~ 10%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104275174A (en) * | 2014-09-17 | 2015-01-14 | 宁夏金海创科化工科技有限公司 | Low-mercury catalyst and preparation method of low-mercury catalyst |
| CN104987439B (en) * | 2015-06-29 | 2017-05-24 | 贵州大龙银星汞业有限责任公司 | Preparation method for ethyne hydrochlorination homogeneous complex catalyst |
| CN105032453B (en) * | 2015-06-29 | 2018-03-09 | 贵州大龙银星汞业有限责任公司 | New low solid mercury catalyst of acetylene hydrochlorination and preparation method thereof |
| CN105195184B (en) * | 2015-10-27 | 2018-07-17 | 宁夏新龙蓝天科技股份有限公司 | A method of low-mercury catalyst is prepared using high mesoporosity activated carbon |
| CN105413719B (en) * | 2015-10-27 | 2018-06-22 | 宁夏新龙蓝天科技股份有限公司 | A kind of method that low-mercury catalyst is prepared using high Penetrating curve activated carbon |
| CN105413746B (en) * | 2015-10-27 | 2018-06-22 | 宁夏新龙蓝天科技股份有限公司 | A kind of preparation of the high ultralow mercury catalyst of catalytic activity and its recovery method |
| CN107321389B (en) * | 2015-10-27 | 2020-05-26 | 宁夏新龙蓝天科技股份有限公司 | Preparation method of ultralow-mercury catalyst for catalytic synthesis of chloroethylene |
| CN105251531B (en) * | 2015-10-27 | 2018-08-24 | 宁夏新龙蓝天科技股份有限公司 | A kind of preparation of ultralow mercury catalyst with long service life and its recovery method |
| CN105195225B (en) * | 2015-10-27 | 2017-11-17 | 宁夏新龙蓝天科技股份有限公司 | A kind of method for preparing low-mercury catalyst using palladium bichloride collaboration accelerator absorption |
| CN105195230B (en) * | 2015-10-27 | 2017-12-26 | 宁夏新龙蓝天科技股份有限公司 | A kind of method that low-mercury catalyst is prepared using high iodine number activated carbon |
| CN110833838A (en) * | 2019-11-18 | 2020-02-25 | 铜仁市万山区昊海化工有限公司 | Ultra-low mercury catalyst and preparation method thereof |
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| US1934324A (en) * | 1931-04-10 | 1933-11-07 | Carbide & Carbon Chem Corp | Preparation of vinyl chloride |
| CN100363101C (en) * | 2006-03-01 | 2008-01-23 | 那风换 | Composite metal chloride catalyst and its production process |
| CN101890360B (en) * | 2010-08-05 | 2012-07-25 | 李伟 | Method for preparing novel catalyst used for hydrochlorination of acetylene |
| CN102125830B (en) * | 2011-01-21 | 2012-09-26 | 李伟 | Mercury-free catalyst for use in production of chloroethylene by calcium carbide method |
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