CN103191760B - A kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst - Google Patents
A kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst Download PDFInfo
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Abstract
The invention discloses a kind of for Acetylene-hydrochlorlow-content low-content gold compound catalyst, particularly a kind of non-mercury catalyst being applicable to acetylene hydrochlorination Reactive Synthesis vinyl chloride, this catalyst comprises carrier active carbon 10000 parts, main catalytic composition is the thiosulfate of gold, main catalytic component content is 1 ~ 120 part, each 50 ~ 1000 parts of auxiliary element A and B, auxiliary element A are the thiosulfate of silver, and auxiliary element B is alkali metal compound and composition thereof.The content of the catalyst compounded middle gold of the prepared gold of the present invention is low, and significantly reducing the cost of noble metal catalyst, is that a kind of activity is good, stability is strong, selective high novel mercury-free catalyst.Have that production technology is simple, with short production cycle, the advantage of environmental protection.
Description
Technical field
The present invention relates to a kind of catalyst, particularly a kind of catalyst being applicable to acetylene hydrochlorination synthesizing chloroethylene.
Background technology
VCM is the important synthesis material of polyvinyl chloride, and polyvinyl chloride is one of maximum synthetic resin of China's consumption and output, and the few oily fundamental realities of the country of the many coals of China determines producing vinyl chloride by acetylene hydrochlorination and still occupies leading status in China.Present the faced subject matter of acetylene hydrochlorination method synthesizing chloroethylene is a large amount of consumption of the environmental pollution that brings of the use of mercury catalyst and mercury resource.Along with day by day strengthening and the international growing tension limitting the negotiation of mercury treaty of people's environmental consciousness, for maintaining the living space of calcium carbide process PVC, the exploitation without mercury catalyst is imperative.
The research and development of current catalyst without mercury are divided into the gentle liquid-phase reaction system of gas-solid phase reaction.Liquid phase reaction refers to catalyst activity component to be dissolved in a certain amount of solvent, passes into the reaction that reacting gas prepares vinyl chloride.The Typical Representative of liquid phase reaction is CN200910236255.7 and CN201010185916.The conversion ratio of the acetylene of current liquid phase reaction is not very high, catalyst system and catalyzing inactivation is very fast, in addition due to the existence of hydrogen chloride, certain corrosion may be caused to equipment, in addition the serial side reaction owing to there occurs in system may cause the problem of practical operation and the enforcement such as to solidify of under normal temperature state liquid phase, and these catalyst system and catalyzings all do not obtain practical application at present.
Gas-solid phase reaction system is then different from liquid phase reaction system completely.Gas-solid phase reaction is by a certain amount of active constituent loading on specific solid phase carrier, then passes into the reaction that reaction gas prepares vinyl chloride.The research of gas-solid phase catalyst without mercury is simple to operate due to it, and existing reaction unit can be utilized directly to carry out reacting etc. becoming current study hotspot.Acetylene hydrochlorination gas-solid phase catalyst without mercury is mainly divided into base metal and noble metal to be main active component both direction.Base metal is due to the cheap common concern being subject to researcher, and wherein CN101497046, CN101671293, CN102151581A are respectively with the catalyst system and catalyzing of the base metals such as Cu, Bi, MoP for main active component, achieve certain achievement.Some base metal catalysts activity is higher, but inactivation is very fast, and the life-span of catalyst is undesirable.
The research of noble metal catalyst aspect also achieves certain progress.Mentioning with 0.5 ~ 3 part of (namely 0.24 ~ 1.43%) palladium, platinum, gold, rhodium chloride in patent CN200810044560.1 is main active component, and in 1 ~ 10 part of stannous chloride, cerium chloride and bismuth chloride, one or more are co-catalyst, at air speed 250 ~ 500h
-1, under the reaction condition that reaction temperature is 110 ~ 160 DEG C, obtain conversion of alkyne 95% ~ 98%, vinyl chloride is selective is greater than 99%.Patent CN 200910196849.X adopts the halide of the gold of 0.1 ~ 10%, complex compound is main active component, adopts the halide of the potassium of 0.1 ~ 10%, barium, lanthanum, copper, acetate, phosphate, complex compound for helping active component, at air speed 50 ~ 200h
-1under, under reaction temperature 120 ~ 180 DEG C of conditions, obtain conversion of alkyne 90% ~ 99%, the selective of vinyl chloride is 97 ~ 99.9%.The main active component of patent CN200910228149.4 is the chloride of 2 ~ 15% palladiums or gold, help active component be 1 ~ 5% rare earth compound, its main feature is adopt the method for two vacuum soakage to prepare noble metal catalyst without mercury, by it at 30 ~ 90h
-1air speed under, 150 DEG C reaction reaction condition under react, obtain conversion of alkyne 98 ~ 99%, selective 98 ~ 99.9% of vinyl chloride.
The gold of the low precious metal content of 0.05 ~ 0.5%, platinum, rhodium, ruthenium, palladium, iridium metals chloride, phosphate, sulfate and oxide is adopted to be main active component in patent CN 201010272612.8, the phosphate of the copper of 0.1 ~ 5%, zinc, potassium, barium, nickel, bismuth, calcium, lithium and rare-earth metal chloride, sulfate and oxide for helping active component, with active carbon, molecular sieve, silica gel, CNT, TiO
2or aluminium oxide is carrier, at 20 ~ 2000h
-1under air speed, under 100 ~ 250 DEG C of reaction temperatures, obtain conversion of alkyne 40 ~ 85%, selective 98 ~ 99% of vinyl chloride.
Patent CN201110150287.2 also uses the chlorauride of the low precious metal content of 0.05 ~ 0.5% or ruthenic chloride is main active component, adopt the chloride of the bismuth, barium, manganese, iron etc. of 0.05 ~ 0.5% for helping active component, take active carbon as carrier, but its feature is that wherein active carbon is washed to pH=4-5 through persalt stir process, re-use modifier ultrasonic process under the condition of 25 ~ 60KHz after drying, modifier is: the ethanol solution of ethamine, ethylenediamine, triethylamine, hexamethylenetetramine, KH-550, KH-560, KH-570 silane coupler.This kind of noble metal catalyst without mercury can obtain the conversion of alkyne of 65 ~ 99%.Adopt respectively in patent CN201110257696.2 and patent CN 201110257697.7 halide of the palladium of 0.1 ~ 5% or complex compound and 0.1 ~ 3% noble metal be active component, carrier is for being respectively molecular sieve HZSM-5, NaZSM-5, H β type and HY type modenite and active carbon, its main feature same is also vehicle treated method: carrier is added pretreating reagent through stirring, dipping, backflow or ultrasonic, then clean to faintly acid.Pretreating reagent is: hydrochloric acid, nitric acid, phosphoric acid, potassium permanganate, hydrogen peroxide, NaOH, potassium hydroxide, ammoniacal liquor, organic acid etc.Under certain air speed and reaction condition, all higher conversion ratio can be obtained.
Patent CN201110199651.4 adopts the chloride of gold element, cobalt element, lanthanum element or nitrate to be active component, auxiliary agent is the chloride of potassium, sodium, bismuth, iron etc., take chloroazotic acid as the equipment of dipping liquid noble metal catalyst without mercury, wherein the content of Precious Metals-Gold is 0.3 ~ 2%.Be wherein 0.3% content at gold, employing molecular sieve is carrier, at 12h
-1air speed under maintain conversion of alkyne reach 970h more than 99%.
The main active component of precious metal element gold as catalyst is all have employed in these several patents.In the last few years, because the catalytic activity of Precious Metals-Gold is high, catalysis scope extensively becomes the study hotspot of industry, also make some progress, obtain good conversion ratio, but in acetylene hydrochlorination reaction system, because acetylene has higher reproducibility, easily make the Au in main active component in catalyst
3+and Au
+be transformed into Au
0thus result in the inactivation of catalyst, so although the catalytic activity of Precious Metals-Gold catalyst is high, but its less stable, life-span is shorter, and adding the scope that in noble metal catalyst without mercury, gold content covers is 0.05 ~ 15%, all higher, the cost of Precious Metals-Gold catalyst without mercury is remained high, is difficult to obtain commercial Application in acetylene hydrochlorination.
Summary of the invention
The object of the invention is to solve in carbide acetylene method Production of PVC and uses highly toxic mercury catalyst, in production, mercury consumption is large, environmental pollution is serious, existing noble metal catalyst less stable, the problem that cost is high, and then it is good to provide a kind of catalytic activity, selective height, bullion content low (being low to moderate less than 0.5%), the one that catalyst cost is low is used for Acetylene-hydrochlorlow-content low-content gold compound catalyst.
A kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, comprise the component of following content: carrier active carbon 10000 parts, main catalytic composition composite metal salt 1 ~ 120 part, each 50 ~ 1000 parts of auxiliary element A and B, main catalytic composition is the compound of gold, auxiliary element A is the compound of silver, and auxiliary element B is alkali metal compound or its mixture.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, its main catalytic composition is the thiosulfate of gold.Its Main Function is the sodium byposulfite stable complex ion forming gold, makes gold ion be not easy to be reduced.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, its auxiliary element A is the thiosulfate of silver.Its Main Function selects the same main group compound silver with similar electronic structure as composite component, and the thiosulfate complexes of silver, make activity component impregnation evenly, gold and the composite of silver have certain synergy simultaneously.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, its auxiliary element B is potassium chloride.Its Main Function selects alkali metal compound, alkali metal compound has the effect of certain anti-carbon deposit, what make active component disperse is more tiny homogeneous simultaneously, increase the decentralization of active component, and the coalescence inactivation of active component can also be prevented in course of reaction, therefore auxiliary element potassium chloride add the stability that can improve catalyst further.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, its auxiliary element B is cesium chloride.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, first it prepare certain density chlorauric acid solution, then it is for subsequent use to prepare certain density hypo solution; Take a certain amount of chlorauric acid solution, add the dilution of a certain amount of deionized water; Take a certain amount of silver salt again and stir; Then add a certain amount of hypo solution to stir; Last take a certain amount of auxiliary element B again and add in above-mentioned solution and stir, in this solution, add active carbon, impregnation drying.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, the mass percent concentration of its thiosulfate solution is 3 ~ 35.6%, forms the stable complex ion of the thiosulfate of gold.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, its dip time is 4-24h, and baking temperature is 60-180 DEG C.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, the carrier active carbon specific area described in it is 800 ~ 3500m
2/ g, micropore ratio>=50% of carrier.Adopt the active carbon of bigger serface, active component is disperseed evenly, increasing the decentralization of active component, when ensure that the avtive spot of catalyst, greatly reducing gold content.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, its thiosulfate solution can be ammonia thiosulfate or potassium thiosulfate.
Described a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, its auxiliary element B can be alkaline earth metal compound, rare earth compound and composition thereof.
First the present invention adopts S
2o
3 2-and Au
3+complexing forms the stable [Au (S with δ-Π feedback bonding
2o
3)
2]
3-complex ion, makes the Au in main active component
+more difficultly to be reduced; Secondly, the thiosulfate complexes [Ag (S of same main group transistion metal compound silver is adopted
2o
3)
2]
3-and alkali metal compound potassium chloride and cesium chloride are composite component, wherein silver not only has similar electronic structure with gold, and has similar complex structure, can activity component impregnation be made evenly, gold and the composite of silver have certain synergy simultaneously, can improve the conversion ratio of catalyst; Composite with alkali metal potassium chloride and cesium chloride again, what can active component particles be made further to disperse be more tiny and homogeneous, in this external course of reaction, potassium chloride or cesium chloride adds the effect also playing the coalescence preventing active component, also can play certain anti-carbon effect simultaneously, thus improve the stability of catalyst, the life-span of extending catalyst; Finally adopt the active carbon of bigger serface, active component is disperseed evenly, increasing the decentralization of active component, when ensure that the avtive spot of catalyst, greatly reducing gold content.
The present invention greatly reduces the content of gold under the prerequisite not reducing catalyst activity and stability in sum, and the cost of noble metal catalyst without mercury is reduced greatly.
One provided by the invention is used for Acetylene-hydrochlorlow-content low-content gold compound catalyst, at 12h
-1air speed reaction time, initial conversion can reach 40 ~ 99%, after reaction 4 ~ 15h, conversion ratio still can remain stable, and the selective of vinyl chloride reaches more than 98%, can solve in carbide acetylene method Production of PVC and use highly toxic mercury catalyst, in production, mercury consumption is large, environmental pollution is serious, existing noble metal catalyst less stable, the problem that cost is high, wherein gold accounts for the mass percent of carrier is in 5 ‰ ~ 0.05 ‰ scopes, greatly reduces the cost of Precious Metals-Gold catalyst.
Detailed description of the invention
In order to better the present invention is described, enumerate following instance.But scope of the present invention is also not only confined to example, and its claimed scope is recorded in the claim of claim.
First chlorauric acid solution is prepared: 1g gold chloride is dissolved in 100ml volumetric flask and is mixed with chlorauric acid solution.For subsequent sample preparation is prepared.
Embodiment 1
Weigh Na
2s
2o
3﹒ 5H
2o is 16.9485g, is dissolved in 30ml deionized water, for subsequent use after stirring.Weigh chlorauric acid solution 1.5839g in beaker, in this beaker, add the dilution of 10ml deionized water.Weigh AgNO again
3for 0.6000g adds in the middle of the chlorauric acid solution diluted, after stirring, add hypo solution for subsequent use, be stirred to without precipitation.Finally weigh the KCL of 0.4500g, to join in above-mentioned solution liquid and to stir.Add 15g active carbon in above-mentioned maceration extract, stir, normal temperature dipping 12h, then dry 12h under 105 DEG C of conditions.This catalyst is used in the middle of acetylene hydrochlorination synthesizing chloroethylene, at 12h
-1under air speed, logical nitrogen drying 30min under 180 DEG C of conditions, then logical hydrogen chloride activation 30min, finally passes into acetylene and starts reaction, obtain conversion of alkyne 99%, selective 98% of vinyl chloride.
Embodiment 2
Weigh Na
2s
2o
3﹒ 5H
2o is 155.85g, is dissolved in 30ml deionized water, for subsequent use after stirring.Weigh chlorauric acid solution 15.8390g in beaker, in this beaker, add the dilution of 10ml deionized water.Weigh AgNO again
3for 0.0750g adds in the middle of the chlorauric acid solution diluted, after stirring, add hypo solution for subsequent use, be stirred to without precipitation.Finally weigh the KCL of 1.5000g, to join in above-mentioned solution liquid and to stir.Add 15g active carbon in above-mentioned maceration extract, stir, normal temperature dipping 12h, then dry 12h under 105 DEG C of conditions.This catalyst is used in the middle of acetylene hydrochlorination synthesizing chloroethylene, at 12h
-1under air speed, logical nitrogen drying 30min under 180 DEG C of conditions, then logical hydrogen chloride activation 30min, finally passes into acetylene and starts reaction, obtain conversion of alkyne 99.8%, selective 99% of vinyl chloride.
Embodiment 3
Weigh Na
2s
2o
3﹒ 5H
2o is 5.0079g, is dissolved in 30ml deionized water, for subsequent use after stirring.Weigh chlorauric acid solution 0.1584g in beaker, in this beaker, add the dilution of 10ml deionized water.Weigh AgNO again
3for 1.5000g adds in the middle of the chlorauric acid solution diluted, after stirring, add hypo solution for subsequent use, be stirred to without precipitation.Finally weigh the KCL of 0.1500g, to join in above-mentioned solution liquid and to stir.Add 15g active carbon in above-mentioned maceration extract, stir, normal temperature dipping 12h, then dry 12h under 105 DEG C of conditions.This catalyst is used in the middle of acetylene hydrochlorination synthesizing chloroethylene, at 12h
-1under air speed, logical nitrogen drying 30min under 180 DEG C of conditions, then logical hydrogen chloride activation 30min, finally passes into acetylene and starts reaction, obtain conversion of alkyne 45%, selective 98% of vinyl chloride.
Embodiment 4
Weigh Na
2s
2o
3﹒ 5H
2o is 16.9485g, is dissolved in 30ml deionized water, for subsequent use after stirring.Weigh chlorauric acid solution 1.5839g in beaker, in this beaker, add the dilution of 10ml deionized water.Weigh AgNO again
3for 0.6000g adds in the middle of the chlorauric acid solution diluted, after stirring, add hypo solution for subsequent use, be stirred to without precipitation.Finally weigh the CsCL of 0.4500g, to join in above-mentioned solution liquid and to stir.Add 15g active carbon in above-mentioned maceration extract, stir, normal temperature dipping 12h, then dry 12h under 105 DEG C of conditions.This catalyst is used in the middle of acetylene hydrochlorination synthesizing chloroethylene, at 12h
-1under air speed, logical nitrogen drying 30min under 180 DEG C of conditions, then logical hydrogen chloride activation 30min, finally passes into acetylene and starts reaction, obtain conversion of alkyne 95%, selective 98% of vinyl chloride.
Embodiment 5
Weigh Na
2s
2o
3﹒ 5H
2o is 155.85g, is dissolved in 30ml deionized water, for subsequent use after stirring.Weigh chlorauric acid solution 15.8390g in beaker, in this beaker, add the dilution of 10ml deionized water.Weigh AgNO again
3for 0.0750g adds in the middle of the chlorauric acid solution diluted, after stirring, add hypo solution for subsequent use, be stirred to without precipitation.Finally weigh the CsCL of 1.5000g, to join in above-mentioned solution liquid and to stir.Add 15g active carbon in above-mentioned maceration extract, stir, normal temperature dipping 12h, then dry 12h under 105 DEG C of conditions.This catalyst is used in the middle of acetylene hydrochlorination synthesizing chloroethylene, at 12h
-1under air speed, logical nitrogen drying 30min under 180 DEG C of conditions, then logical hydrogen chloride activation 30min, finally passes into acetylene and starts reaction, obtain conversion of alkyne 99%, selective 99% of vinyl chloride.
Embodiment 6
Weigh Na
2s
2o
3﹒ 5H
2o is 5.0079g, is dissolved in 30ml deionized water, for subsequent use after stirring.Weigh chlorauric acid solution 0.1584g in beaker, in this beaker, add the dilution of 10ml deionized water.Weigh AgNO again
3for 1.5000g adds in the middle of the chlorauric acid solution diluted, after stirring, add hypo solution for subsequent use, be stirred to without precipitation.Finally weigh the CsCL of 0.1500g, to join in above-mentioned solution liquid and to stir.Add 15g active carbon in above-mentioned maceration extract, stir, normal temperature dipping 12h, then dry 12h under 105 DEG C of conditions.This catalyst is used in the middle of acetylene hydrochlorination synthesizing chloroethylene, at 12h
-1under air speed, logical nitrogen drying 30min under 180 DEG C of conditions, then logical hydrogen chloride activation 30min, finally passes into acetylene and starts reaction, obtain conversion of alkyne 40%, selective 98% of vinyl chloride.
Claims (5)
1.
a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst, it is characterized in that the component comprising following content: carrier active carbon 10000 parts, main catalytic composition composite metal salt 1 ~ 120 part, each 50 ~ 1000 parts of auxiliary element A and B, main catalytic composition is the thiosulfate of gold, auxiliary element A is the thiosulfate of silver, and auxiliary element B is cesium chloride.
2.
a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst as claimed in claim 1, it is characterized in that first preparing certain density chlorauric acid solution, then it is for subsequent use to prepare certain density hypo solution; Take a certain amount of chlorauric acid solution, add the dilution of a certain amount of deionized water; Take a certain amount of silver salt again and stir; Then add a certain amount of hypo solution to stir; Last take a certain amount of auxiliary element B again and add in above-mentioned solution and stir, in this solution, add active carbon, impregnation drying.
3.
a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst as claimed in claim 2, is characterized in that the mass percent concentration of thiosulfate solution is 3 ~ 35.6%.
4.
a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst as claimed in claim 2, it is characterized in that dip time is 4-24h, baking temperature is 60-180 DEG C.
5.
a kind of Acetylene-hydrochlorlow-content low-content gold compound catalyst as claimed in claim 1, is characterized in that described carrier active carbon specific area is 800 ~ 3500m2/g, micropore ratio>=50% of carrier.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EA030122B1 (en) * | 2013-12-13 | 2018-06-29 | Солвей Са | Method for production of vinyl chloride from acetylene and hydrogen chloride |
| CN104289233A (en) * | 2014-08-29 | 2015-01-21 | 冯良荣 | Sulfide catalyst for preparing vinyl chloride through hydrochlorination of acetylene |
| CN107185533A (en) * | 2017-05-19 | 2017-09-22 | 新疆中泰化学股份有限公司 | Induction period controllable VCM synthesis Au-based catalyst and preparation method thereof |
| CN107442118B (en) * | 2017-08-04 | 2021-03-23 | 内蒙古大学 | Preparation method of tantalum-based catalyst for preparing vinyl chloride by hydrochlorinating acetylene |
| CN107715915B (en) * | 2017-09-29 | 2020-07-28 | 浙江工业大学 | Sulfide ionic liquid complexed palladium catalyst and preparation method and application thereof |
| CN107715919B (en) * | 2017-09-29 | 2020-10-09 | 浙江工业大学 | Load type [ PdSClx]x-Catalyst, preparation thereof and application of catalyst in vinyl chloride synthesis |
| CN108126721B (en) * | 2017-12-21 | 2019-06-28 | 厦门大学 | A kind of Au-based catalyst and its preparation method and application |
| CN109876864B (en) * | 2019-02-14 | 2021-12-28 | 西安凯立新材料股份有限公司 | Ultralow-content noble metal composite catalyst for acetylene hydrochlorination and preparation method thereof |
| GB201908844D0 (en) * | 2019-06-20 | 2019-08-07 | Johnson Matthey Plc | Gold containing catalyst, method of preparation and use |
| CN112007695B (en) * | 2020-09-23 | 2021-10-08 | 中国科学院大连化学物理研究所 | Sulfur-containing silane coupling agent modified gold catalyst for acetylene hydrochlorination |
| CN112570043B (en) * | 2020-12-08 | 2023-08-01 | 西安凯立新材料股份有限公司 | Catalyst for hydrochlorination of acetylene and application thereof |
| CN113663740A (en) * | 2021-07-28 | 2021-11-19 | 新疆至臻化工工程研究中心有限公司 | Passivation type ultralow-content gold catalyst |
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