CN103157499A - Preparation of novel nitrogen modified Au/N-AC catalyst and catalytic activity of catalyst on acetylene hydrochlorination reaction - Google Patents
Preparation of novel nitrogen modified Au/N-AC catalyst and catalytic activity of catalyst on acetylene hydrochlorination reaction Download PDFInfo
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- CN103157499A CN103157499A CN2013101064383A CN201310106438A CN103157499A CN 103157499 A CN103157499 A CN 103157499A CN 2013101064383 A CN2013101064383 A CN 2013101064383A CN 201310106438 A CN201310106438 A CN 201310106438A CN 103157499 A CN103157499 A CN 103157499A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 title claims abstract description 20
- 238000007038 hydrochlorination reaction Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 title claims description 14
- 230000003197 catalytic effect Effects 0.000 title claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 235000013162 Cocos nucifera Nutrition 0.000 claims abstract description 8
- 244000060011 Cocos nucifera Species 0.000 claims abstract description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 239000003607 modifier Substances 0.000 claims abstract description 3
- 239000010931 gold Substances 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000003610 charcoal Substances 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 3
- 150000001345 alkine derivatives Chemical class 0.000 claims description 3
- 239000010903 husk Substances 0.000 claims description 3
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 229920000877 Melamine resin Polymers 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- 239000000178 monomer Substances 0.000 abstract 1
- 229910001220 stainless steel Inorganic materials 0.000 abstract 1
- 239000010935 stainless steel Substances 0.000 abstract 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 5
- 229910052753 mercury Inorganic materials 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 238000006424 Flood reaction Methods 0.000 description 2
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- RZXUKBRHXFSGJL-UHFFFAOYSA-N [N].C(=C)Cl Chemical compound [N].C(=C)Cl RZXUKBRHXFSGJL-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Landscapes
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
本发明涉及一种新型氮改性椰壳活性炭的制备方法及应用。它主要以尿素、氨水、三聚氰胺为改性剂改性椰壳活性炭，将改性后的活性炭作为载体，Au为活性组分，采用等体积浸渍法制备得到催化剂。该催化剂在T＝180℃、C2H2(GHSV)＝360h-1、V(HCl)/V(C2H2)＝1.15和Au的质量分数为0.2％的条件下，在不锈钢固定床反应器中进行乙炔氢氯化反应活性测试，经过一段时间反应，可使乙炔的转化率达到89％以上，氯乙烯单体选择性达到99.91％以上。The invention relates to a preparation method and application of a novel nitrogen-modified coconut shell activated carbon. It mainly uses urea, ammonia water, and melamine as modifiers to modify coconut shell activated carbon, uses the modified activated carbon as a carrier, and uses Au as an active component. The catalyst is prepared by an equal-volume impregnation method. The catalyst was placed in a stainless steel fixed bed under the conditions of T=180°C, C 2 H 2 (GHSV)=360h -1 , V(HCl)/V(C 2 H 2 )=1.15 and the mass fraction of Au was 0.2%. The reaction activity test of acetylene hydrochlorination is carried out in the reactor. After a period of reaction, the conversion rate of acetylene can reach more than 89%, and the selectivity of vinyl chloride monomer can reach more than 99.91%.
Description
Technical field
The present invention relates to a kind of preparation method of acetylene hydrochlorination synthesizing chloroethylene nitrogen modification catalyst without mercury
Background technology
Vinyl chloride (vinyl chloride monoder) is called for short VCM, mainly for the production of polyvinyl chloride (PVC), it is one of large resins for universal use in the world five (PVC, PE, PP, PS and ABS), have the plurality of advantages such as wear-resisting, anti-combustion, insulation, anticorrosive and mechanical strength be high, be widely used in the fields such as industrial or agricultural, building industry, commodity.The synthetic method of vinyl chloride mainly adopts process for oxychlorination of ethylene and acetylene hydrochlorination method, and the rich coal of China, the energy resource structure that oil-poor, weak breath is special cause the ethylene raw shortage, but abundant coal resource provide sufficient acetylene raw material for the acetylene hydrochlorination method.Therefore, China overwhelming majority's vinyl chloride adopts the acetylene hydrochlorination method to synthesize.Be catalyst because acetylene hydrochlorination technique adopts mercury chloride/active carbon always, this catalyst has severe toxicity, mercury chloride easily to run off, easily health and environment are worked the mischief, therefore how to eliminate mercury pollution, realize that the process for cleanly preparing of the standby vinyl chloride of acetylene hydrochlorination legal system is current numerous researcher urgent problem.The exploitation of catalyst without mercury and popularization are the preferred plan that addresses this problem at present proposition, many researchers have also carried out a large amount of research to this, most literature report be fit to the acetylene hydrochlorination reaction catalytic activity be precious metal salt such as Au, Rh, Pt, Pd etc.
Can be from two aspects to the improvement of catalyst without mercury, the one, reduce metal catalyst content by adding auxiliary agent, the 2nd, select new carrier to increase the adhesion of metal and carrier, improve its activity and stable.Present most of experimental study emphasis is in screening and research to noble metal, and therefore relatively less to the research report of carrier select suitable carrier to have larger space to the acetylene hydrochlorination repercussion study.Early-stage Study shows that the higher nitrogen content of active carbon, degree of graphitization and heat endurance have higher catalytic performance as carrier.Activated carbon surface can show acidity, alkalescence and neutral, and these features depend on that there is surface functional group in its surface.Therefore, thus further the activated carbon modified extra physical chemistry function of active carbon of can giving is improved their application in practice.So be the research direction of acetylene hydrochlorination reaction novel mercury-free catalyst to support modification.
Summary of the invention
The object of the present invention is to provide a kind of active component content low, catalyst without mercury of catalytic activity and stable all reasonable acetylene hydrochlorination synthesizing chloroethylenes and preparation method thereof.
Main technical schemes: the catalyst of acetylene hydrochlorination preparing chloroethylene comprises nitrogen modified support carrier and metal active constituent, wherein take urea, ammoniacal liquor, cyanurotriamide modified cocoanut active charcoal as carrier, take gold as active component.The preparation method of acetylene hydrochlorination synthesizing chloroethylene catalysts is:
1., respectively with urea, ammoniacal liquor, cyanurotriamide modified dose and coconut husk charcoal x in mass ratio: 1 is immersed in the appropriate aqueous solution, stirs 24h at 85 ℃ of temperature, takes out, and drains, in 80～120 ℃ of dry 12h;
2., the said goods is placed in tube furnace, the speed with 2～8 ℃/min in nitrogen stream rises to 550～700 ℃ from room temperature, and is keeping being cooled to room temperature after 1h at this temperature, and namely to the x-AC active carbon that changes after surname, x represents modifier.
3., with the HAuCl that measures
44H
2O is made into wang aqueous solution with the chloroazotic acid of new preparation, and it is 0.5%～3% of catalyst weight that the concentration of wang aqueous solution makes the content of Au in final catalyst, floods the nitrogen modified support in the Au wang aqueous solution, and dip time is more than 8h;
4., water bath method, then put into 120～160 ℃ of oven dry of baking oven, be placed on logical hydrogen chloride activation in reactor, reaction, conversion of alkyne can reach more than 89%, vinyl chloride selectively reaches more than 99.91%.
The invention has the advantages that: the preparation method is simple to operate, economy, environmental protection, can reduce carrier and active component cost with catalyst acetylene hydrochlorination of the present invention, and product is selectively good, and accessory substance is few, and catalytic reaction activity is high.
The specific embodiment
Embodiment 1:
The preparation method of acetylene hydrochlorination synthesizing chloroethylene catalysts is:
1., cyanurotriamide modified dose is immersed in the appropriate aqueous solution in mass ratio with the coconut husk charcoal at 0.8: 1, stir 24h at 85 ℃ of temperature, take out, drain, in 80 ℃ of dry 12h;
2., the said goods is placed in tube furnace, the speed with 5 ℃/min in nitrogen stream rises to 650 ℃ from room temperature, and is keeping being cooled to room temperature after 1h at this temperature, namely to the M-AC active carbon that changes after surname.
3., with the HAuCl that measures
44H
2O is made into wang aqueous solution with the chloroazotic acid of new preparation, and it is 0.5%～3% of catalyst weight that the concentration of wang aqueous solution makes the content of Au in final catalyst, floods above-mentioned nitrogen modification M-AC absorbent charcoal carrier in the Au wang aqueous solution, and dip time is more than 8h;
4., water bath method, then put into 140 ℃ of oven dry of baking oven, be placed on logical hydrogen chloride activation in reactor, reaction.At 180 ℃, C
2H
2(GHSV)=360h
-1, V (HCl)/V (C
2H
2The load capacity of)=1.15, Au is under 0.2% reaction condition, and the conversion of alkyne of Au/M-AC catalyst can reach 89% (improving 7% than Au/AC), selectively near 99.91%.Adopt Shimadzu GC-2014C type chromatograph to analyze.Fid detector, the GDX-301 (packed column of 2m * 4mm).
Claims (4)
1. novel nitrogen modification Au/N-AC catalyst is characterized in that mainly take urea, ammoniacal liquor, cyanurotriamide modified cocoanut active charcoal as carrier, take gold as active component, wherein the content of Au accounts for 0.2%～1%. of catalyst weight
2. novel nitrogen modification Au/N-AC catalyst according to claim 1, the preparation method who it is characterized in that the nitrogen modified support: 1., respectively with urea, ammoniacal liquor, cyanurotriamide modified dose and coconut husk charcoal x in mass ratio: 1 is immersed in the appropriate aqueous solution, stir 24h at 85 ℃ of temperature, take out, drain, in 80～120 ℃ of dry 12h; 2., the said goods is placed in tube furnace, the speed with 2-8 ℃/min in nitrogen stream rises to 550～700 ℃ from room temperature, and is keeping being cooled to room temperature after 1h at this temperature, and namely to the x-AC active carbon that changes after surname, x represents modifier.
3. novel nitrogen modification Au/N-AC catalyst according to claim 1 is characterized in that with urea, ammoniacal liquor, cyanurotriamide modified cocoanut active charcoal as carrier, in preparation Au/N-AC catalyst, the content of Au accounts for catalyst weight and can drop to 0.2% from 1%.
1., with the HAuCl of metering 4. the catalytic activity of Au/N-AC catalyst to acetylene hydrochlorination reaction according to claim 1 is characterized in that:
44H
2The chloroazotic acid of the new preparation of 0 use is made into wang aqueous solution, and it is 0.5%～3% of catalyst weight that the concentration of wang aqueous solution makes the content of Au in final catalyst; 2., in the Au wang aqueous solution dipping nitrogen modified support, dip time is more than 8h; 3., water bath method, then put into 120～160 ℃ of oven dry of baking oven, be placed on logical hydrogen chloride activation in reactor, reaction, conversion of alkyne can reach more than 89%, vinyl chloride selectively reaches more than 99.91%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103381369A (en) * | 2013-07-10 | 2013-11-06 | 清华大学 | Nitrogen doped carbon material loaded catalyst |
| CN107442175A (en) * | 2017-08-29 | 2017-12-08 | 贵州重力科技环保有限公司 | Low solid mercury catalyst of a kind of high degree of dispersion of acetylene hydrochlorination and preparation method thereof |
| CN107442118A (en) * | 2017-08-04 | 2017-12-08 | 内蒙古大学 | A kind of preparation method of acetylene hydrochlorination preparing chloroethylene tantalum base catalyst |
| CN107456990A (en) * | 2017-08-29 | 2017-12-12 | 贵州重力科技环保有限公司 | A kind of high degree of dispersion ruthenium-based catalyst of acetylene hydrochlorination and preparation method thereof |
| CN108043467A (en) * | 2017-11-27 | 2018-05-18 | 宁夏新龙蓝天科技股份有限公司 | Mercury-free catalyst for improving yield of chloroethylene and preparation method thereof |
| CN108126721A (en) * | 2017-12-21 | 2018-06-08 | 厦门大学 | A kind of Au-based catalyst and its preparation method and application |
| JP2018515579A (en) * | 2015-05-27 | 2018-06-14 | ジョンソン、マッセイ、パブリック、リミテッド、カンパニーＪｏｈｎｓｏｎ Ｍａｔｔｈｅｙ Ｐｕｂｌｉｃ Ｌｉｍｉｔｅｄ Ｃｏｍｐａｎｙ | Process for the preparation of vinyl chloride |
| CN110142053A (en) * | 2019-05-28 | 2019-08-20 | 沈阳化工大学 | Preparation method of a mercury-free catalyst for the synthesis of vinyl chloride by acetylene hydrochlorination |
| CN111420694A (en) * | 2020-04-02 | 2020-07-17 | 鄂尔多斯市瀚博科技有限公司 | Copper-based catalyst taking nitrogen modified activated carbon as carrier and preparation method and application thereof |
| CN112570043A (en) * | 2020-12-08 | 2021-03-30 | 西安凯立新材料股份有限公司 | Catalyst for acetylene hydrochlorination and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103381369A (en) * | 2013-07-10 | 2013-11-06 | 清华大学 | Nitrogen doped carbon material loaded catalyst |
| JP2018515579A (en) * | 2015-05-27 | 2018-06-14 | ジョンソン、マッセイ、パブリック、リミテッド、カンパニーＪｏｈｎｓｏｎ Ｍａｔｔｈｅｙ Ｐｕｂｌｉｃ Ｌｉｍｉｔｅｄ Ｃｏｍｐａｎｙ | Process for the preparation of vinyl chloride |
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| CN107442118B (en) * | 2017-08-04 | 2021-03-23 | 内蒙古大学 | A kind of preparation method of acetylene hydrochlorination to vinyl chloride tantalum-based catalyst |
| CN107456990A (en) * | 2017-08-29 | 2017-12-12 | 贵州重力科技环保有限公司 | A kind of high degree of dispersion ruthenium-based catalyst of acetylene hydrochlorination and preparation method thereof |
| CN107442175B (en) * | 2017-08-29 | 2020-04-07 | 贵州重力科技环保有限公司 | Acetylene hydrochlorination high-dispersity low-solid-mercury catalyst and preparation method thereof |
| CN107442175A (en) * | 2017-08-29 | 2017-12-08 | 贵州重力科技环保有限公司 | Low solid mercury catalyst of a kind of high degree of dispersion of acetylene hydrochlorination and preparation method thereof |
| CN108043467A (en) * | 2017-11-27 | 2018-05-18 | 宁夏新龙蓝天科技股份有限公司 | Mercury-free catalyst for improving yield of chloroethylene and preparation method thereof |
| CN108126721A (en) * | 2017-12-21 | 2018-06-08 | 厦门大学 | A kind of Au-based catalyst and its preparation method and application |
| CN110142053A (en) * | 2019-05-28 | 2019-08-20 | 沈阳化工大学 | Preparation method of a mercury-free catalyst for the synthesis of vinyl chloride by acetylene hydrochlorination |
| CN111420694A (en) * | 2020-04-02 | 2020-07-17 | 鄂尔多斯市瀚博科技有限公司 | Copper-based catalyst taking nitrogen modified activated carbon as carrier and preparation method and application thereof |
| CN112570043A (en) * | 2020-12-08 | 2021-03-30 | 西安凯立新材料股份有限公司 | Catalyst for acetylene hydrochlorination and application thereof |
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Application publication date: 20130619 |