CN102671698A - Method for preparing catalyst for synthesizing vinyl acetate from acetylene in gas phase by ultrasonic waves - Google Patents
Method for preparing catalyst for synthesizing vinyl acetate from acetylene in gas phase by ultrasonic waves Download PDFInfo
- Publication number
- CN102671698A CN102671698A CN2012100955935A CN201210095593A CN102671698A CN 102671698 A CN102671698 A CN 102671698A CN 2012100955935 A CN2012100955935 A CN 2012100955935A CN 201210095593 A CN201210095593 A CN 201210095593A CN 102671698 A CN102671698 A CN 102671698A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- vinyl acetate
- combined
- acetylene gas
- zinc acetate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 57
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 32
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 title claims abstract description 31
- 230000002194 synthesizing effect Effects 0.000 title abstract description 6
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004246 zinc acetate Substances 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000006424 Flood reaction Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 4
- 238000005457 optimization Methods 0.000 abstract 1
- 229940117958 vinyl acetate Drugs 0.000 description 35
- 239000007789 gas Substances 0.000 description 25
- 239000000243 solution Substances 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 6
- 238000007598 dipping method Methods 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- 239000012808 vapor phase Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 229920002689 polyvinyl acetate Polymers 0.000 description 3
- 239000011118 polyvinyl acetate Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000005273 aeration Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- HDERJYVLTPVNRI-UHFFFAOYSA-N ethene;ethenyl acetate Chemical group C=C.CC(=O)OC=C HDERJYVLTPVNRI-UHFFFAOYSA-N 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000002803 maceration Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 239000005997 Calcium carbide Substances 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- DBJUEJCZPKMDPA-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O DBJUEJCZPKMDPA-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- SXYCCJAPZKHOLS-UHFFFAOYSA-N chembl2008674 Chemical compound [O-][N+](=O)C1=CC=C2C(N=NC3=C4C=CC=CC4=CC=C3O)=C(O)C=C(S(O)(=O)=O)C2=C1 SXYCCJAPZKHOLS-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229920006026 co-polymeric resin Polymers 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Abstract
The invention aims to provide a method for preparing a catalyst for synthesizing vinyl acetate from acetylene in gas phase by ultrasonic waves, which is especially applicable to the field of vinyl acetate production in chemical industry. Different from the common catalyst method, the invention introduces ultrasonic technology in the impregnation-method zinc acetate preparation process, and utilizes energy generated by ultrasonic waves to promote the structural and functional optimization of the activated carbon supported zinc acetate catalyst. The catalyst has the characteristics of simple technique, short preparation period, uniformly dispersed active component and high activity.
Description
Technical field
The present invention is that a kind of ultrasonic wave prepares the method that acetylene gas is combined to vinyl acetate catalyst, is specifically related to catalyzing acetylene gas phase catalyzer for synthesizing vinyl acetate, especially is adapted to produce in the chemical industry vinyl acetate field.
Background technology
Vinyl acetate (Vinyl Acetate is hereinafter to be referred as VAC) full name vinylacetate as one of 50 kinds of maximum chemical industry Organic Ingredients of output in the world, is a kind of extremely important industrial chemicals.VAC through self polymerization or with other monomer copolymerizations, can generate organic derivatives such as polyvinyl alcohol (PVA), copolymer resins (EVA) or vinyl acetate-ethylene copolymerization emulsions (VAE), polyvinyl acetate (PVAC), vinyl acetate-chloride copolymer (EVC) and polyacrylonitrile deformable body.The polyacrylonitrile deformable body can improve the dyeability and reduction softening point of polyacrylonitrile.Vinyl acetate-chloride copolymer can be used for adhesive, coating, printing ink, plastics printing paste of manufacturer's fabricate-leather, floor tile, tape and other purposes etc.Polyvinyl acetate can be used for emulsion paint, paper figure layer etc.The vinyl acetate-ethylene copolymerization emulsions superior performance can be widely used in coating, fabric processing, paper conversion, building, packing etc.Vinyl acetate has brought very big interests in the extensive use of chemical circles to the human lives, but measure the big vinyl acetate of producing is a difficult problem in the industry of fine qualityly all the time.
See that from domestic and international research situation the Calanese company and the Japanese synthetic chemistry company of ICI company and the U.S. of Britain all once had the ethene liquid phase method to produce vinyl acetate as far back as nineteen sixty, but since technology the heavy corrosion of equipment is had to stop production.The technology that the Bayer company of the National Distillers company of 1969 the afterwards left and right sides U.S. and USI company of subsidiary thereof, Germany and three families of Hochest company have developed jointly ethene vapor phase method and permanent vinyl acetate.Through the development of decades, though the ethene vapor phase method has been applied in very most of in the world country, comprise many countries in West Europe and some countries in Eastern Europe, Korea etc. all adopt the acetylene vapor phase method to produce vinyl acetate always.In view of coal resources in China, natural gas resource rich, adopt the acetylene vapor phase method to produce vinyl acetate in China and still occupy an leading position.Therefore, the good used catalyst of acetylene vapor phase method of research processability with this productive rate that improves vinyl acetate, has realistic meaning.
At present, be combined to vinyl acetate for acetylene gas, mercury, zinc, cadmium etc. all have catalyst effectiveness preferably.Because the compound that general mercury forms has toxicity, and cadmium is a kind of expensive metal, therefore to go up the compound that surely belongs to zinc formation that can widely apply be active component in industry, and active carbon is the preparing carriers catalyst.Industrial acetic acid zinc/activated-carbon catalyst is to adopt fluid bed to spray immersion process for preparing, and still, spraying causes the load of active component zinc acetate uneven easily, and it is active relatively poor that the catalyst of production is had, and the life-span is short, and problem needs to be resolved hurrily.
The related a kind of acetylene gas of Chinese patent CN102218340A is combined to the preparation method of vinyl acetate catalyst; Be that the sealing dipping makes zinc acetate be impregnated in the active carbon as much as possible with in the impregnation drying tower of the zinc acetate solution for preparing through the filling dry activated carbon; Utilize gravity that excessive solution and free water are flowed out after accomplishing dipping; With conduction oil or hot water indirect the moisture evaporate to dryness is taken away then, accomplished the drying of catalyst, thereby make catalyst.Though this catalyst heat transfer coefficient is high, drying time is short, has reduced the fragmentation of active carbon, and catalyst preparation process is comparatively complicated.
The Preparation of Catalyst method that is used for vinyl acetate production that Chinese patent CN102039180A relates to; Method is to be that 10%～70% zinc acetate solution joins in lanthanon acetate/rare earth nitrades/rare earth-iron-boron in 50～100 ℃ of matured 0.5～3 hour with mass fraction; Again through crystallization under 10～50 ℃ of temperature, dehydrate and process.This catalyst has improved the level of production of vinyl acetate, but the Preparation of Catalyst cycle is longer.
Chinese patent CN101884920A relates to a kind of preparation method of synthesizing vinyl acetate fluid catalyst, is with SiO
2For the material of main body is made carrier, this carrier with aqueous solution of alkali matters handle precursor I, then to water, Pd compound and Au compound is prone to dissolve but in to the organic solvent of above-mentioned alkaline matter indissoluble precursor I is flooded the Pd compound and the Au compound gets precursor II; Handle precursor II with reducing agent afterwards; The Pd of ionic state is converted into metal Pd, the Au of ionic state is converted into metal A u, remove and desolvate; Washing; Drying obtains precursor II I, and precursor II I and KOAc aqueous solution are through the dry finished catalyst that gets.Though it is the strong problem of solution corrosion property that the method has solved with acetic acid, the Preparation of catalysts process is loaded down with trivial details.
The present invention compares with above several kinds of patents, is carrier with the active carbon, is maceration extract with the zinc acetate solution; Utilize the ultrasonic technology preparation, technology is simple, and manufacturing cycle is short; Environmental pollution is little, and the catalyst that makes can be combined in the vinyl acetate reaction at acetylene gas and show good activity.
Summary of the invention
The purpose of this invention is to provide a kind of ultrasonic wave prepares acetylene gas and is combined to the vinyl acetate catalyst method; Specifically be a kind of greater activity, be combined to the preparation method of vinyl acetate catalyst than high selectivity and acetylene gas with longer life; Utilize the ultrasonic technology preparation, technology is simple, and manufacturing cycle is short; Environmental pollution is little, and the catalyst that makes can be combined in the vinyl acetate reaction at acetylene gas and show good activity.
Technical scheme of the present invention: being to be carrier with the active carbon, is maceration extract with excessive zinc acetate solution, and introduces ultrasonic technology, and the preparation acetylene gas is combined to the catalyst of vinyl acetate.Concrete preparation process is following:
According to solid-to-liquid ratio (g/ml) is 0.07～0.08:1; Active carbon is added zinc acetate solution, and the container that will fill zinc acetate solution then is fixed in the ultrasonoscope of water filling, and water temperature is heated to 40～50 ℃; The adjusting ultrasonic frequency is 30～40MHz; The dipping reaction is after 15～25 minutes down to keep the vibrations of water temperature and supersonic frequency, and suction filtration is drying to obtain the catalyst that acetylene gas is combined to vinyl acetate.
The concentration of said zinc acetate solution is 0.8～1mol/L.
The granularity of said active carbon is 20～40 orders, and is common commercially available.
Principle of the present invention: ultrasonic wave energy is regulated and control catalyst structure and is optimized, and the active component zinc acetate is loaded on the carrier more uniformly, is combined to the activity of vinyl acetate catalyst and purpose optionally realize to improve acetylene gas.Ultrasonic wave is meant vibration frequency greater than the sound wave more than 20000 Hz, when ultrasonic wave is propagated in liquid, because the high vibration of liquid particle can produce little cavity at liquid internal.These little cavities swell rapidly and are closed, can make the fierce effect of impact of generation between the liquid particle, thereby produce very high pressure.This violent interaction between particulate raises the temperature of liquid, thereby has played good stirring action.Just having benefited from this stirring action can make zinc acetate be adsorbed on the surface of active carbon fully; Can also avoid the obstruction of zinc acetate in the active carbon duct; Not only can improve the load capacity of zinc acetate, also can improve its specific surface, thus maybe be to the help that will improve a lot of its activity.
Acetylene gas of the present invention is combined to vinyl acetate catalyst and when dipping, has added ultrasonic energy.
Advantage of the present invention and good effect:
(1) the catalyst process of this method preparation is simple; Adding ultrasonic wave makes the zinc acetate load on the active carbon more even later on; Load capacity is improved, and has reached 32.327%, and the catalyst (load capacity is about 30%) for preparing than commonsense method has improved nearly 8 percentage points.
(2) conversion ratio of the catalyzing acetylene gas phase synthesizing vinyl acetate of the method preparation is higher, has reached 25.57%, is that about 24% catalyst has improved nearly 15 percentage points than the conversion ratio of present factory application.
(3) catalyst that a process for preparing is higher than the specific surface of the catalyst that factory's controlling catalyst and common dipping make, and has reached 323.349 m
2/ g has almost improved nearly 30 percentage points.
(4) catalyst strength for preparing under the method is high, and environmental pollution is little, and preparation technology is simple, and catalyst performance is higher.
The specific embodiment
Below in conjunction with embodiment the present invention is further described, but the invention is not restricted to the following stated scope.
Embodiment 1:
The Preparation of Catalyst practical implementation method that the acetylene gas of present embodiment is combined to vinyl acetate is following:
According to solid-to-liquid ratio: 0.08:1g/ml; With granularity is that 20～40 order active carbons adding concentration is the zinc acetate solution of 1mol/L, and the container that will fill zinc acetate solution then is fixed in the ultrasonoscope of water filling, and water temperature is heated to 45 ℃; The adjusting ultrasonic frequency is 36MHz; After keeping the vibrations of water temperature and supersonic frequency to flood reaction 20min down, suction filtration is drying to obtain the catalyst that acetylene gas is combined to vinyl acetate.
The catalyst for preparing with successively through through the clorox aeration tower; NaOH gas washing tower; The water aeration tower; And through anhydrous calcium chloride, the acetylene gas that the calcium carbide of active carbon and discolour silica gel dry decontamination and water react generation is 270 mL/ (mLh) in air speed in the integration fixed-bed tube reactor, and reaction gas consists of C
2H
2: the reaction condition of HAc=5:1 reacts.Chromatogram analysis method is adopted in the reaction back, in time gets gas phase appearance with six-way valve, analyzes gas phase and forms.Catalyst is made indicator through eriochrome black T, measures its zinc acetate load capacity, and parameters such as the specific area of the void ratio surface area analyzer analysis of catalyst of producing with Builder company, pore-size distribution, pore volume.
The catalyst process of this method preparation is simple, and the conversion ratio of catalyzing acetylene gas phase synthesizing vinyl acetate is higher, has reached 25.57%, and the zinc acetate load is even, and the zinc acetate load capacity is 32.327%, and the specific surface of catalyst is 323.349 m
2/ g, the catalyst performance that makes than factory controlling catalyst and common dipping has improved nearly 15 percentage points, and manufacturing cycle is short.
Embodiment 2:
The Preparation of Catalyst practical implementation method that the acetylene gas of present embodiment is combined to vinyl acetate is following:
According to solid-to-liquid ratio: 0.075:1g/ml; With granularity is that 20～30 order active carbons adding concentration is the 0.8mol/L zinc acetate solution, and the container that will fill zinc acetate solution then is fixed in the ultrasonoscope of water filling, and water temperature is heated to 40 ℃; The adjusting ultrasonic frequency is 30MHz; After keeping the vibrations of water temperature and supersonic frequency to flood reaction 15min down, suction filtration is drying to obtain the catalyst that acetylene gas is combined to vinyl acetate.
Embodiment 3:
The Preparation of Catalyst practical implementation method that the acetylene gas of present embodiment is combined to vinyl acetate is following:
According to solid-to-liquid ratio: 0.07:1g/ml; With granularity is that 30～40 order active carbons adding concentration is the 0.9mol/L zinc acetate solution, and the container that will fill zinc acetate solution then is fixed in the ultrasonoscope of water filling, and water temperature is heated to 50 ℃; The adjusting ultrasonic frequency is 40MHz; After keeping the vibrations of water temperature and supersonic frequency to flood reaction 25min down, suction filtration is drying to obtain the catalyst that acetylene gas is combined to vinyl acetate.
Claims (3)
1. a ultrasonic wave prepares the method that acetylene gas is combined to vinyl acetate catalyst; It is characterized in that concrete preparation process is following: according to solid-to-liquid ratio: 0.07～0.08:1; Active carbon is added zinc acetate solution, and the container that will fill zinc acetate solution then is fixed in the ultrasonoscope of water filling, and water temperature is heated to 40～50 ℃; The adjusting ultrasonic frequency is 30～40MHz; After keeping the vibrations of water temperature and supersonic frequency to flood reaction 15～25min down, suction filtration is drying to obtain the catalyst that acetylene gas is combined to vinyl acetate.
2. ultrasonic wave according to claim 1 prepares the method that acetylene gas is combined to vinyl acetate catalyst, it is characterized in that: the granularity of said active carbon is 20～40 orders.
3. ultrasonic wave according to claim 1 prepares the method that acetylene gas is combined to vinyl acetate catalyst, it is characterized in that: the concentration of said zinc acetate solution is 0.8～1mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100955935A CN102671698A (en) | 2012-04-01 | 2012-04-01 | Method for preparing catalyst for synthesizing vinyl acetate from acetylene in gas phase by ultrasonic waves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100955935A CN102671698A (en) | 2012-04-01 | 2012-04-01 | Method for preparing catalyst for synthesizing vinyl acetate from acetylene in gas phase by ultrasonic waves |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102671698A true CN102671698A (en) | 2012-09-19 |
Family
ID=46804638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012100955935A Pending CN102671698A (en) | 2012-04-01 | 2012-04-01 | Method for preparing catalyst for synthesizing vinyl acetate from acetylene in gas phase by ultrasonic waves |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102671698A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437626A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Catalyst for acetylene-method vinyl acetate and synthesis method of vinyl acetate |
| CN104437627A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Acetylene method vinyl acetate catalyst and preparation method thereof |
| CN104437623A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Catalyst for acetylene-method vinyl acetate and synthesis method of vinyl acetate |
| CN105457683A (en) * | 2014-09-25 | 2016-04-06 | 中国石油化工股份有限公司 | Vinyl acetate catalyst |
| CN108144648A (en) * | 2018-01-29 | 2018-06-12 | 安徽皖维高新材料股份有限公司 | A kind of preparation method of acetylene in gas phase method synthesizing vinyl acetate catalyst |
| CN113620802A (en) * | 2020-05-08 | 2021-11-09 | 中国石油化工股份有限公司 | Catalyst for synthesizing vinyl acetate by acetylene method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101695653A (en) * | 2009-10-22 | 2010-04-21 | 昆明理工大学 | Modified activated carbon adsorbent for low-concentration phosphine, preparation method and application thereof |
| CN102218340A (en) * | 2010-04-16 | 2011-10-19 | 天华化工机械及自动化研究设计院 | Preparation method for synthesizing vinyl acetate catalyst by using acetylene gas phase method |
-
2012
- 2012-04-01 CN CN2012100955935A patent/CN102671698A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101695653A (en) * | 2009-10-22 | 2010-04-21 | 昆明理工大学 | Modified activated carbon adsorbent for low-concentration phosphine, preparation method and application thereof |
| CN102218340A (en) * | 2010-04-16 | 2011-10-19 | 天华化工机械及自动化研究设计院 | Preparation method for synthesizing vinyl acetate catalyst by using acetylene gas phase method |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437626A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Catalyst for acetylene-method vinyl acetate and synthesis method of vinyl acetate |
| CN104437627A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Acetylene method vinyl acetate catalyst and preparation method thereof |
| CN104437623A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Catalyst for acetylene-method vinyl acetate and synthesis method of vinyl acetate |
| CN104437626B (en) * | 2013-09-24 | 2016-09-07 | 中国石油化工股份有限公司 | Acetylene method vinyl acetate catalyst and the synthetic method of vinyl acetate |
| CN104437623B (en) * | 2013-09-24 | 2017-03-01 | 中国石油化工股份有限公司 | Acetylene method vinyl acetate catalyst and the synthetic method of vinyl acetate |
| CN105457683A (en) * | 2014-09-25 | 2016-04-06 | 中国石油化工股份有限公司 | Vinyl acetate catalyst |
| CN105457683B (en) * | 2014-09-25 | 2018-01-09 | 中国石油化工股份有限公司 | Vinyl acetate catalyst |
| CN108144648A (en) * | 2018-01-29 | 2018-06-12 | 安徽皖维高新材料股份有限公司 | A kind of preparation method of acetylene in gas phase method synthesizing vinyl acetate catalyst |
| CN113620802A (en) * | 2020-05-08 | 2021-11-09 | 中国石油化工股份有限公司 | Catalyst for synthesizing vinyl acetate by acetylene method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102671698A (en) | Method for preparing catalyst for synthesizing vinyl acetate from acetylene in gas phase by ultrasonic waves | |
| CN104108713B (en) | A kind ofly come from the porous carbon of Vegetable Sponge of Luffa and the preparation method of matrix material thereof and application | |
| CN105152281A (en) | Preparation method of capacitive type desalination electrode prepared from hierarchical porous carbon material with core-shell structure | |
| CN102824895B (en) | Mesoporous limited functionalized ionic liquid composite material and preparation method and application thereof | |
| CN103638979A (en) | Magnetic zeolite imidazate metal organic skeletal material, preparation thereof and application to liquid phase condensation catalytic reaction | |
| CN109260967B (en) | Metal organic framework composite membrane and preparation method and application thereof | |
| CN102728328B (en) | Renewable asphalt mixture modifier for absorbing automobile exhaust and preparation method thereof | |
| CN104226243A (en) | Preparation method of novel enteromorpha-based carbon material | |
| CN102114413A (en) | Macroporous spherical polyacrylonitrile chelatesorbent and microwave radiating preparation process thereof | |
| CN103962097A (en) | Method for preparing CO2 carbon-based absorbent on basis ofenteromorpha | |
| CN105854818A (en) | Aerogel-based oil eliminating agent and preparation method thereof | |
| CN108246269B (en) | Lithium ion adsorbent and preparation method and application thereof | |
| CN109232781A (en) | A kind of preparation method of nitrogenous porous organic polymer | |
| CN105772057A (en) | Preparation method of ordered mesoporous catalyst for synthesizing acrylic acid by acetic acid and methanol | |
| CN110421665B (en) | Energy storage wood takes titanium dioxide loaded rhodamine red as heat conduction filler | |
| CN100482348C (en) | Process of treating catalyst carrier waste active carbon for synthesizing vinyl acetate | |
| CN105061657A (en) | Novel nanoporous organic framework solid alkali material, preparation method and applications thereof | |
| CN107903575A (en) | A kind of preparation method of electrode for capacitors graphene phenolic-resin based composite fibre film | |
| CN102351168B (en) | Preparation method of vinylidene chloride polymer base mesopore-micropore composite porous charcoal | |
| CN106582853A (en) | Catalyst for acetylene method vinyl acetate synthesis | |
| CN104399527A (en) | Preparation method of attapulgite/polymerized ionic liquid composite catalyst | |
| CN102151581A (en) | Molybdenum phosphide catalyst for production of chloroethylene and preparation method thereof | |
| CN101428239A (en) | Absorbent charcoal based catalyst carrier, catalyst, preparation and uses thereof | |
| CN109499493B (en) | polypyrrole/ZIF-67 composite aerogel and preparation method thereof | |
| CN110407208A (en) | A kind of preparation method of mesoporous graphene-based charcoal-aero gel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120919 |