CN107456989A - A kind of high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination and preparation method thereof - Google Patents
A kind of high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination and preparation method thereof Download PDFInfo
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- CN107456989A CN107456989A CN201710756769.XA CN201710756769A CN107456989A CN 107456989 A CN107456989 A CN 107456989A CN 201710756769 A CN201710756769 A CN 201710756769A CN 107456989 A CN107456989 A CN 107456989A
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- catalyst
- mercury
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- activated carbon
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- 239000003054 catalyst Substances 0.000 title claims abstract description 53
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 title claims abstract description 48
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 34
- 239000006185 dispersion Substances 0.000 title claims abstract description 31
- 238000007038 hydrochlorination reaction Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 230000000802 nitrating effect Effects 0.000 claims abstract description 25
- PSCMQHVBLHHWTO-UHFFFAOYSA-K Indium trichloride Inorganic materials Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910019032 PtCl2 Inorganic materials 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005470 impregnation Methods 0.000 claims abstract description 4
- 230000008859 change Effects 0.000 claims description 9
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 239000002006 petroleum coke Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 239000002817 coal dust Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 230000003197 catalytic effect Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 230000006698 induction Effects 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000002270 dispersing agent Substances 0.000 abstract description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 235000011164 potassium chloride Nutrition 0.000 description 8
- 239000001103 potassium chloride Substances 0.000 description 8
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 7
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 238000007259 addition reaction Methods 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 230000002860 competitive effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 239000002156 adsorbate Substances 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
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OTUXCLKRSRDYPV-UHFFFAOYSA-N acetylene hydrochloride Chemical compound Cl.C#C OTUXCLKRSRDYPV-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/40—
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/07—Preparation of halogenated hydrocarbons by addition of hydrogen halides
- C07C17/08—Preparation of halogenated hydrocarbons by addition of hydrogen halides to unsaturated hydrocarbons
Abstract
The invention discloses high degree of dispersion nanometer catalyst without mercury of a kind of acetylene hydrochlorination and preparation method thereof, the catalyst is with PtCl2For main catalyst component, KCl and InCl3For catalyst aid, particle diameter is less than 5nm nano-TiO2For dispersant, nitrating activated carbon is carrier, is prepared using the method for ultrasonic disperse step impregnation microwave drying.The catalyst has that decentralization is high, active site position is small and narrow particle size distribution, the advantages of anti-carbon deposit effect is good, catalytic conversion is high, induction period is short, service life is long.
Description
Technical field
The present invention relates to a kind of chemical catalyst, the high degree of dispersion nanometer catalyst without mercury of particularly a kind of acetylene hydrochlorination
And preparation method thereof.
Background technology
Acetylene hydrochlorination method and process for oxychlorination of ethylene are vinyl chloride（VCM）The synthetic method mainly used in production process,
Due to being restricted by China " oil-poor, rich coal, few gas " resource structures, about 75% or so vinyl chloride at present（VCM）It is to use acetylene
Hydrogen chloride method is produced, but it is dirty to have serious environment always mainly using mercury chloride/activated carbon of severe toxicity as catalyst for the route
Dye problem.On October 10th, 2013, sponsored what Japan held by United Nations Environment Programme《Minamata pact》Diplomatic full powers
In conference, the per pro of 92 countries and regions including China《Minamata pact》, control and reduce hand in hand global mercury
Discharge.Therefore, development and mercury emission reduction of the research and development of nanometer catalyst without mercury for PVC industries are all significant.
In acetylene hydrochlorination course of reaction, catalytic conversion depends primarily on the decentralization of catalyst surface active component,
Total molecular number in bioactive molecule number/activated carbon of decentralization=carrier surface, and catalyst aid, dispersant, competitive adsorbate and
The selection of carrier, preparation technology have an impact for decentralization.
Therefore, existing catalyst exist decentralization is low, anti-carbon deposit effect is poor, catalytic conversion is low, induction period length with
And service life it is shorter the shortcomings that.Its main cause is：1. decentralization is low, preparation technology, carrier, dispersant, competitive adsorbate
Selection it is improper, cause active component to exist in the form of cluster, amount of activated component is not combined effectively with carrier, catalyzed conversion
Rate is relatively low；2. in the mixed gas of chemical inactivation, acetylene and hydrogen chloride and catalytic active component contact process, acetylene is easily activity
Component reduces；3. coking deactivation, acetylene self-polymeric reaction produces autopolymer, has blocked catalytic active component.
The content of the invention
It is an object of the present invention to provide high degree of dispersion nanometer catalyst without mercury of a kind of acetylene hydrochlorination and preparation method thereof.
The catalyst of the present invention has that decentralization is high, active site position is small and narrow particle size distribution, anti-carbon deposit effect is good, catalytic conversion is high,
The advantages of induction period is short, service life is long.
Technical scheme：A kind of high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination, it is characterised in that：Institute
State catalyst and use PtCl2、KCl、InCl3, nano-TiO2It is made with nitrating activated carbon.
A kind of high degree of dispersion nanometer catalyst without mercury of foregoing acetylene hydrochlorination, the catalyst calculate by weight：Adopt
Use PtCl20.05-1 parts, KCl0.028-0.56 parts, InCl30.12-2.5 parts, nano-TiO20.06-1.2 parts and nitrating activated carbon
94.74-99.742 part is made.
In a kind of high degree of dispersion nanometer catalyst without mercury of foregoing acetylene hydrochlorination, the PtCl2、KCl、InCl3With receive
Rice TiO2The amount ratio of material be：1:2:3:4.
In a kind of high degree of dispersion nanometer catalyst without mercury of foregoing acetylene hydrochlorination, the nano-TiO2The diameter of particle
Less than 5nm.
In a kind of high degree of dispersion nanometer catalyst without mercury of foregoing acetylene hydrochlorination, the nitrating activated carbon is by coal
Powder, petroleum coke, melamine are 10 in mass ratio:1：0.5-1 is by stirring, granulation, charing, activation, rinsing and dries preparation
's.
The preparation method of the high degree of dispersion nanometer catalyst without mercury of foregoing acetylene hydrochlorination, is prepared according to the following steps：
（a）By PtCl2、KCl、InCl3And nano-TiO2Add in the aqueous solution and be well mixed, obtain A product；
（b）Nitrating activated carbon is impregnated using A product, obtains B product；
（c）B product are dried, obtain the high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination.
In foregoing preparation method, the step（b）It is middle that nitrating activated carbon is impregnated using A product, it is to divide equally A product
Into 2 ~ 3 equal portions, under 80 DEG C of ultrasound conditions, step impregnation is carried out to nitrating activated carbon.
In foregoing preparation method, the step（c）In B product are dried, be to use microwave drying, dry to B product
Middle moisture is less than 0.3%.
Compared with prior art, 1. major catalyst PtCl2Nano particle size directly influence acetylene hydrochlorination catalysis
The conversion ratio of reaction, 5nm nano-TiO is less than by adding particle diameter2, do using ultrasonic step impregnation and using microwave
It is dry to each contribute to control PtCl2Particle diameter in 0.25nm or so, narrow particle size distribution and decentralization can be increased, improve catalyzed conversion
Rate；
2. one of the main reason for causing platinum chloride catalyst to inactivate is carbon deposit caused by acetylene autohemagglutination, autopolymer is deposited on activity
On point position, the contact of acetylene and chlorine hydride mixed gas body with chlorauride active site position is blocked, by adding nano-TiO2Help
In the generation of anti-carbon deposit phenomenon, the service life of catalyst can be extended；
3. by by InCl3Added as catalyst aid, in adsorption process is impregnated, competitive Adsorption, the portion of nitrating carrier be present
Divide surface by InCl3Occupy, increase the decentralization of active site position；Secondly, InCl3PtCl can be increased2The density of electron cloud,
The ability of adsorbing chlorinated hydrogen is improved, the catalytic conversion of catalyst can be improved；
4. the effect that decomposition induction time is shortened in the addition of potassium chloride is more obvious, this is probably because alkali metal K is without d
Electronics and d holes, there is stronger electron donation, increase the cloud density of mercury chloride, can shorten induction period and
Improve catalytic conversion；
5. by being used as carrier from nitrating activated carbon, the nitrogen-atoms in nitrating activated carbon affects carbon around as electron donor
While atom and the catalytic active component of load, there is grappling effect to active component.
⑥PtCl2、KCl、InCl3And nano-TiO2The amount ratio of material be：1:2:3:4 acetylene hydrochlorinations being prepared
High degree of dispersion nanometer catalyst without mercury, catalytic conversion >=99.5%, catalytic conversion highest.
In summary, catalyst of the invention has that decentralization is high, active site position is small and narrow particle size distribution, anti-carbon deposit effect
Well, the advantages of catalytic conversion is high, induction period is short, service life is long.
Embodiment
With reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiment 1.A kind of high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination, is calculated by weight, is used
PtCl20.1 part, KCl0.056 parts, InCl30.25 part, nano-TiO of the diameter less than 5nm of particle20.12 part and nitrating activity
99.474 parts of charcoal is made.
It is 10 in mass ratio by coal dust, petroleum coke, melamine that nitrating activated carbon, which is,:1：0.5 by stirring, granulation, charcoal
Change, activate, rinse and dry what is prepared.
The preparation method of the high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination, is prepared according to the following steps：
（a）By the PtCl of above-mentioned parts by weight2、KCl、InCl3And nano-TiO2Add in the aqueous solution and be well mixed, obtain A product；
（b）A product are divided into 2 deciles, under 80 DEG C of ultrasound conditions, nitrating 2 steps of activated carbon point impregnated；
（c）B product are dried by the way of microwave drying, it is 0.26% to dry into B product moisture, obtains acetylene hydrogen chlorine
The high degree of dispersion nanometer catalyst without mercury of change.
With the high degree of dispersion catalyst without mercury of acetylene hydrochlorination made from the raw material of this parts by weight, for acetylene and hydrogen chloride
Addition reaction when, be 20h in acetylene space flow speed-1, acetylene is 1 with hydrogen chloride molecular proportion：Under conditions of 1.15, determine it and urge
It is 98% to change conversion ratio.
Embodiment 2.A kind of high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination, is calculated by weight, is used
PtCl20.4 part, KCl0.224 parts, InCl31 part, the diameter of particle is less than 5nm nano-TiO20.48 part and nitrating activated carbon
97.896 part is made.
It is 10 in mass ratio by coal dust, petroleum coke, melamine that nitrating activated carbon, which is,:1：0.8 by stirring, granulation, charcoal
Change, activate, rinse and dry what is prepared.
The preparation method of the high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination, is prepared according to the following steps：
（a）By the PtCl of above-mentioned parts by weight2、KCl、InCl3And nano-TiO2Add in the aqueous solution and be well mixed, obtain A product；
（b）A product are divided into 3 deciles, under 80 DEG C of ultrasound conditions, nitrating 3 steps of activated carbon point impregnated；
（c）B product are dried by the way of microwave drying, it is 0.27% to dry into B product moisture, obtains acetylene hydrogen chlorine
The high degree of dispersion nanometer catalyst without mercury of change.
With the high degree of dispersion catalyst without mercury of acetylene hydrochlorination made from the raw material of this parts by weight, for acetylene and hydrogen chloride
Addition reaction when, be 20h in acetylene space flow speed-1, acetylene is 1 with hydrogen chloride molecular proportion：Under conditions of 1.15, determine it and urge
It is 98.5% to change conversion ratio.
Embodiment 3.A kind of high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination, is calculated by weight, is used
PtCl20.8 part, KCl0.448 parts, InCl32 parts, the diameter of particle is less than 5nm nano-TiO20.96 part and nitrating activated carbon
95.792 part is made.
It is 10 in mass ratio by coal dust, petroleum coke, melamine that the nitrating activated carbon, which is,:1：1 by stirring, be granulated,
Charing, activation, rinsing and dry preparation.
The preparation method of the high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination, is prepared according to the following steps：
（a）By the PtCl of above-mentioned parts by weight2、KCl、InCl3And nano-TiO2Add in the aqueous solution and be well mixed, obtain A product；
（b）A product are divided into 4 deciles, under 80 DEG C of ultrasound conditions, nitrating 4 steps of activated carbon point impregnated；
（c）B product are dried by the way of microwave drying, it is 0.28% to dry into B product moisture, obtains acetylene hydrogen chlorine
The high degree of dispersion nanometer catalyst without mercury of change.
With the high degree of dispersion catalyst without mercury of acetylene hydrochlorination made from the raw material of this parts by weight, for acetylene and hydrogen chloride
Addition reaction when, be 20h in acetylene space flow speed-1, acetylene is 1 with hydrogen chloride molecular proportion：Under conditions of 1.15, determine it and urge
It is 99% to change conversion ratio.
Claims (8)
- A kind of 1. high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination, it is characterised in that：The catalyst uses PtCl2、 KCl、InCl3, nano-TiO2It is made with nitrating activated carbon.
- A kind of 2. high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination according to claim 1, it is characterised in that：Institute Catalyst is stated, by weight：Using PtCl20.05-1 parts, KCl0.028-0.56 parts, InCl30.12-2.5 parts, nanometer TiO20.06-1.2 parts and nitrating activated carbon 94.74-99.742 parts are made.
- 3. a kind of high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination according to claim 1 or 2, its feature exist In：The PtCl2、KCl、InCl3And nano-TiO2The amount ratio of material be：1:2:3:4.
- 4. a kind of high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination according to claim 1 or 2, its feature exist In：Nano-TiO2The diameter of particle is less than 5nm.
- A kind of 5. high degree of dispersion nanometer catalyst without mercury of acetylene hydrochlorination according to claim 1 or claim 2, it is characterised in that： It is 10 in mass ratio by coal dust, petroleum coke, melamine that nitrating activated carbon, which is,:1：0.5-1 passes through stirring, is granulated, carbonizes, be living Change, rinse and dry what is prepared.
- 6. according to the high degree of dispersion nanometer catalyst without mercury of the acetylene hydrochlorination described in claim 1 to 5 any claim Preparation method, it is characterised in that：Prepare according to the following steps：（a）By PtCl2、KCl、InCl3And nano-TiO2Add in the aqueous solution and be well mixed, obtain A product；（b）Nitrating activated carbon is impregnated using A product, obtains B product；（c）B product are dried, obtain catalyst.
- 7. preparation method according to claim 6, it is characterised in that：The step（b）It is middle to use A product to nitrating activated carbon Impregnated, be that A product are divided into 2 ~ 3 equal portions, under 80 DEG C of ultrasound conditions, step impregnation is carried out to nitrating activated carbon.
- 8. preparation method according to claim 6, it is characterised in that：The step（c）In B product are dried, be to adopt With microwave drying, dry into B product moisture and be less than 0.3%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110548499A (en) * | 2019-08-16 | 2019-12-10 | 西安凯立新材料股份有限公司 | Composite carrier catalyst for acetylene hydrochlorination and application thereof |
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| CN110548499A (en) * | 2019-08-16 | 2019-12-10 | 西安凯立新材料股份有限公司 | Composite carrier catalyst for acetylene hydrochlorination and application thereof |
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