CN107321371A - A kind of preparation method of acrylic acid catalyst - Google Patents
A kind of preparation method of acrylic acid catalyst Download PDFInfo
- Publication number
- CN107321371A CN107321371A CN201710389399.0A CN201710389399A CN107321371A CN 107321371 A CN107321371 A CN 107321371A CN 201710389399 A CN201710389399 A CN 201710389399A CN 107321371 A CN107321371 A CN 107321371A
- Authority
- CN
- China
- Prior art keywords
- acrylic acid
- acid catalyst
- preparation
- catalyst
- precipitated liquid
- 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.)
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 36
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000003377 acid catalyst Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 6
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 6
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 6
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 6
- 230000002378 acidificating effect Effects 0.000 claims abstract description 4
- 230000003321 amplification Effects 0.000 claims abstract description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 238000000975 co-precipitation Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 238000003199 nucleic acid amplification method Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims 1
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 abstract description 6
- 238000003556 assay Methods 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012827 research and development Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000006467 substitution reaction 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method of acrylic acid catalyst, investigate in propylene oxidation prepares acrylic acid catalyst preparation process, ammonium molybdate before the speed and precipitated liquid of precipitated liquid addition speed are added during coprecipitation reaction, ammonium metavanadate, influence of the reaction time of ammonium paratungstate three to catalyst performance, and the surface acidity of auxiliary agent improvement catalyst is adjusted by preferred acidic, determine priority control technological parameter in acrylic acid catalyst amplification production, the assay of the 6 150Kg grades of catalyst of batch produced on this condition shows, the yield of acrylic acid is more than 87%, catalyst preparation is reproducible.
Description
Technical field
The present invention relates to a kind of preparation method of acrylic acid catalyst.
Background technology
Acrylic acid is the particularly important basic material and intermediate of modern chemical industry, because its active strong polar molecule,
Unsaturated double-bond and carboxylic acid structure, therefore a variety of polymer formulators for possessing superperformance can be derived, and through emulsion polymerization,
The processing modes such as polymerisation in solution, copolymerization prepare the polymer such as plasticity, crosslinking.
At present, the large-scale plant of whole world industrial production acrylic acid all produces acrylic acid using propylene oxidation technology.In
Petroleum Chemical Engineering Institute of state completes LY-A-9601, LY-A-9602 acrylic acid catalyst R＆D work the nineties, in
Carry out first industrial application within 2003.For being applicable the problem of propylene air speed is low, acrylic acid selectivity is poor, research institute carries out high-altitude
Speed, high selectivity methacrylaldehyde, the research and development of acrylic acid catalyst, have completed lab scale, the research work in pilot scale stage at present.Middle sea
Oily Tianjin Chemical Research ＆ Desing Inst, Shanghai Huayi Acrylic Acid Co., Ltd., Shanghai Petroleum Chemical Engineering Institute are also all being engaged in propylene
The R＆D work of aldehyde, acrylic acid catalyst, but there is not yet its industrialized report.
Therefore, a kind of preparation method of acrylic acid catalyst is worth inquiring into.
The content of the invention
Goal of the invention：The problems such as in order to solve low acrylic acid yield, poor selectivity, unstable catalytic performance, the present invention is carried
Go out each reaction controlling key element in investigation oxidation preparation process, obtain high income, the good, catalyst preparation of selectivity reproducible
Acrylic acid catalyst preparation method.
Technical scheme：In order to solve the above problems, the technical solution adopted in the present invention is：A kind of acrylic acid catalyst
Preparation method, is investigated in propylene oxidation prepares acrylic acid catalyst preparation process, precipitated liquid adds speed during coprecipitation reaction
Speed and precipitated liquid add before ammonium molybdate, ammonium metavanadate, the reaction time of ammonium paratungstate three to catalyst performance
Influence, and the surface acidity of catalyst is improved by preferred acidic adjustment auxiliary agent, determine weight in acrylic acid catalyst amplification production
Point control technological parameter.
Further, the precipitated liquid adds speed and is converted into time for adding to count, and range set is 2-10min.
Further, the reaction time is set as 0.5-5h.
Further, the acid adjustment auxiliary agent is set as A, B, C, D, E, F.
Beneficial effect：A kind of preparation method for acrylic acid catalyst that the present invention is provided, investigates and prepares third in propylene oxidation
In olefin(e) acid catalyst preparation process, molybdic acid before the speed and precipitated liquid of precipitated liquid addition speed are added during coprecipitation reaction
The influence of ammonium, ammonium metavanadate, the reaction time of ammonium paratungstate three to catalyst performance, and changed by preferred acidic adjustment auxiliary agent
The surface acidity of kind catalyst, determines priority control technological parameter in acrylic acid catalyst amplification production, produces on this condition
The assays of 6 150Kg grades of catalyst of batch show that the yield of acrylic acid is more than 87%, catalyst preparation repeatability
It is good.
Embodiment
With reference to embodiment, the present invention is described in further detail：
Embodiment 1：
A kind of preparation method of acrylic acid catalyst, it is coprecipitated in propylene oxidation prepares acrylic acid catalyst preparation process
Precipitated liquid when reacting of forming sediment adds speed and is converted into time for adding to count, and is defined as 2min；Ammonium molybdate, inclined vanadium before precipitated liquid is added
Sour ammonium, the reaction time of ammonium paratungstate three are defined as 0.5h；Acidity adjustment auxiliary agent selection is A.
Embodiment 2：
A kind of preparation method of acrylic acid catalyst, it is coprecipitated in propylene oxidation prepares acrylic acid catalyst preparation process
Precipitated liquid when reacting of forming sediment adds speed and is converted into time for adding to count, and is defined as 5min；Ammonium molybdate, inclined vanadium before precipitated liquid is added
Sour ammonium, the reaction time of ammonium paratungstate three are defined as 1h；Acidity adjustment auxiliary agent selection is D.
Embodiment 3：
A kind of preparation method of acrylic acid catalyst, it is coprecipitated in propylene oxidation prepares acrylic acid catalyst preparation process
Precipitated liquid when reacting of forming sediment adds speed and is converted into time for adding to count, and is defined as 8min；Ammonium molybdate, inclined vanadium before precipitated liquid is added
Sour ammonium, the reaction time of ammonium paratungstate three are defined as 3h；Acidity adjustment auxiliary agent selection is F.
Finally it should be noted that：Above example only not limits technology described in the invention to illustrate the present invention
Scheme, therefore, although this specification with reference to above-mentioned various embodiments to present invention has been detailed description, this
Field it is to be appreciated by one skilled in the art that still can be modified to the present invention or equivalent substitution, and all do not depart from this
The technical scheme of the spirit and scope of invention and improvement, it all should cover in scope of the presently claimed invention.
Claims (4)
1. a kind of preparation method of acrylic acid catalyst, it is characterised in that investigate and prepare acrylic acid catalyst system in propylene oxidation
During standby, during coprecipitation reaction precipitated liquid add speed speed and precipitated liquid add before ammonium molybdate, ammonium metavanadate, secondary
Influence of the reaction time of ammonium tungstate three to catalyst performance, and the surface of catalyst is improved by preferred acidic adjustment auxiliary agent
Acidity, determines priority control technological parameter in acrylic acid catalyst amplification production.
2. a kind of preparation method of acrylic acid catalyst according to claim 1, it is characterised in that：The precipitated liquid is added
Speed is converted into time for adding to count, and range set is 2-10min.
3. a kind of preparation method of acrylic acid catalyst according to claim 1, it is characterised in that：The reaction time sets
It is set to 0.5-5h.
4. a kind of preparation method of acrylic acid catalyst according to claim 1, it is characterised in that：The acid adjustment is helped
Agent is set as A, B, C, D, E, F.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710389399.0A CN107321371A (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of acrylic acid catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710389399.0A CN107321371A (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of acrylic acid catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107321371A true CN107321371A (en) | 2017-11-07 |
Family
ID=60193229
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710389399.0A Pending CN107321371A (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of acrylic acid catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107321371A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1689700A (en) * | 2004-03-25 | 2005-11-02 | 株式会社日本触媒 | Catalyst for production of acrylic acid and process for production of acrylic acid using this catalyst |
| CN102992977A (en) * | 2011-09-08 | 2013-03-27 | 中国石油天然气股份有限公司 | Preparation method of acrolein |
| CN104107697A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Preparation method of acrylic acid catalyst |
-
2017
- 2017-05-27 CN CN201710389399.0A patent/CN107321371A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1689700A (en) * | 2004-03-25 | 2005-11-02 | 株式会社日本触媒 | Catalyst for production of acrylic acid and process for production of acrylic acid using this catalyst |
| CN102992977A (en) * | 2011-09-08 | 2013-03-27 | 中国石油天然气股份有限公司 | Preparation method of acrolein |
| CN104107697A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Preparation method of acrylic acid catalyst |
Non-Patent Citations (1)
| Title |
|---|
| 刘肖飞等: "丙烯氧化制备丙烯酸催化剂研究", 《当代化工》 * |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171107 |