CN85102268A - The Preparation of Catalyst and the regeneration techniques of chlorination system termil fluid bed - Google Patents
The Preparation of Catalyst and the regeneration techniques of chlorination system termil fluid bed Download PDFInfo
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- CN85102268A CN85102268A CN85102268.5A CN85102268A CN85102268A CN 85102268 A CN85102268 A CN 85102268A CN 85102268 A CN85102268 A CN 85102268A CN 85102268 A CN85102268 A CN 85102268A
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- catalyst
- fluid bed
- regeneration
- termil
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Abstract
A kind of by isophthalodinitrile system termil fluid catalyst preparation method and regeneration techniques.Adopt the metal chloride of several different proportions in the charcoal absorption, again through a physical method handle make active good, the life-span long, the load high, be suitable for the catalyst of fluid bed in the multiple-hearth or single fluidized bed usefulness, available again a kind of straightforward procedure is with the decreased activity catalyst regeneration, after the regeneration, active significantly recovery is a kind of of great value production technology.
Description
The invention belongs to a kind of organic catalyst method for making of production chlorination virtue nitrile that is applied to.
More external patents also once announced, adopted one or more metal chloride (chlorides such as iron, copper, zinc or nickel) of charcoal absorption, as the catalyst of producing termil.As: United States Patent (USP) 365267, day special permission 43-22298 and day special permission 43-22589, but above patent was not announced composition and the preparation method and the regeneration techniques of composite catalyst.
The object of the present invention is to provide a kind of Preparation of Catalyst and regeneration techniques that can be applicable to fluid bed in the multiple-hearth or single fluidized bed system termil.
Main points of the present invention are:
1. adopt the metal chloride of active carbon (20～100 order) absorption different proportion, wherein: FeCl
3: 7～8%; ZuCl
2: 0.8～1.2%; GuCl
2: 3.8～4.2%(is 100% in total catalyst weight).
2. temperature was handled 8～12 hours for 80～120 ℃ under negative pressure.
Preparation technology's flow process is as follows:
1. get a certain amount of active carbon (20～100 order).
2. 1/5 the concentrated hydrochloric acid that adds water volume with active carbon equal-volume water boiled one hour, gave a baby a bath on the third day after its birth time with distilled water then.
3. preparation maceration extract: use concentrated hydrochloric acid dissolving FeCl with isopyknic distilled water of active carbon and 1/20 water volume
3, ZnCl
2, CuCl
2
4. adding maceration extract in the active carbon of washing boils dry.
5. fry and do or oven dry.
6. the catalyst of oven dry is put into special device, under negative pressure, temperature is handled for 80～120 ℃ and was made fluid bed catalyst (being called for short the 50# catalyst) in 8～12 hours.
The good catalyst activity that this law makes can be kept long active stabilization period under higher load.Because this law has adopted the suitable ratio metal chloride of absorption on the active carbon, and strict control FeCl
3Adsorbance on active carbon, and carry out application of vacuum at a certain temperature, thereby it is good to make made catalyst activity go up other ratio metal chloride than absorption.The catalyst that this law makes is higher than general fluid catalyst load.The catalyst loading that this law makes is 15 gram isophthalodinitriles/100 gram catalyst hour.No. 10 P834～837 1964 of U.S.'s organic chemistry 22 volumes, the catalyst loading 0.34～0.45 * 10 of the research report of phthalonitrile gas phase catalysis halogenation
-3Mole isophthalodinitrile/gram hour.Because the load of catalyst is directly connected to its life-span and exchange capacity, the low life-span of load can prolong, and exchange capacity can be less.
The catalyst that this law makes is made fluid catalyst in multiple-hearth, at exchange capacity is that 1/35 of loaded catalyst just can guarantee that the outlet conversion ratio maintains 60～75% runnings steady in a long-term, fixed bed is reduced the heavy burdens, qualified products conversion ratio 〉=98%, molecular yield 〉=95%.The catalyst that this law makes makes multiple-hearth running steady in a long-term in the above conditions.
This course of reaction of isophthalodinitrile high temperature gas phase chlorination system termil, be characterized in the temperature height, chlorine and phase transition process are arranged, isophthalodinitrile is a solid, make the termil of solid by catalyst high temperature gas phase chlorination, thereby catalyst is easily enclosed carbide impurity and solid matter, the easy inactivation of catalyst, the method of regenerating behind the catalysqt deactivation of activated carbon types, report is also arranged in the physical data, as: purging, calcination, steam activation etc., but be not reported for the renovation process of this class catalyst.
The present invention adopts simple method, and with the catalyst regeneration after leaving the bed, activity is significantly recovered, and can be used as fluid bed exchange catalyst again.
The main points of catalyst regeneration of the present invention, the catalyst (the outlet conversion ratio is lower than 60% catalyst) that activity is dropped to a certain degree purges through nitrogen, put into regenerator, temperature is 100 ℃～120 ℃ under negative pressure, handled 8～12 hours with physical method, active significantly recover, can be used as the fluid bed exchange again and use catalyst, but the 1/24 stable maintenance fluid bed that per 8 hours exchange capacities are loaded catalyst exports conversion ratio 60%～75%.
Example 1
With FeCl in active carbon (20～100 order) absorption
37.5%, CuCl
24.1%, ZnCl
21.1%(is 100% in the gross weight of catalyst) put into a special device after the catalyst drying formed and vacuumized (residual pressure 80 millimetress of mercury) 10 hours for inherent 110 ℃, make fluid bed 50# catalyst, put into the fluid bed of multiple-hearth.Experimental condition: 861 milliliters of loadings, 450 millimeters of the quiet height of bed, catalyst loading is 15 gram isophthalodinitriles/100 gram catalyst hour, isophthalodinitrile: chlorine=1: the 8(mol ratio), linear speed U=0.24 meter per second, 320 ℃ of temperature, activity stabilized in 300 hours, when activity drops to below 70%, exchange raw catelyst amount was 1/35 of a loadings in per 8 hours, and fluid bed outlet conversion ratio is maintained in 60～75% scopes, and the catalyst of emitting during exchange is put into regenerator and vacuumized (residual pressure 20 millimetress of mercury), temperature is 120 ℃ and handled 8 hours, as fluid catalyst exchange usefulness, exchange capacity was 1/24 of a loadings in per 8 hours, kept fluid bed outlet conversion ratio 60～75%, multiple-hearth final products conversion ratio 98%, molecular yield 〉=95%.
Claims (3)
1, a kind of Preparation of catalysts method and regeneration techniques that is applicable to fluid bed in the multiple-hearth or single fluidized bed chlorination isophthalodinitrile system termil, it is characterized in that charcoal absorption different proportion metal chloride, after the drying, again in an isolated plant under the negative pressure, temperature was handled 8～12 hours for 80～120 ℃, can make the fluid bed catalyst, can be in regenerator behind this catalysqt deactivation, renewable through uniform temperature, pressure treatment.
2, according to claim 1, it is characterized in that controlling on the active carbon the muriatic composition of absorption metal is FeCl
37～8%, CuCl
23.8～4.2%, ZnCl
20.8～1.2%.
3, according to claim 1, it is characterized in that: regeneration is under negative pressure, and temperature is 100～120 ℃ and handled 8～12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85102268.5A CN1006043B (en) | 1985-04-01 | 1985-04-01 | Technology of preparation and regeneration of catalyst for the chlorination process of production of tetrachloro-m-benqenedicyanide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85102268.5A CN1006043B (en) | 1985-04-01 | 1985-04-01 | Technology of preparation and regeneration of catalyst for the chlorination process of production of tetrachloro-m-benqenedicyanide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85102268A true CN85102268A (en) | 1986-09-24 |
| CN1006043B CN1006043B (en) | 1989-12-13 |
Family
ID=4792382
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85102268.5A Expired CN1006043B (en) | 1985-04-01 | 1985-04-01 | Technology of preparation and regeneration of catalyst for the chlorination process of production of tetrachloro-m-benqenedicyanide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1006043B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133523A (en) * | 2011-01-11 | 2011-07-27 | 湘潭大学 | Method for re-activating inactivated catalyst through catalytic chlorination of pyridine nitrile |
| CN107511155A (en) * | 2016-06-15 | 2017-12-26 | 江苏新河农用化工有限公司 | A kind of catalyst for preparing Bravo and its preparation method and application |
| CN108212135A (en) * | 2017-12-29 | 2018-06-29 | 南通泰禾化工股份有限公司 | The recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology |
| CN111870988A (en) * | 2020-07-17 | 2020-11-03 | 江苏新河农用化工有限公司 | Trapping method and trapping system for tetrachloroisophthalonitrile reaction gas |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4612703B2 (en) | 2008-04-02 | 2011-01-12 | シャープ株式会社 | Operating device and image forming apparatus |
-
1985
- 1985-04-01 CN CN85102268.5A patent/CN1006043B/en not_active Expired
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133523A (en) * | 2011-01-11 | 2011-07-27 | 湘潭大学 | Method for re-activating inactivated catalyst through catalytic chlorination of pyridine nitrile |
| CN102133523B (en) * | 2011-01-11 | 2012-11-14 | 湘潭大学 | Method for re-activating inactivated catalyst through catalytic chlorination of pyridine nitrile |
| CN107511155A (en) * | 2016-06-15 | 2017-12-26 | 江苏新河农用化工有限公司 | A kind of catalyst for preparing Bravo and its preparation method and application |
| CN107511155B (en) * | 2016-06-15 | 2020-05-12 | 江苏新河农用化工有限公司 | Catalyst for preparing chlorothalonil and preparation method and application thereof |
| CN108212135A (en) * | 2017-12-29 | 2018-06-29 | 南通泰禾化工股份有限公司 | The recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology |
| CN111870988A (en) * | 2020-07-17 | 2020-11-03 | 江苏新河农用化工有限公司 | Trapping method and trapping system for tetrachloroisophthalonitrile reaction gas |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1006043B (en) | 1989-12-13 |
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