CN102294274A - Continuous production technology for chloridizing and reducing heavy metal catalyst - Google Patents
Continuous production technology for chloridizing and reducing heavy metal catalyst Download PDFInfo
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- CN102294274A CN102294274A CN2010102054811A CN201010205481A CN102294274A CN 102294274 A CN102294274 A CN 102294274A CN 2010102054811 A CN2010102054811 A CN 2010102054811A CN 201010205481 A CN201010205481 A CN 201010205481A CN 102294274 A CN102294274 A CN 102294274A
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- chlorination
- metal catalyst
- carbon tetrachloride
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Abstract
The invention relates to a continuous production technology for chloridizing and reducing a heavy metal catalyst, and the innovation point is characterized in that the method comprises the following steps: the heavy metal catalyst is placed a chlorination and reduction reactor, cycle hot-air is introduced in the reactor, carbon tetrachloride is injected from the top of the reactor and uniformly dispersed in cycle hot-air, carbon tetrachloride is performed a chlorination reaction to prepare a chloridized updated oxidation state catalyst; cycle hot-air is flow out from the bottom of the reactor when the chlorination reaction is carried out, a few residual carbon tetrachloride gas brought by hot-air is introduced in a dechlorination reactor equipped with a antichlor, the residual carbon tetrachloride is removed; a chloridizing and reducing reactor is carried out a nitrogen displacement and then hydrogen is introduced, hydrogen is performed a reduction reaction with heavy metal catalyst for reducing the heavy metal oxide in the catalyst to a heavy metal simple substance, a reduction state catalyst which takes the heavy metal simple substance as an active component. The invention has the advantages that the heavy metal catalyst performed a chloridizing and reducing reaction which not require transferring the raw materials, so that the production efficiency can be raised and the catalyst waste can be minimized, the residual carbon tetrachloride is removed by the dechlorination reactor which has no pollution to atmosphere.
Description
Technical field
The present invention relates to a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for.
Background technology
Noble metal catalyst be petrochemical industry, fine chemistry industry and medication chemistry extensively quoted a kind of be the catalysis material of active component with the noble metal composition.Noble metal obtains using always in catalyst platinum, palladium, rhodium, silver, a ruthenium etc., wherein most widely used with platinum, palladium, rhodium especially.Their electron orbit does not all fill up, and the surface is the adsorption reaction thing easily, and intensity is moderate, be beneficial to and form middle " reactive compound ", have advantages of high catalytic activity, also have comprehensive good characteristics such as high temperature resistant, anti-oxidant, corrosion-resistant simultaneously, become most important catalyst material.The production of the raw catelyst of noble metal catalyst and the regeneration of old catalyst generally all will be upgraded and two technical process of hydrogen reducing through superchlorination, and catalyst could obtain excellent catalytic activity.
Traditional process adopts carries out earlier the chlorination renewal with catalyst in vertical cylindrical heater, catalyst is transferred to carried out hydrogen reducing in another reactor then; Production cycle is long, and efficient is low, and loss is big, and labour intensity is big; In chlorination process, superfluous chlorine directly discharges in air, and environmental pollution is big.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of production efficiency height, low noble metal catalyst chlorination, the reduction continuous production processes of pollution.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for, its innovative point is that processing step is: with described noble metal catalyst and carbon tetrachloride place be connected with circulation, temperature carried out chlorination reaction at least 2 hours at chlorination, the reduction reactor of 450 ℃-570 ℃ hot-air, made the oxidized catalyst that chlorination is upgraded; Again the hot-air in chlorination, the reduction reactor is carried out feeding hydrogen behind the nitrogen replacement, carry out reduction reaction with noble metal catalyst, make the metal oxide containing precious metals in the noble metal catalyst be reduced into precious metal simple substance, thus obtain with the precious metal simple substance be active component go back the ortho states catalyst.
Further, after chlorination reaction, contain a spot of carbon tetrachloride gas in the hot-air of described circulation, its method of removing carbon tetrachloride gas is: the hot-air that will contain a small amount of carbon tetrachloride gas feeds and is equipped with in the dechlorination reaction device of antichlor, and the carbon tetrachloride of remnants is removed.
Further, described antichlor is: the TL-10 high-temperature dechlorinating agent.
Further, described carbon tetrachloride injection rate is 2.0-100.0 kilogram per hour.
Further, with the oxygen in nitrogen replacement chlorination, the reduction reactor, after the displacement, the volume content of oxygen is less than or equal to 0.5%.
Further, described hydrogen purity is more than or equal to 93%.
Further, the temperature of described reduction reaction is at least 1 hour 450 ℃-530 ℃ reaction time.
Further, the mass ratio of described carbon tetrachloride and noble metal catalyst is 0.1-5.0.
The invention has the advantages that: noble metal catalyst carries out chlorination, reduction reaction in reactor, need not to carry out the transfer of material, improved production efficiency, reduced the waste of catalyst, remaining carbon tetrachloride removes by the dechlorination reaction device, can not cause the pollution of atmosphere.
The specific embodiment
Embodiment 1:
At first, with the 1000kg platinum catalyst, place chlorination, in the reduction reactor, be connected with the circulating air after heater via heats in the reactor, when the platinum catalyst material layer temperature reaches 450 ℃, per hour 10.0 in reactor, to inject carbon tetrachloride liquid 2 hours to the speed of 30.0kg, after its distributor gasification by reactor head disperses, be dispersed in the hot-air of circulation, in reactor under 450-530 ℃ of the platinum catalyst material layer temperature, chlorination reaction obtained the platinum catalyst that chlorination is upgraded more than 2 hours after the reaction, the chlorinity in the catalyst can reach 1.0% (m) to 3.0% (m).
By in the dechlorination reaction device that antichlor is housed, antichlor TL-10 high-temperature dechlorinating agent is with the complete absorbing and removing of carbon tetrachloride with circulating air for residual carbon tetrachloride;
Next, with the air in nitrogen replacement chlorination, the reduction reactor, after being not more than 0.5% to volume content, feeding purity is the hydrogen more than 93%, in reaction temperature is under the 460-510 ℃ of condition, the catalyst generation reduction reaction after the chlorination that obtains with chlorination process is upgraded, and reaction is more than 1 hour, the oxide of platinum is reduced to simple substance platinum in the catalyst, makes the platinum catalyst of going back ortho states.
Embodiment 2:
With the 600kg palladium catalyst, place chlorination, reduction reactor, be connected with the circulating air after heater via heats in the reactor, when the palladium catalyst material layer temperature reaches 420 ℃, per hour 3.0 in reactor, to inject carbon tetrachloride liquid 2 hours to the speed of 10.0kg, after its distributor gasification by reactor head disperses, be dispersed in the hot-air of circulation, under temperature 450-530 ℃, chlorination reaction is more than 1 hour, obtain the palladium catalyst that chlorination is upgraded after the reaction, the chlorinity in the catalyst can reach 0.5% (m) to 2.0% (m).
By in the dechlorination reaction device that antichlor TL-10 high-temperature dechlorinating agent is housed, antichlor is with the complete absorbing and removing of carbon tetrachloride with circulating air for residual carbon tetrachloride;
Again with system with nitrogen all thoroughly replace be not more than 0.5% to volume of air content after, feeding purity is the hydrogen more than 93%, in reaction temperature is under the 460-510 ℃ of condition, catalyst generation reduction reaction after the chlorination that obtains with chlorination process is upgraded, reaction is more than 1 hour, the oxide of palladium is reduced to the simple substance palladium in the catalyst, makes the palladium catalyst of going back ortho states.
Embodiment 3:
With the 400kg ruthenium catalyst, place chlorination, in the reduction reactor, be connected with the circulating air after heater via heats in the reactor, when the ruthenium catalyst material layer temperature reaches 420 ℃, per hour 3.0 in reactor, to inject carbon tetrachloride liquid 2 hours to the speed of 10.0kg, after its distributor gasification by reactor head disperses, be dispersed in the hot-air of circulation, keep the material layer temperature of ruthenium catalyst in reactor at 420-500 ℃, chlorination reaction is more than 1 hour, obtain the ruthenium catalyst that chlorination is upgraded after the reaction, the chlorinity in the catalyst can reach 0.5% (m) to 2.0% (m).
By in the dechlorination reaction device that antichlor TL-10 high-temperature dechlorinating agent is housed, antichlor is with the complete absorbing and removing of carbon tetrachloride with circulating air for residual carbon tetrachloride;
Again with system with nitrogen all thoroughly replace be not more than 0.5% to volume content after, feeding purity is the hydrogen more than 93%, in reaction temperature is under the 420-480 ℃ of condition, catalyst generation reduction reaction after the chlorination that obtains with chlorination process is upgraded, reaction is more than 1 hour, the oxide of ruthenium is reduced to the simple substance ruthenium in the catalyst, makes the ruthenium catalyst of going back ortho states.
Claims (8)
1. one kind is used for noble metal catalyst chlorination, reduction quantity-produced technology, it is characterized in that processing step is: with described noble metal catalyst and carbon tetrachloride place be connected with circulation, temperature is at 450 ℃---chlorination, the reduction reactor of 570 ℃ hot-air carried out chlorination reaction at least 2 hours, made the oxidized catalyst that chlorination is upgraded; Again the hot-air in chlorination, the reduction reactor is carried out feeding hydrogen behind the nitrogen replacement, carry out reduction reaction with noble metal catalyst, make the metal oxide containing precious metals in the noble metal catalyst be reduced into precious metal simple substance, thus obtain with the precious metal simple substance be active component go back the ortho states catalyst.
2. a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for according to claim 1, it is characterized in that: after chlorination reaction, contain a spot of carbon tetrachloride gas in the hot-air of described circulation, its method of removing carbon tetrachloride gas is: the hot-air that will contain a small amount of carbon tetrachloride gas feeds and is equipped with in the dechlorination reaction device of antichlor, and the carbon tetrachloride of remnants is removed.
3. a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for according to claim 2, it is characterized in that: described antichlor is: the TL-10 high-temperature dechlorinating agent.
4. a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for according to claim 1 is characterized in that: described carbon tetrachloride injection rate is per hour 2.0---100.0 kilograms.
5. a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for according to claim 1, it is characterized in that: with the oxygen in nitrogen replacement chlorination, the reduction reactor, after the displacement, the volume content of oxygen is less than or equal to 0.5%.
6. a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for according to claim 5, it is characterized in that: described hydrogen purity is more than or equal to 93%.
7. a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for according to claim 1, it is characterized in that: the temperature of described reduction reaction is at least 1 hour 450 ℃-530 ℃ reaction time.
8. a kind of noble metal catalyst chlorination, reduction quantity-produced technology of being used for according to claim 1, it is characterized in that: the mass ratio of described carbon tetrachloride and noble metal catalyst is 0.1---5.0.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102054811A CN102294274A (en) | 2010-06-22 | 2010-06-22 | Continuous production technology for chloridizing and reducing heavy metal catalyst |
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| CN2010102054811A CN102294274A (en) | 2010-06-22 | 2010-06-22 | Continuous production technology for chloridizing and reducing heavy metal catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107096577A (en) * | 2017-06-21 | 2017-08-29 | 南通金源催化剂有限公司 | The reduction of low temperature isomerization catalyst, chlorination integrated apparatus |
| CN108499615A (en) * | 2017-06-21 | 2018-09-07 | 南通金源催化剂有限公司 | The high temperature circulation chloridization process of low temperature isomerization catalyst |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008082534A2 (en) * | 2006-12-20 | 2008-07-10 | Saudi Basic Industries Corporation | Regeneration of platinum-germanium zeolite catalyst |
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2010
- 2010-06-22 CN CN2010102054811A patent/CN102294274A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008082534A2 (en) * | 2006-12-20 | 2008-07-10 | Saudi Basic Industries Corporation | Regeneration of platinum-germanium zeolite catalyst |
Non-Patent Citations (1)
| Title |
|---|
| 李生运等: "催化重整系列脱氯剂的研究与应用", 《石油炼制与化工》, vol. 37, no. 2, 28 February 2006 (2006-02-28) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107096577A (en) * | 2017-06-21 | 2017-08-29 | 南通金源催化剂有限公司 | The reduction of low temperature isomerization catalyst, chlorination integrated apparatus |
| CN108499615A (en) * | 2017-06-21 | 2018-09-07 | 南通金源催化剂有限公司 | The high temperature circulation chloridization process of low temperature isomerization catalyst |
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Application publication date: 20111228 |