CN1631538A - Regenerating, cleaning and separating method of titanium silicon molecular sieve catalyst - Google Patents
Regenerating, cleaning and separating method of titanium silicon molecular sieve catalyst Download PDFInfo
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- CN1631538A CN1631538A CN 200310110682 CN200310110682A CN1631538A CN 1631538 A CN1631538 A CN 1631538A CN 200310110682 CN200310110682 CN 200310110682 CN 200310110682 A CN200310110682 A CN 200310110682A CN 1631538 A CN1631538 A CN 1631538A
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- sieve catalyst
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Abstract
The invention concerns a separating way of Ti-Si numerator sieve catalyst in the rebirth washing process. Its feature is: In the process of Ti-Si numerator sieve rebirth washing, add the things including catalyst grains, rebirth liquid or washing liquid into the film separating equipment of certain hole diameter, control the press of the pump exit. We get the rebirth liquid or the washing liquid on the permeate side of the film separating equipment, on the exit of the film separating equipment we get the stopping liquid and the catalyst, and they return to birth or washing equipment. Control the vacuum rate of the stopping liquid and the permeate liquid, and control certain flow speed. On some day to press the film tube on the opposite, control certain press, time and time partition.
Description
One, technical field:
The present invention relates to the continuous separation method in a kind of titanium-silicon molecular sieve catalyst regeneration, the washing process.
Two, background technology:
HTS is a kind of new catalytic material that development in recent years is got up, the various organic oxidizing reactions that participate in hydrogen peroxide had unique catalytic performance, the selectivity of product height, the reaction condition gentleness, environmental friendliness, but the oxidation of the hydroxylating of the oxidation of the partial oxidation of the epoxidation of its catalyzed alkene, alkane, alcohols, phenol and benzene and cyclohexanone etc.But the titanium-silicon molecular sieve catalyst particle is little, generally has only 0.2 μ m, is a kind of quasi-nano molecular sieve catalyst, utilizes traditional separation method such as sedimentation separation, centrifugation and conventional filtration separation etc., and effect is all undesirable.
Three, summary of the invention:
The purpose of this invention is to provide the continuous separation method in a kind of titanium-silicon molecular sieve catalyst regeneration washing process.
The present invention is achieved in that in HTS regeneration washing process, the material that will contain pellet type catalyst directly is the membrane separator of 0.05～0.2 μ m with pump adding film pore, the controlled filter temperature is 20～90 ℃, and the pressure reduction with per-meate side in the film pipe is no more than 0.10～0.60Mpa.Raffinate after the per-meate side of membrane separator is regenerated or washed, obtain containing in the outlet of membrane separator under the effect of trapped fluid at pressure reduction of catalyst and return regeneration carrying out washing treatment device, the trapped fluid that comes out from membrane separator and the volume ratio of penetrating fluid were controlled at 1.5: 1～5.5: 1, the crossflow velocity of material in membrane separator is 1～8m/s, and the best is 2～5m/s.Regularly the film pipe is recoiled, the recoil time interval is 1～60 minute, and the best is 2～30 minutes, 1～10 second flow container feed liquor time of buffering, pressure reduction in recoil nitrogen and the film pipe is controlled at 0.10～0.60MPa, and the recoil duration is 0.5～5 second, and the best is 1～3 second.So circulation can be carried catalyst concn dense to the highest by 20% (percentage by weight).
Good effect of the present invention is to realize separating fully of catalyst and material, can guarantee that the continous-stable of regeneration and washing carries out.Its separating technology is directly to adopt the ceramic membrane separator or combine with other method, the material that will contain catalyst is squeezed into membrane separation device with pump, at the per-meate side of membrane separator obtain regenerating raffinate or washing raffinate, outlet at membrane separator obtains trapped fluid and catalyst, regeneration and the washing of finishing whole catalyst by new regeneration of continuous interpolation and cleaning treatment liquid.Its characteristics are that circulating filtration combines with the recoil operation, and simple to operation, the cycle is long, and good separating effect after testing, does not contain catalyst granules in the penetrating fluid, solved the difficult problem of catalyst separation effectively.
Four, description of drawings:
Fig. 1 is the continuous separation technology schematic flow sheet in the regeneration of film device titanium-silicon molecular sieve catalyst.
As shown in the figure: the material that contains pellet type catalyst in the regeneration carrying out washing treatment jar 1 is squeezed into membrane separator 7 with pump 3 through valve 5, flowmeter 6 through valve 2, and by the aperture control crossflow velocity of control valve 4, the trapped fluid that contains catalyst returns regeneration carrying out washing treatment jar.The penetrating fluid of membrane separator 7 is metered into residual liquid tank 19 by flowmeter 18 after ball valve 11 is regulated flow.Regularly with nitrogen membrane separator is recoiled, nitrogen recoils through the per-meate side of valve 16, gas buffer jar 17, valve 12 and 13 pairs of film pipes of fluid cushion jar, and open valve 14 exhausts regularly are to the fluid infusion of liquid surge tank.After treating that the catalyst regeneration washing is finished, shut off valve 5,8 and nitrogen recoil, open valve 9 is with catalyst barrelling to 10.
Five, the specific embodiment:
Embodiment 1: film device is applied to the isolated by filtration after the acid solution processing in the HTS regenerative process.The regeneration treatment fluid that will contain PH＜1 of 10kg water, 0.25kg titanium-silicon molecular sieve catalyst, at room temperature through pump 3 pressure-raisings by gate valve 5 and flowmeter 6 squeeze into membrane separator 7 contain from, the trapped fluid that contains catalyst returns regeneration carrying out washing treatment jar 1, and penetrating fluid enters residual liquid tank 19 through flowmeter 18.The proportion control of trapped fluid and penetrating fluid was at 3: 1, and crossflow velocity is 3.3m/s.Regularly with nitrogen two film pipes are recoiled, the recoil time interval controls is 300 seconds, and the duration of at every turn recoiling is 1 second, and the pressure reduction in recoil nitrogen and the film pipe is controlled at 0.4～0.5MPa.Nitrogen recoils through the per-meate side that gas buffer jar 17 and fluid cushion jar 13 enter two film pipes.When every interval 600 seconds is opened gate valve 14 and is 3～5 seconds.Through detecting penetrating fluid, do not find catalyst granules.
Embodiment 2: film device is applied to the isolated by filtration after aqueous slkali is handled in the HTS regeneration.The regeneration treatment fluid that will contain PH＞12 of 14.kg water, 0.5kg titanium-silicon molecular sieve catalyst, squeeze into membrane separator 7 through pump 3 pressure-raisings by gate valve 5 and flowmeter 6 at 60 ℃, the trapped fluid that contains catalyst returns regeneration carrying out washing treatment jar, and penetrating fluid enters residual liquid tank 19 through flowmeter 18.The proportion control of trapped fluid and penetrating fluid was at 4: 1, and crossflow velocity is 2.3m/s.Regularly with nitrogen two film pipes are recoiled, the recoil time interval controls is 200 seconds, and the duration of at every turn recoiling is 2 seconds, and the pressure reduction in recoil nitrogen and the film pipe is controlled at 0.1～0.3MPa.Nitrogen recoils through the per-meate side that gas buffer jar 17 and fluid cushion jar 13 enter two film pipes.When every interval 300 seconds is opened gate valve 14 and is 1～2 second.Through detecting penetrating fluid, do not find catalyst granules.
Embodiment 3: film device is applied to the isolated by filtration after the HTS solvent wash is handled.To contain 11.3kg water, 4Kg acetone, the 2Kg tert-butyl alcohol and 0.7kg titanium-silicon molecular sieve catalyst treatment fluid, squeeze into membrane separator 7 through pump 3 pressure-raisings by gate valve 5 and flowmeter 6 at 80 ℃, the trapped fluid that contains catalyst returns regeneration carrying out washing treatment jar, and penetrating fluid enters residual liquid tank 19 through flowmeter 18.The proportion control of trapped fluid and penetrating fluid was at 5: 1, and crossflow velocity is 4m/s.Regularly with nitrogen two film pipes are recoiled, the recoil time interval controls is 240 seconds, and the duration of at every turn recoiling is 2 seconds, and the pressure reduction in recoil nitrogen and the film pipe is controlled at 0.2～0.4MPa.Nitrogen recoils through the per-meate side that gas buffer jar 17 and fluid cushion jar 13 enter two film pipes.When every interval 240 seconds is opened gate valve 14 and is 1～2 second.Through detecting penetrating fluid, do not find catalyst granules.
Embodiment 4: film device is applied to the isolated by filtration after the HTS water washing is handled and concentrates.To contain 20kg water, 0.9kg titanium-silicon molecular sieve catalyst treatment fluid, and squeeze into membrane separator 7 through pump 3 pressure-raisings by gate valve 5 and flowmeter 6 under 30 ℃, the trapped fluid that contains catalyst returns regeneration carrying out washing treatment jar, and penetrating fluid enters residual liquid tank 19 through flowmeter 18.When catalyst was concentrated into concentration and is 20%, closing gate valve 5,8 and nitrogen recoil were opened gate valve 9, with catalyst barrelling to 10.The proportion control of trapped fluid and penetrating fluid was at 3.5: 1, and crossflow velocity is 3m/s.Regularly with nitrogen two film pipes are recoiled, the recoil time interval controls is 120 seconds, and the duration of at every turn recoiling is 2 seconds, and the pressure reduction in recoil nitrogen and the film pipe is controlled at 0.2～0.4MPa.Nitrogen recoils through the per-meate side that gas buffer jar 17 and fluid cushion jar 13 enter two film pipes.When every interval 240 seconds is opened gate valve 14 and is 2～5 seconds.Through detecting penetrating fluid, do not find catalyst granules.
Claims (4)
1, a kind of titanium-silicon molecular sieve catalyst regeneration washing separating method is characterized in that: the material after will regenerating, washing is with filtering in the pump adding membrane separator, and filtration temperature is 20～90 ℃, and the pressure reduction with per-meate side in the film pipe is no more than 0.10～0.60Mpa; Raffinate after the per-meate side of membrane separator is regenerated or washed, obtain containing in the outlet of membrane separator under the effect of trapped fluid at pressure reduction of catalyst and return regeneration carrying out washing treatment device, the trapped fluid that comes out from membrane separator and the volume ratio of penetrating fluid were controlled at 1.5: 1～5.5: 1, the crossflow velocity of material in membrane separator is 1～8m/s, regularly the film pipe is recoiled, the recoil time interval is 1～60 minute, 1～10 second flow container feed liquor time of buffering, pressure reduction in recoil nitrogen and the film pipe is controlled at 0.10～0.60MPa, and the recoil duration is 0.5～5 second.
2, the separation method of a kind of titanium-silicon molecular sieve catalyst regeneration according to claim 1, washing, it is characterized in that: material crossflow velocity the best in membrane separator is 2～5m/s.
3, the separation method of a kind of titanium-silicon molecular sieve catalyst regeneration according to claim 1, washing, it is characterized in that: time interval the best that the film pipe is recoiled is 2～30 minutes.
4, the separation method of a kind of titanium-silicon molecular sieve catalyst regeneration according to claim 1, washing, it is characterized in that: recoil duration the best is 1～3 second.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310110682 CN1631538A (en) | 2003-12-22 | 2003-12-22 | Regenerating, cleaning and separating method of titanium silicon molecular sieve catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310110682 CN1631538A (en) | 2003-12-22 | 2003-12-22 | Regenerating, cleaning and separating method of titanium silicon molecular sieve catalyst |
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| CN1631538A true CN1631538A (en) | 2005-06-29 |
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| CN 200310110682 Pending CN1631538A (en) | 2003-12-22 | 2003-12-22 | Regenerating, cleaning and separating method of titanium silicon molecular sieve catalyst |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314596B (en) * | 2007-05-31 | 2011-04-20 | 中国石油化工股份有限公司 | Method for continuous preparation of epoxypropane |
| CN102145301A (en) * | 2010-12-29 | 2011-08-10 | 中国天辰工程有限公司 | Method for washing micron-level molecular sieve containing nano impurities |
| CN101455980B (en) * | 2007-12-13 | 2011-11-30 | 中国石油化工股份有限公司 | Regeneration method of oxidation-reaction inactive titanium silicon molecule sieve catalyst |
| CN102941117A (en) * | 2012-11-13 | 2013-02-27 | 中国石油化工股份有限公司 | Regeneration method of titanium-silicon molecular sieve catalyst |
| CN103084204A (en) * | 2011-10-27 | 2013-05-08 | 中国石油化工股份有限公司 | Method for treating slurry containing nanometer beta molecular sieve |
| CN113428871A (en) * | 2021-07-12 | 2021-09-24 | 宁夏美邦寰宇化学有限公司 | Separation and purification method and separation and purification system of titanium-silicon molecular sieve |
-
2003
- 2003-12-22 CN CN 200310110682 patent/CN1631538A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314596B (en) * | 2007-05-31 | 2011-04-20 | 中国石油化工股份有限公司 | Method for continuous preparation of epoxypropane |
| CN101455980B (en) * | 2007-12-13 | 2011-11-30 | 中国石油化工股份有限公司 | Regeneration method of oxidation-reaction inactive titanium silicon molecule sieve catalyst |
| CN102145301A (en) * | 2010-12-29 | 2011-08-10 | 中国天辰工程有限公司 | Method for washing micron-level molecular sieve containing nano impurities |
| CN103084204A (en) * | 2011-10-27 | 2013-05-08 | 中国石油化工股份有限公司 | Method for treating slurry containing nanometer beta molecular sieve |
| CN103084204B (en) * | 2011-10-27 | 2015-03-25 | 中国石油化工股份有限公司 | Method for treating slurry containing nanometer beta molecular sieve |
| CN102941117A (en) * | 2012-11-13 | 2013-02-27 | 中国石油化工股份有限公司 | Regeneration method of titanium-silicon molecular sieve catalyst |
| CN113428871A (en) * | 2021-07-12 | 2021-09-24 | 宁夏美邦寰宇化学有限公司 | Separation and purification method and separation and purification system of titanium-silicon molecular sieve |
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