CN103028431A - Cleaner production process for molecular sieve catalytic cracking catalyst - Google Patents
Cleaner production process for molecular sieve catalytic cracking catalyst Download PDFInfo
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- CN103028431A CN103028431A CN2012105786350A CN201210578635A CN103028431A CN 103028431 A CN103028431 A CN 103028431A CN 2012105786350 A CN2012105786350 A CN 2012105786350A CN 201210578635 A CN201210578635 A CN 201210578635A CN 103028431 A CN103028431 A CN 103028431A
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- molecular sieve
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Abstract
The invention discloses a cleaner production process for a molecular sieve catalytic cracking catalyst. The process comprises the steps of: (1) mixing raw materials for synthesizing a molecular sieve, gelatinizing, crystallizing, filtering, washing with water, removing sodium alternatively with ammonium and rare earth, and obtaining the modified molecular sieve or molecular sieve catalytic cracking catalyst, (2) mixing water for washing a molecular sieve crystallized filtering stock and/or a crystallized material with ammonia nitrogen waste water generated during a molecular sieve exchanging course to act as a spray washing solution of a spray washing tower for spray granulation exhaust gas of the catalyst, (3) adding acidized aluminum salt or an acid solution into a spray recovering solution obtained in Step (2), gelatinizing, filtering, discharging filtrate, taking filter residue as a raw material for synthesizing the molecular sieve, and returning to Step (1). With the adoption of the process, while the qualified catalytic cracking catalyst is prepared, the waste water with high ammonia nitrogen content generated during the course can meet the standard and be discharged directly at very low operating cost, and silicon compounds in the waste water can be fully recovered and recycled.
Description
Technical field
The present invention relates to a kind of production technology of synthetic zeolite catalysts cracking catalyst, more particularly, relate to a kind of production technology of synthetic zeolite catalysts cracking catalyst of low ammonia nitrogen discharging.
Background technology
The catalytic cracking catalyst production technology is divided two classes substantially at present: gel method binding type and in-situ crystallization type.The former is siliceous with waterglass, sodium metaaluminate, aluminum sulfate and directed agents or other, aluminium compound is mixed into glue, the intensification crystallization is synthesized the NaY molecular sieve, then filter, wash, and carry out ammonium and rare earth exchanged and take off sodium and obtain modified molecular screen, at last modified molecular screen and carrier, binding agent are mixed into glue, mist projection granulating becomes microspherical catalyst.Its crystallization material filtrated stock and washing water mixing add returns crystallization system (the NaY crystallization mother liquor prepares the Discussion on Technology of Alusil, Zou Lingfeng, " Industrial Catalysis ", vol.10 (6), 2002) after aluminium salt is made silica-alumina gel.The latter mixes making beating with clay and binding agent first, mist projection granulating becomes microballoon, with waterglass, alkali and directed agents or other silicon-aluminum containing compound, the synthetic NaY molecular sieve of intensification in-situ crystallization, then filter, wash after the high-temperature roasting, and carry out ammonium and rare earth exchanged and take off sodium and obtain microspherical catalyst.The all or part of crystallization system of directly returning of its crystallization material mother liquor.Its crystallization washing water and/or partially-crystallized mother liquor add and filter filtrate discharge after acidifying aluminium salt or acid solution become glue.Two types of catalytic cracking catalyst production processes all adopt excessive ammonium salt exchange modification, therefore produce the technique waste water that contains a large amount of ammonia nitrogen substances, ammonia-nitrogen content is generally 4000～10000 μ g/g in its ammonium exchange process filtrate, and ammonia-nitrogen content is generally 150～1500 μ g/g in the rear washings of exchange.If these ammonia nitrogen waste waters enter water body, easily cause algae and other microorganism amount reproduction in the water, form the serious environmental problems that body eutrophication pollutes.It is 15 μ g/g that there are strict standard, national grade one discharge standard in China to ammonia nitrogen in sewage discharging, and secondary discharge standard is 50 μ g/g.
The synthetic zeolite catalysts cracking catalyst manufacturer is administered main alkali stripping or the technology such as stripping, film separation and biochemical denitrification of adding that adopt to the Coal Gas Washing Cycling Water ammonia nitrogen.Though it is ripe to add alkali blow-off method treatment technology, need to consume a large amount of steam and alkali, operating cost is high, and equipment corrosion is serious, and is difficult to ammonia nitrogen in the waste water is down to below the 200 μ g/g.Membrane separation process is only applicable to the ammonia nitrogen of the little water yield and processes.Biochemical process is difficult to realize for not having carbon source and high ammonia-nitrogen content waste water system.In addition, absorption exchange process, chemical precipitation method, electrochemical process have a large amount of bibliographical informations, but all have the shortcomings such as investment is large, complicated operation, operating cost height.Do not have also at present that a kind of flow process is simple, reduced investment, technology maturation, control is convenient and the processing synthetic zeolite catalysts cracking Catalyst Production of non-secondary pollution in high efficient, the economical plan that contains ammonia-nitrogen sewage.
The Lanzhou Petrochemical catalyst plant adopt add alkali air stripping and ABFT process integration process produce in its Catalyst Production process contain waste liquor of ammonium (" Industrial Catalysis ", 14 (8), 27～30,2006), operating cost is high.
The method that Chinese patent CN1948191A adopts counter-infiltration to separate combination with film is processed the catalyst ammonia nitrogen waste water.
Chinese patent CN1958471A adopts stripping deamination and biochemical processing method to process oil refining catalyst and produces the middle and high concentration ammonia nitrogen waste water.
Chinese patent CN1485281A adopts the 13X molecular sieve to process ammonia nitrogen waste water, and molecular sieve adopts the regeneration of 20% sodium chloride solution.
Chinese patent CN1274406C adopts NaY molecular sieve and aluminum hydroxide solid elastomer powder, the sesbania powder, the adsorbent of organic acid and inorganic acid mixing moulding preparation removes ammonia nitrogen in the waste water with the fixed bed form, and adsorbent adopts the regeneration of 1～20% sodium carbonate liquor, and adsorption capacity can be recovered more than 90%.
Chinese patent CN100497174C adopts the conventional method synthesis zeolite, and the nitrogen-containing wastewater of the exchange of molecular sieve ammonium and washing generation is contacted with the silica-alumina gel that molecular sieve mother solution adds the formation of aluminium salt, thereby reduces ammonia-nitrogen content in the waste water.Contain the crystallization process that the ammonia gel is back to Zeolite synthesis.But above-mentioned gel adsorption capacity is low, be not suitable for the wastewater treatment of high strength ammonia nitrogen content, only can process the very fraction high ammonia-nitrogen wastewater that produces in the catalytic cracking catalyst production process, and height contained that the ammonia gel adds the crystallization system and the crystallization that heats up after to additionally increase air and/or steam stripping process, highly in addition contain the quality that the reuse of ammonia gel may affect synthesis of molecular sieve greatly.
Chinese patent 200910047060.8 adopts adverse current ammonium exchange more than three grades, sodium that can be in removing molecular sieve, sodium content is reached in the technological requirement, and the ammonia nitrogen in waste water of discharging is reduced greatly.But need increase or change belt filter in existing catalyst factory, invest larger.
Summary of the invention
The objective of the invention is for prior art not enoughly, a kind of easy and catalytic cracking catalyst process for cleanly preparing that operating cost is low is provided.Technique of the present invention may further comprise the steps:
(1) raw material of synthetic zeolite catalyst being mixed into glue, crystallization, filtration, washing, ammonium and rare earth exchanged takes off sodium and obtains modified molecular screen or synthetic zeolite catalysts cracking catalyst;
(2) ammonia nitrogen waste water that Crystallization of Zeolite filtrated stock and/or crystallization material washing water and molecular sieve exchange process is produced mixes the spray washing liquid as the spray scrubber of catalyst mist projection granulating tower tail gas, stripping goes out the ammonia nitrogen in the spray washing liquid in the dust in removing mist projection granulating tower tail gas, the spray that obtains low ammonia-nitrogen content reclaims liquid, connect ammonia absorber behind the spray scrubber, the ammonia absorber absorption liquid is as ammonium in the step (1) and rare earth exchanged liquid or batching;
(3) acidifying aluminium salt or acid solution are added the resulting spray recovery of step (2) liquid, stir into glue, filtration, filtrate discharge, filter residue returns step (1) as the synthesis of molecular sieve raw material.
The ammonia nitrogen waste water mixed proportion that the described Crystallization of Zeolite filtrated stock of step (2) and/or crystallization material washing water and molecular sieve exchange process produce is determined according to the pH value of mixed liquor, the pH value is 9.5～13.0, so that ammonium hydroxide and the ammonia of its mineralized nitrogen for being separated by stripping.
The ammonia-nitrogen content that the temperature of the described spray scrubber of step (2) and gas liquid ratio reclaim in liquid and step (3) filtrate according to drip washing is determined, make preferably that ammonia-nitrogen content is lower than 50 μ g/g in step (3) filtrate, make more preferably that ammonia-nitrogen content is lower than 15 μ g/g in step (3) filtrate.
The described ammonia absorber of step (2) adopts acid water as absorption liquid, and described acid is one or more in sulfuric acid, nitric acid, the hydrochloric acid.
The acid of step (3) described acidifying aluminium salt or acid solution is selected from one or more in sulfuric acid, hydrochloric acid, the nitric acid.Aluminium salt is selected from one or more in aluminum sulfate, aluminium chloride, the aluminum nitrate.The addition of described acidifying aluminium salt or acid solution is definite according to pH value after becoming glue, and the pH value is 7.0～11.0.
Adopt technique provided by the invention, synthetic zeolite catalysts cracking catalyst producer is not increasing under the prerequisite of equipment investment and operating cost substantially, obtaining qualified synthetic zeolite catalysts cracking catalyst prod simultaneously, the industrial wastewater ammonia-nitrogen content of the high ammonia-nitrogen content of discharging is reduced greatly, directly qualified discharge.For example, the ammonia-nitrogen content that is derived from the exchange of molecular sieve ammonium and washing is the industrial wastewater of 6541 μ g/g, and ammonia nitrogen can be to 30 μ g/g in the discharge water after PROCESS FOR TREATMENT of the present invention.In addition, full recycling use of silicon compound in the waste water.And existing catalytic cracking molecular sieve catalyst manufacturer adopts and adds alkali air stripping or stripping and add biochemical process and process high ammonia-nitrogen wastewater, 20～25 kilograms in waste water hydro-oxidation sodium per ton, only this item wastewater treatment expense per ton is (CN1958471A) more than 50 yuan, and wastewater treatment need 150～200 kg of vapor per ton heating, cost is more than 30 yuan.
Description of drawings
Fig. 1 is the process for cleanly preparing schematic diagram of in-situ crystallization type catalytic cracking catalyst provided by the invention.
Fig. 2 is the process for cleanly preparing schematic diagram of gel method binding type catalytic cracking catalyst provided by the invention.
The specific embodiment
Be described in further detail technical scheme of the present invention below in conjunction with embodiment, protection scope of the present invention is not limited to the following specific embodiment.
Embodiment 1
Process flow diagram such as Fig. 1 of certain company in-situ crystallization catalytic cracking catalyst factory.By this flow process, kaolin and waterglass are mixed making beating by 100: 10 (mass ratio), solid content 40%, then pumping into mist projection granulating tower mist projection granulating is microballoon; Again 3 parts of 920 ℃ of calcined kaolin microspheres and 1 part of 850 ℃ of calcined kaolin microspheres and waterglass, alkali, directed agents are mixed and be warming up to the synthetic NaY type molecular sieve of 95 ℃ of in-situ crystallizations, degree of crystallinity 45%; Containing NaY type molecular sieve solid-liquid mixed liquor filters and washing through the belt filter, collect crystallization mother liquor and crystallization material washing water, filter cake is through ammonium and rare earth-iron-boron repeatedly exchanges and sodium is taken off in roasting, and last expansion drying obtains the catalytic cracking catalyst finished product, sodium oxide content 0.25%.Collect exchange filtrate mixed liquor, ammonia-nitrogen content is 6541 μ g/g.Crystallization material washing water and partially-crystallized mother liquor are added exchange filtrate mixed liquor, the pH value that makes its mixed liquor is 12.0, then with the spray washing liquid of this mixed liquor as the spray scrubber of mist projection granulating tower tail gas, the temperature that spray reclaims liquid is 90 ℃, and ammonia-nitrogen content is 232 μ g/g; Again Sulfated aluminum sulfate solution is added drip washing and reclaim liquid, making its pH value is 8.5, and aging 1 hour, press filtration obtained silica-alumina gel, and its filtrate ammonia-nitrogen content is 25 μ g/g.
Embodiment 2
Such as embodiment 1 preparation calcined kaolin microspheres.3 parts of 950 ℃ of calcined kaolin microspheres and 1 part of 820 ℃ of calcined kaolin microspheres and waterglass, alkali, directed agents and embodiment 1 resulting silica-alumina gel mixed be warming up to the synthetic NaY type molecular sieve of 90 ℃ of in-situ crystallizations, degree of crystallinity 44%; Containing NaY type molecular sieve solid-liquid mixed liquor filters and washing through the belt filter, collect crystallization mother liquor and crystallization material washing water, filter cake is through ammonium and rare earth-iron-boron repeatedly exchanges and sodium is taken off in roasting, and last expansion drying obtains the catalytic cracking catalyst finished product, sodium oxide content 0.27%.Collect exchange filtrate mixed liquor, ammonia-nitrogen content is 6362 μ g/g, crystallization material washing water and partially-crystallized mother liquor are added exchange filtrate mixed liquor, the pH value that makes its mixed liquor is 12.5, then with the spray washing liquid of this mixed liquor as the spray scrubber of mist projection granulating tower tail gas, the temperature that spray reclaims liquid is 92 ℃, and ammonia-nitrogen content is 204 μ g/g; Sulfuric acid solution is added drip washing again and reclaim liquid, making its pH value is 9.0, and aging 1 hour, press filtration obtained gel, and its filtrate ammonia-nitrogen content is 21 μ g/g.
Embodiment 3
Process flow diagram such as Fig. 2 of certain company gel method binding type catalytic cracking catalyst factory.By this flow process, be warming up to the synthetic NaY type molecular sieve of 95 ℃ of crystallization, degree of crystallinity 90% after waterglass, sodium metaaluminate, aluminum sulfate, directed agents be mixed into glue; NaY type molecular sieve solid-liquid mixed liquor filters and washing through the belt filter, collects crystallization mother liquor and crystallization material washing water, and filter cake takes off sodium through ammonium and twice exchange of rare earth-iron-boron and middle roasting, obtains modified Y molecular sieve, sodium oxide content 1.2%; Modified Y molecular sieve and kaolin, boehmite, aluminium colloidal sol are mixed into glue, solid content 38%, obtain the catalytic cracking catalyst microballoon finally by mist projection granulating tower mist projection granulating, again this microballoon is carried out the ammonium exchange at belt filter, filter cake sodium oxide content 0.20%, filter cake obtain the catalytic cracking catalyst finished product behind expansion drying.Collect exchange filtrate mixed liquor, ammonia-nitrogen content is 5962 μ g/g, crystallization material washing water and partially-crystallized mother liquor are added exchange filtrate mixed liquor, the pH value that makes its mixed liquor is 12.5, then with the spray washing liquid of this mixed liquor as the spray scrubber of mist projection granulating tower tail gas, the temperature that spray reclaims liquid is 92 ℃, and ammonia-nitrogen content is 185 μ g/g; Again Sulfated aluminum sulfate solution is added drip washing and reclaim liquid, making its pH value is 9.5, aging 1 hour, and filter and obtain silica-alumina gel, its filtrate ammonia-nitrogen content is 15 μ g/g.
Embodiment 4
Technological process such as embodiment 3 that gel method binding type catalytic cracking catalyst is produced.Waterglass, sodium metaaluminate, aluminum sulfate, directed agents and embodiment 3 resulting silica-alumina gels are mixed into are warming up to the synthetic NaY type molecular sieve of 98 ℃ of crystallization, degree of crystallinity 91% behind the glue; NaY type molecular sieve solid-liquid mixed liquor filters and washing through the belt filter, collects crystallization mother liquor and crystallization material washing water, and filter cake takes off sodium through ammonium and twice exchange of rare earth-iron-boron and middle roasting, obtains modified Y molecular sieve, sodium oxide content 1.3%; Modified Y molecular sieve and kaolin, boehmite, aluminium colloidal sol are mixed into glue, solid content 36%, obtain the catalytic cracking catalyst microballoon finally by mist projection granulating tower mist projection granulating, again this microballoon is carried out the ammonium exchange at belt filter, filter cake sodium oxide content 0.22%, filter cake obtain the catalytic cracking catalyst finished product behind expansion drying.Collect exchange filtrate mixed liquor, ammonia-nitrogen content is 5805 μ g/g, crystallization material washing water and partially-crystallized mother liquor are added exchange filtrate mixed liquor, the pH value that makes its mixed liquor is 11.5, then with the spray washing liquid of this mixed liquor as the spray scrubber of mist projection granulating tower tail gas, the temperature that spray reclaims liquid is 95 ℃, and ammonia-nitrogen content is 197 μ g/g; Again Sulfated aluminum sulfate solution is added drip washing and reclaim liquid, making its pH value is 9.0, aging 1 hour, and filter and obtain silica-alumina gel, its filtrate ammonia-nitrogen content is 14 μ g/g.
Claims (4)
1. the process for cleanly preparing of a synthetic zeolite catalysts cracking catalyst, this technique comprises:
(1) raw material of synthesis of molecular sieve being mixed into glue, crystallization, filtration, washing, ammonium and rare earth exchanged takes off sodium and obtains modified molecular screen or synthetic zeolite catalysts cracking catalyst;
(2) ammonia nitrogen waste water that Crystallization of Zeolite filtrated stock and/or crystallization material washing water and molecular sieve exchange process is produced mixes the spray washing liquid as the spray scrubber of catalyst mist projection granulating tower tail gas, stripping goes out the ammonia nitrogen in the spray washing liquid in the dust in removing mist projection granulating tower tail gas, the spray that obtains low ammonia-nitrogen content reclaims liquid, connect ammonia absorber behind the spray scrubber, the ammonia absorber absorption liquid is as ammonium in the step (1) and rare earth exchanged liquid or batching;
(3) acidifying aluminium salt or acid solution are added the resulting spray recovery of step (2) liquid, stir into glue, filtration, filtrate discharge, filter residue returns step (1) as the synthesis of molecular sieve raw material.
2. technique according to claim 1, it is characterized in that, the ammonia nitrogen waste water mixed proportion that the described Crystallization of Zeolite filtrated stock of step (2) and/or crystallization material washing water and molecular sieve exchange process produce is definite according to the pH value of mixed liquor, and the pH value is 9.5～13.0.
3. technique according to claim 1 is characterized in that, the acid of step (3) described acidifying aluminium salt or acid solution is selected from one or more in sulfuric acid, hydrochloric acid, the nitric acid; Aluminium salt is selected from one or more in aluminum sulfate, aluminium chloride, the aluminum nitrate.
4. technique according to claim 1 is characterized in that, the addition of step (3) described acidifying aluminium salt or acid solution is definite according to pH value after becoming glue, and the pH value is 7.0～11.0.
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| CN113753910A (en) * | 2020-06-03 | 2021-12-07 | 中国石油化工股份有限公司 | Method for treating crystallization mother liquor of mordenite molecular sieve |
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| US20070082809A1 (en) * | 2005-10-07 | 2007-04-12 | Sk Corporation | Hydrothermally stable microporous molecular sieve catalyst and preparation method thereof |
| CN101007261A (en) * | 2006-12-17 | 2007-08-01 | 于向真 | Zeolite adsorbent and its preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20070082809A1 (en) * | 2005-10-07 | 2007-04-12 | Sk Corporation | Hydrothermally stable microporous molecular sieve catalyst and preparation method thereof |
| CN101007261A (en) * | 2006-12-17 | 2007-08-01 | 于向真 | Zeolite adsorbent and its preparation method |
Non-Patent Citations (1)
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| 王欢等: "原位晶化NaY分子筛制备过程中含硅废水的处理工艺研究", 《石化技术与应用》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113753910A (en) * | 2020-06-03 | 2021-12-07 | 中国石油化工股份有限公司 | Method for treating crystallization mother liquor of mordenite molecular sieve |
| CN113753910B (en) * | 2020-06-03 | 2023-03-28 | 中国石油化工股份有限公司 | Method for treating crystallization mother liquor of mordenite molecular sieve |
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Application publication date: 20130410 |