WO2021136413A1 - 一种催化裂化油浆高温连续无灰化处理方法及系统 - Google Patents

一种催化裂化油浆高温连续无灰化处理方法及系统 Download PDF

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WO2021136413A1
WO2021136413A1 PCT/CN2020/141554 CN2020141554W WO2021136413A1 WO 2021136413 A1 WO2021136413 A1 WO 2021136413A1 CN 2020141554 W CN2020141554 W CN 2020141554W WO 2021136413 A1 WO2021136413 A1 WO 2021136413A1
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oil
slurry
settler
oil slurry
catalytic cracking
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PCT/CN2020/141554
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English (en)
French (fr)
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段征宇
段华山
胡幼元
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深圳市科拉达精细化工有限公司
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Publication of WO2021136413A1 publication Critical patent/WO2021136413A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/01—Separation of suspended solid particles from liquids by sedimentation using flocculating agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/24—Feed or discharge mechanisms for settling tanks
    • B01D21/2488—Feed or discharge mechanisms for settling tanks bringing about a partial recirculation of the liquid, e.g. for introducing chemical aids

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  • the invention relates to the field of petrochemical industry, in particular to a method and system for high-temperature continuous ashless treatment of catalytic cracking oil slurry.
  • Oil slurry is a by-product with very special properties produced in the process of heavy oil catalytic cracking. It is rich in aromatics, has a wide range of uses, and has good economic value. When high ash slurry is used as fuel oil and delayed coking feedstock, It will have a certain degree of negative impact on the quality and use of the product, but in terms of economy, it is generally acceptable. The application in the following fields has strict requirements on the ash content of the slurry.
  • Oil slurry is an important source of raw materials for carbon black production. According to statistics, more than 50% of the world's carbon black feedstock (CBO) is a catalytic cracking oil slurry.
  • the ash content (ASTM D-482) of CBO is required to be less than 500ppm, and the ash index of premium products is less than 300ppm.
  • Slurry is a high-quality raw material for oil-based needle coke.
  • Needle coke has a wide range of uses. It is used to prepare high-end carbon products such as high-power and ultra-high-power electrodes, graphite electrodes, special carbon materials, carbon fibers and their composite materials, and high-efficiency energy storage. The raw material of the capacitor.
  • the production of needle coke has very strict requirements on the ash content of the oil slurry, and the ash content must be below 50ppm. Practice has proved that the lower the ash content, the better the needle production and the better the quality.
  • Slurry can be used as a vacuum residue hydrocracking diluent.
  • white petroleum products such as steam, coal, diesel, etc.
  • it can also peptize the asphaltenes in the vacuum residue and effectively reduce the residue hydrogenation catalyst bed.
  • the pressure drop of the catalyst can prolong the service life of the catalyst.
  • the oil slurry is used as the diluting oil, the ash content should be reduced to below 50ppm.
  • the ash content of the slurry is also required to be below 200ppm.
  • the catalyst powder that accounts for 0.1-0.9% of the oil slurry and has a diameter of less than 100 ⁇ m must be removed.
  • the main contributor to the ash content of the oil slurry is the catalyst powder and its adsorbed heavy metals.
  • the methods for removing the ash content of the oil slurry are roughly as follows: natural sedimentation method, chemical aid sedimentation method, mechanical filtration method, electrostatic separation method and centrifugation Separation method, etc.
  • natural sedimentation method chemical aid sedimentation method
  • mechanical filtration method mechanical filtration method
  • electrostatic separation method electrostatic separation method
  • centrifugation Separation method etc.
  • the only real industrialization is the chemical aid sedimentation method and the mechanical filtration method.
  • the chemical aid sedimentation method has the advantages of low investment, simple operation, large processing volume flexibility, and high ash removal rate, such as Patent Publication Zhao 60-245696, USP4407707, USP4919792, USP4686048, CN01113133, CN1297981A, CN01205472A, CN200510116840, CN101670199B CN108611117A
  • the disclosed expressions have the following obvious shortcomings to varying degrees:
  • the temperature of the oil slurry is 80 ⁇ 100°C, and the highest is not more than 150°C.
  • the chemical sedimentation separation is carried out at the applicable temperature. If the clarified oil is further processed in the subsequent equipment such as residual oil hydrogenation and delayed coking, the temperature needs to be raised from a low temperature to 365°C.
  • This sedimentation separation process is one process. It is more complicated and investment is increased; second, the temperature rises and falls tortuously, which is not conducive to energy saving.
  • a special settling tank is required, and the settling operation is interrupted.
  • the settling tank needs to be cleaned regularly and frequently. Because the volume of the settling tank is mostly small, it is inconvenient to clean the tank mechanically. Manual cleaning is generally used. In addition to increasing labor intensity, there are also certain problems. Safety and health risks.
  • the sediment cleaned out of the settling tank is a solid hazardous waste, and it needs to be paid to a qualified professional organization for harmless treatment.
  • the chemical agent method will produce an average of 1% sediment.
  • the company has to pay an additional 60 yuan/ton. Yuan/ton of solid hazardous waste treatment costs.
  • the catalyst particles in the oil slurry contain an average of at least 50% combustibles, mainly coke and asphaltenes. These combustibles are sent to the factory for processing after sedimentation and separation, which is a waste of oil refineries. Taking a catalytic device with an annual by-product of 200,000 oil slurry as an example, the use of chemical aid sedimentation method will waste about 1,000 tons of combustible matter every year.
  • the mechanical filtration method is described in CN201810504927.7 and CN201710402670.X. Although the filtration operation can be carried out at high temperature, it has the advantages of higher precision and higher removal rate, but its shortcomings are also quite prominent. According to incomplete statistics, more than 40 sets of oil slurry mechanical filtration equipment have been introduced in China. At present, the Qilu Petrochemical Refinery provides a set of filtering devices for the residue hydrocracking unit to purify the catalytic refining (lighter than oil slurry), and the Jinzhou Petrochemical provides a set of filtering devices for the needle coke production unit to provide clarified oil. In addition to operation, all other filter devices are out of service due to various reasons, and some have been dismantled due to a long period of outage. In summary, the mechanical filtration method of oil slurry mainly has the following defects:
  • a filter device with an annual oil slurry processing capacity of about 150,000 tons requires at least 30 million yuan in one-time fixed assets.
  • Short service life of the filter There are two main reasons for the short service life of the filter: one is that frequent washing and backwashing will cause great damage to the filter element, which will easily cause the filter element to perforate and lose the filtering function; the second is the oil slurry Polar substances such as colloids and asphaltenes are adsorbed on the filter element, and even coke and block the filter pores. Even with washing and backwashing, it is difficult to remove these polar dirt and coke. It accumulates over time and seriously affects the filter area of the filter element. When the filter element is perforated or the filter area is satisfied, the filter element must be updated, and the filter element is often updated every 6 months.
  • the present invention discloses a high-temperature ash-free treatment method for catalytic cracking oil slurry, which is used for ash-free treatment of catalyst particles in the catalytic cracking oil slurry at high temperature, and includes the following steps:
  • S2 slurry continuous dynamic Purification Coagulation from the lower outer Slurry Oil Press amount Q of 100 to 400% outside the coagulation slurry withdrawn and injected into the lower portion of the settler, the settler has sequentially from bottom to top enriching section, a settling section and arranged refining stage, when the temperature T sink settler was 100 °C ⁇ 360 °C, Shen operating pressure P is 0.3 to 0.5MPa, coagulation slurry in the pre-settling enrichment section The pre-sedimentation residence time is 10-60 minutes, and the coagulation oil slurry is separated into two parts in the enrichment section: one is the enriched liquid with more catalyst particles, and the other is the pre-clarification with lower catalyst particles.
  • the oil and the enriched liquid remain in the enrichment section, and the pre-clarified oil overflows the enrichment section and enters the sedimentation section to continue dynamic sedimentation.
  • the dynamic sedimentation time is 30 to 480 minutes, and the pre-clarified oil is separated by sedimentation.
  • the clarified oil overflows from the top of the sedimentation section and enters the clarification section. Section, wherein the rising line of the pre-clarified oil level in the settling section is not greater than the apparent settling velocity of the catalyst particles;
  • S3 clear oil collection and transport the step S2, the input to the clear oil sump, tank temperature T of the current collector is cleared to 100 °C ⁇ 360 °C, operating at a pressure P of 0.3 ⁇ 0.5MPa clear condition, After the residence time of the clarified oil in the sump is 10-60 minutes, the clarified oil in the sump is pumped out and sent to the next process;
  • Reuse of the enriched liquid extract the enriched liquid from the outlet provided at the bottom of the settler according to 0-300% of the amount of oil slurry Q outside , and a part of it shall be 0-300% of the total amount of the enriched liquid.
  • the coagulator re-enters steps S2 and S3 to perform an ash-free process, which is used to increase the concentration of the dispersed phase in the oil slurry, so as to achieve faster and more complete flocculation and aggregation of the dispersed catalyst particles.
  • step S23 is included between the steps S2 and S3:
  • the oil slurry electrical neutralization liquid is 0.03-0.1%, preferably 0.06%, of the amount Q of the slurry thrown out of the catalytic cracking unit according to the weight ratio.
  • the fresh oil slurry delivered by the catalytic cracking unit and the settler The enriched liquid of the recycled catalyst is added to the coagulator, and the coagulation time is 1-60 minutes, preferably 30 minutes, at 100-360°C, preferably 300°C, to obtain coagulation Oil slurry.
  • the coagulation oil slurry is drawn at 100-400%, preferably 150%, of the amount Q of the externally thrown oil slurry, and is pumped out and injected into the settler for ash-free purification and sedimentation, and the sedimentation temperature is 100°C to 360°C , Preferably 300°C; the residence time of the slurry in the slurry settler is 40-540 minutes, preferably 260 minutes.
  • the catalyst-rich liquid produced at the bottom of the settler is pumped out at 0-100% and returned to the coagulator to enter the ash-free treatment again.
  • the catalyst-rich liquid at the bottom of the settler is respectively 0% , Or 50%, or 90% of the proportion is returned to the coagulator for reuse, and the operating temperature is maintained at 300°C.
  • the invention discloses a high-temperature ash-free treatment system for catalytic cracking oil slurry, which is used to implement any one of the above-mentioned high-temperature ash-free treatment methods for catalytic cracking oil slurry.
  • the treatment system includes: a coagulator, a metering pump, a reflux pump, and a sedimentation system.
  • the lower part of the coagulator is connected to one end of the metering pump, the other end of the metering pump is connected to the feed port of the settler, and the discharge port of the settler is connected to the intermediate tank
  • the upper part is connected, the bottom outlet of the settler is connected to one end of the reflux pump, and the other end of the reflux pump is connected to the mixing input port of the coagulator through an oil pipe.
  • a homogenizer is provided in the coagulator, and the homogenizer is used for the electric neutralization liquid of the oil slurry, the external sludge of catalytic cracking, and the reuse of the enriched slurry added to the coagulator.
  • the collected liquid is uniformly coagulated to obtain a coagulated oil slurry.
  • the settler has an enrichment section, a sedimentation section, and a clarification section sequentially arranged from bottom to top.
  • the enrichment section is provided with a sparger, and a grid is provided above the sparger, and the clarification section
  • a liquid collection tank is arranged inside, and the settler is also provided with a sampling port.
  • a first thermostat for controlling temperature and a first pressure gauge for measuring pressure are provided in the coagulator.
  • the settler is provided with a second temperature controller for controlling temperature and a second pressure gauge for measuring pressure.
  • the clarified oil can meet all the requirements for use, such as the raw materials for the production of carbon black and needle coke with strict ash requirements, and the residual oil hydrogenation dilution oil;
  • This technical solution can be operated at the operating temperature of the catalysis and subsequent treatment devices, avoiding the tortuous rise and fall of temperature, and is beneficial to energy saving;
  • This technical solution adopts the process of returning the enriched liquid of catalyst particles to the riser of the catalytic device for re-refining.
  • the catalyst particles are separated by the cyclone in the catalytic reactor and recycled into the regenerated catalyst system through catalyst regeneration. These regenerated catalysts It can be recycled and reused by the catalyst production plant, avoiding the defects of solid hazardous waste generated by the chemical aid sedimentation method and mechanical filtration method.
  • the reuse of the catalyst particle-enriched liquid is not the recovery of hazardous waste, but avoids the generation of hazardous waste, is beneficial to environmental protection, and saves hazardous waste treatment costs.
  • Fig. 1 is a functional diagram of a high-temperature ash-free treatment method of a catalytic cracking oil slurry according to an embodiment of the present invention
  • FIG. 2 is a schematic diagram of a high-temperature ash-free treatment system for catalytic cracking oil slurry according to an embodiment of the present invention
  • FIG. 3 is a schematic diagram of the structure of a settler in a high-temperature ash-free treatment system of a catalytic cracking oil slurry according to an embodiment of the present invention.
  • a high-temperature ash-free treatment method for catalytic cracking oil slurry used for ash-free treatment of catalyst particles in the catalytic cracking oil slurry under high temperature conditions, including the following step:
  • Step 1 The slurry electrical neutralization liquid is 0.03-0.1 % (mass ratio) of the amount of slurry Q outside the catalytic cracking unit, preferably 0.06% (mass ratio), and the oil from the catalytic cracking unit
  • the slurry and the recycled catalyst-enriched liquid are added to the coagulator 1, and the coagulation time is 1-60 minutes at 100-360°C, preferably at 300°C, preferably 30 minutes, and the coagulation time is 30 minutes.
  • the operating pressure P is mixed at 0.3-0.5 MPa to prepare a coagulated oil slurry.
  • Step 2 The coagulation slurry prepared in step 1 is pumped out at 100% to 400% of the external slurry volume Q, preferably 150%, and injected into the slurry settler 4 from the lower part of the settler 4 for ashlessness Purification and sedimentation, the sedimentation temperature is 300°C; the residence time of the oil slurry in the slurry settler 4 is 40-540 minutes, the preferred pre-sedimentation time is 20 minutes, and the sedimentation time is 240 minutes; the operating pressure P sedimentation is 0.3-0.5 MPa;
  • Step 3 The oil slurry purified in step 2 overflows from the top 47a of the oil slurry settler 4 to the intermediate tank 5, and the purified oil slurry in the settler 4 is emptied from the sampling port 47c;
  • Step 4 After the clarified oil slurry of step 2 is emptied from sampling port 47c, the catalyst-rich liquid produced at the bottom is pumped out at 0-100% and returned to the coagulator 1 to re-enter the ash-free treatment procedure.
  • the slurry settler 4 The catalyst rich liquid in the lower part is returned to the coagulator 1 at a ratio of 0%, 50%, or 90% for reuse for a comparative test; the operating temperature is maintained at 300°C.
  • the oil slurry after step two is divided into two parts, the upper part is about 85% as ash-free oil slurry, and the lower part is about 15% as the catalyst enriched liquid.
  • a catalytic cracking oil slurry high temperature ashless treatment system the treatment system includes: coagulator 1, metering pump 2, reflux pump 3, settler 4, intermediate tank 5 and a number of oil pipelines 6, the lower part of the coagulator 1 is connected to one end of the metering pump 2, the other end of the metering pump 2 is connected to the feed port 48 of the settler 4, and the discharge port 49 of the settler 4 is connected to the upper part of the intermediate tank 5.
  • the bottom outlet 46 of the vessel 4 is connected to one end of the reflux pump 3, and the other end of the reflux pump 3 is connected to the mixing input port of the coagulator 1 through an oil pipe 6.
  • a homogenizer 7 is provided in the coagulator 1, and the homogenizer 7 is used to uniformly mix the slurry electrical neutralization liquid, the FCC externally thrown oil slurry, and the recycled enriched liquid added to the coagulator 1. Coagulated to obtain a coagulated oil slurry,
  • the settler 4 has an enrichment section 41, a sedimentation section 42, and a clarification section 43 arranged from bottom to top.
  • the enrichment section 41 is provided with a sparger 44, and a grid 45 is provided above the sparger 44, and the clarification section 43 is provided with There is a sump, the settler 4 is also provided with a sampling port 47, and there are multiple sampling ports 47, including a first sampling port 47a, a second sampling port 47b, a third sampling port 47c, and a fourth sampling port 47d;
  • the distributor is Umbrella-shaped distributors can also be distributors in the shape of ribs and branches.
  • the coagulator 1 is provided with a first thermostat 8 for controlling temperature and a first pressure gauge for measuring pressure.
  • the settler 4 is provided with a first thermostat 9 for controlling temperature and a second pressure gauge for measuring pressure.
  • the clarified oil is taken from the sampling port 47a shown in FIG. 3, and the enriched liquid is taken from the sampling port 47d, and the ash content is analyzed separately.
  • the high-temperature ash-free treatment method of the catalytic cracking oil slurry provided by this technical solution has a fast purification time and a significant purification effect.
  • the ash content of the purified oil slurry can be reduced to a minimum of about 30 ppm.
  • the high-temperature continuous ash-free treatment method and system of the catalytic cracking oil slurry in the present invention can reduce the ash content of the catalytic cracking oil slurry, refining oil or their mixture to less than 0.005% after the ash-free treatment process.
  • the technology is novel. Rapid and continuous purification at high temperature, good purification effect, continuous dynamic sedimentation and separation, environmentally friendly reuse of catalysts, energy saving and consumption reduction, and safe and reliable industrial operation.

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Abstract

一种催化裂化油浆高温连续无灰化处理方法及系统，利用化学助剂电性中和液、油浆及催化剂富集液混合后经过混凝器(1)制备混凝油浆，将混凝油浆输入到沉降器(4)进行连续动态无灰化处理，分离出的澄清油高温收集，回收的催化剂富集液再利用并重新进行动态无灰化处理，可使催化裂化油浆经过无灰化处理后，灰分降低到0.005％以下，其技术方案合理，高温状态快速连续净化，净化效果好，可实现连续化动态沉降分离，催化剂环保再利用，节能降耗，工业化操作安全可靠。

Description

一种催化裂化油浆高温连续无灰化处理方法及系统 技术领域
本发明涉及石油化工领域，尤其涉及一种催化裂化油浆高温连续无灰化处理方法及系统。
背景技术
油浆是重油催化裂化工艺过程中所产生的一种性质极为特殊的副产品，富含量芳烃，用途广泛，具有良好的经济利用价值，高灰分的油浆作燃料油和延迟焦化原料时，虽然会对产品质量和使用造成一定程度的负面影响，但从经济性来讲，总体上是可接受的，在下列几个领域的应用，则对油浆的灰分有较严格的要求。
油浆是碳黑生产的一个重要原料来源。据统计，世界50％以上的碳黑原料油(CBO)是催化裂化油浆，CBO的灰分(ASTM D-482)要求为500ppm以下，优级品的灰分指标则为300ppm以下。
油浆是油系针状焦的优质原料，针状焦用途广泛，是制备高功率和超高功率电极石墨电极、特种碳素材料、炭纤维及其复合材料等高端碳素制品、高效储能电容的原料。但生产针状焦对油浆的灰分要求非常严格，灰分要求必须在50ppm以下，实践证明，灰分越低越有利于针状的生产，质量也越好。
油浆可以作为减压渣油加氢裂化稀释油，除能增产汽、煤、柴等白色石油产品外，还能胶溶减压渣油中的沥青质，有效降低渣油加氢催化剂床层的压力降，延长催化剂的使用寿命，油浆作稀释油时灰分要求降到50ppm以下。
油浆经过溶剂抽提后重质芳烃是橡塑加工的理想填充料，为保证抽提装置和溶剂回收系统的正常操作，以及填充料的性能，也要求油浆的灰分在200ppm以下。
因此，要综合利用油浆，提升油浆的经济价值，必须对油浆中占0.1-0.9％、直径在100μm以下的催化剂粉末予以脱除。
油浆的灰分的主要贡献者是催化剂粉末及其所吸附的重金属，脱除油浆灰分的方法大致有以下几种：自然沉降法、化学助剂沉降法、机械过滤法、静电分离法和离心分离法等。上述方法中真正实现工业化只有化学助剂沉降法、机械过滤法。
化学助剂沉降法具有投资少、操作简单、处理量弹性大、灰分脱除率较高等优点，如专利特开昭60-245696、USP4407707、USP4919792、USP4686048、CN01113133、CN1297981A、CN01205472A、CN200510116840、CN101670199B CN108611117A所公开的表述，但不同程度存在以下明显的缺点：
1、大多要求在较低温度条件下进行使用，即油浆温度在80～100℃，最高不超过150℃，这样就需要油浆从365℃(油浆从催化分馏塔底的抽出温度)冷却到适用温度再进行化学沉降分离，如果澄清油到后续的如渣油加氢、延迟焦化等装置进行深加工，则又需要将温度从低温度升至365℃，这样的沉降分离流程，一是工序较为复杂，增加投资；二是温度经过升降曲折，不利于节能。
2、由于是在低温条件下进行的沉降分离，从沉降原理上分析，低温条件下，油浆的粘度大、催化剂与油浆的密度差小，这些都不利于沉降，沉降条件是比较严苛的。因此，尽管现行的化学助剂沉降法的脱除率比较高，但难以使油浆的灰分达到作碳黑和针状焦原料、以及渣油加氢稀释油的要求。
3、需要专用的沉降罐，沉降间断操作，沉降罐需要定期清理沉渣，并且比较频繁，由于沉降罐容量大多比较小，不便机械清罐，普遍采用人工清理，除增加劳动强度外，也存在一定的安全卫生风险。
4、沉降分离基本上是采用静置沉降，无法做到动态沉降，因此连续化操作难以实现。
5、按照现行的危废管理规定，沉降罐中清理出来的沉渣属于固体危废，需要付费给有资质的专业机构进行无害化处理。根据油浆的平均催化剂含量和目前的化学助剂沉降的技术水平，采用化学助剂法会平均产生1％的沉渣，按目前固体危废处理的市场价格6000元/吨，企业要额外支付60元/吨的固体危废处理费用。
6、油浆中的催化剂颗粒平均至少含有50％的可燃质，主要是焦炭和沥青质等，这部分可燃质经过沉降分离后被送出厂进行处理，对炼油企业来说是个浪 费。以年副产20万油浆的催化装置为例，采用化学助剂沉降法每年将浪费1000吨左右的可燃质。
机械过滤法如CN201810504927.7、CN201710402670.X所述，虽可以高温下进行过滤操作，具有精度较高、脱除率较高等优点，但其缺点也相当突出。据不完全统计，国内先后引进了40多套油浆机械过滤设备。目前，除齐鲁石化炼油厂为渣油加氢裂化装置提供净化催化回炼油(比油浆轻)的一套过滤装置，和锦州石化为针状焦生产装置提供澄清油的一套过滤装置在正常运行外，其他所有过滤装置都因各种各样的原因处于停运状态，有些因停运时间较久，已被拆除。油浆的机械过滤法归纳起来主要有以下几方面的缺陷：
1、投资大：一套年油浆处理量15万吨左右的过滤装置，一次性固定资产至少需要3000万元人民币左右。
2、处理量弹性小：过滤装置选型建成后，油浆的处理量基本没什么操作弹性，尤其是装置运行一段时间，滤孔出现堵塞现象后，处理量更是受到严重影响。
3、运行周期短：油浆中胶质、沥青质等极性物质含量较高，加之催化剂颗粒细小，不易形成桥架，所以滤芯很容易被颗粒和极性物质吸附堵塞，为了保证生产，至少要建设2台相同的过滤器，互为备用，以便在它们之间频繁地进行切换、冲洗和反冲等恢复过滤性能的操作。
4、过滤器使用寿命短：造成过滤器使用寿命短的原因主要有两个：一是频繁地冲洗与反冲洗对滤芯的伤害很大，容易造成滤芯穿孔，丧失过滤的功能；二是油浆中胶质、沥青质等极性物质吸附在滤芯上，甚至结焦而堵塞滤孔，即使进行冲洗与反冲洗也很难将这些极性污垢和焦碳清除，日积月累，严重影响滤芯的过滤面积，当滤芯穿孔，或者过滤面积满足时就必须更新滤芯，滤芯往往每6个月就要进行更新。
5、由于滤饼或冲洗液不返回催化装置进行回炼，所以与化学助剂沉降法一样也会产生1％左右的含油催化剂固体危废。
6、安全风险大：有些过滤装置采用轻烃和干气进行冲洗和吹扫，存在较大的安全风险。
7、运行和维保费用高：过滤器进行频繁的切换、冲洗和反冲等操作；以及不定期的更换，造成运行和维修费用较高。
发明内容
为了解决现有技术不足，本发明公开了一种催化裂化油浆高温无灰化处理方法，用于高温状态下对所述催化裂化油浆中的催化剂颗粒无灰化处理，包括如下步骤：
S1.混凝油浆的制备：在温度T 混为100℃～360℃条件下，将油浆电性中和液、催化裂化外甩油浆、沉降器下部回用富集液按重量比且混凝时间t 混为1～60分钟连续在混凝器中均匀混凝制得混凝油浆，其中，所述油浆电性中和液占催化裂化外甩油浆量Q 外的0.003～0.1％，所述回用富集液量Q 回为外甩油浆量Q 外的0～300％，所述催化裂化外甩油浆量Q 外单位为吨/小时，所述混凝器操作压力P 混为0.3～0.5MPa；
S2.油浆连续动态净化：从混凝器下部按外甩油浆量Q 外的100～400％抽出所述混凝油浆并注入到沉降器下部，所述沉降器具有依次从下到上设置的富集段、沉降段及澄清段，当沉降器中温度T 沉为100℃～360℃，操作压力P 沉为0.3～0.5MPa时，混凝油浆在所述富集段进行预沉降，预沉降停留时间为10～60分钟，混凝油浆在所述富集段被分离成两部分：一部分为含催化剂颗粒较多的富集液，另一部分为含催化剂颗粒较低的预澄清油，富集液留存于所述富集段，预澄清油溢出所述富集段进入所述沉降段继续进行动态沉降，其动态沉降时间为30～480分钟，所述预澄清油被沉降分离成富集液和澄清油，富集液下沉重回所述富集段，澄清油从所述沉降段顶部溢出进入所述澄清段，为防止预澄清油中的催化剂颗粒被携带进入到澄清油段，其中，所述沉降段中预澄清油液面的上升线不大于催化剂颗粒的表观沉降速度；
S3.澄清油收集与输送：将步骤S2中所述澄清油输入到集液槽，所述集液槽的温度T 清为100℃～360℃，操作压力P 清为0.3～0.5MPa条件下，所述澄清油在集液槽的停留时间为10～60分钟后，将所述集液槽中澄清油抽出送往下道工序；
S4.富集液再利用：将所述富集液按外甩油浆量Q 外的0～300％从设于所述沉降器底部的排出口抽出，一部分按富集液总量的0～100％作为回炼油返回催化装 置提升管重新回炼，用于提高催化裂化装置的轻油收率；另一部分按富集液总量的0～100％作循环油与新鲜油浆一起进入所述混凝器重新进入步骤S2及步骤S3进行无灰化过程，用于提高油浆中分散相的浓度，以达到分散的催化剂颗粒更快更完全的絮凝与聚集的目的。
进一步地，所述步骤S2和S3之间包括步骤S23：
S23.净化后的澄清油从沉降器顶部溢出并输送至中间罐。
进一步地，所述油浆电性中和液按重量比为催化裂化装置外甩油浆量Q 外的0.03～0.1％，优选为0.06％，催化裂化装置输送的新鲜油浆和所述沉降器的回用催化剂的富集液加入所述混凝器中，在100～360℃的条件下，优选为300℃条件下，混凝时间为1～60分钟，优选为30分钟，制得混凝油浆。
进一步地，所述混凝油浆按外甩油浆量Q 外的100～400％，优选为150％，抽出并从注入沉降器中进行无灰化净化沉降，沉降温度为100℃～360℃，优选为300℃；油浆在油浆沉降器中的停留时间为40～540分钟，优选为260分钟。
进一步地，所述沉降器底部产生的催化剂富集液按0～100％抽出返回所述混凝器重新进入无灰化处理，优选的，所述沉降器下部的催化剂富集液分别按0％、或50％、或90％比例返回所述混凝器重新进行再利用，操作温度保持在300℃。
本发明公开了一种催化裂化油浆高温无灰化处理系统，用于实施上述任一项催化裂化油浆高温无灰化处理方法，处理系统包括：混凝器、计量泵、回流泵、沉降器、中间罐及若干输油管，所述混凝器的下部与计量泵一端连接，所述计量泵另一端与所述沉降器的进料口，所述沉降器的出料口与所述中间罐上部连接，所述沉降器的底部排出口连接所述回流泵一端，所述回流泵另一端通过输油管连接到所述混凝器的混料输入口。
进一步地，所述混凝器中设有均质机，所述均质机用于对加入到所述混凝器中的油浆电性中和液、催化裂化外甩油浆、回用富集液进行均匀混凝制得混凝油浆。
进一步地，所述沉降器具有依次从下到上设置的富集段、沉降段及澄清段，所述富集段内设有分布器，所述分布器上方设有格栅，所述澄清段内设有集液槽，所述沉降器还设有取样口。
进一步地，所述混凝器中设有用于控制温度的第一温控器及用于测量压力的第一压力表。
进一步地，所述沉降器中设有用于控制温度的第二温控器和用于测量压力的第二压力表。
实施本发明提出的一种催化裂化油浆高温连续无灰化处理方法及系统，具有以下有益的技术效果：
1.本技术方案虽属化学助剂沉降法，与现有技术不同的是本技术方案是连续处理工艺，采用的是在沉降器中进行动态沉降；
2.本技术方案操作简便、处理时间短、处理量大，因此生产成本低；
3.本技术方案灰分脱除率高，经过处理后，澄清油可以满足所有的使用要求，例如对灰分要求较严格的碳黑和针状焦的生产原料以及渣油加氢稀释油；
4.本技术方案没有特别需要维护、检修及频繁更换的设备，因此，运行周期长，既能保证正常生产，又能节省维修费用；
5.本技术方案可在催化和后续处理装置的操作温度下操作运行，避免了升降温的曲折，有利节能；
6.本技术方案由于采用了催化剂颗粒富集液返回催化装置提升管重新进行回炼的工艺，催化剂颗粒在催化反应器中被旋风分离下来，通过催化剂再生回收进入了再生催化剂系统，这些再生催化剂可以由催化剂生产厂进行回收利用，避免了化学助剂沉降法、机械过滤法会产生固体危废的缺陷。催化剂颗粒富集液的再利用并不是危废的回收，而是避免了危废的产生，有利环保，节省了危废处理费用。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1为本发明的实施例一种催化裂化油浆高温无灰化处理方法的功能图；
图2为本发明的实施例一种催化裂化油浆高温无灰化处理系统示意图；
图3为本发明的实施例一种催化裂化油浆高温无灰化处理系统中沉降器结构示意图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
请参阅图1至图3，本发明的实施例，一种催化裂化油浆高温无灰化处理方法，用于高温状态下对所述催化裂化油浆中的催化剂颗粒无灰化处理，包括如下步骤：
步骤一：将油浆电性中和液按催化裂化装置外甩油浆量Q 外的0.03～0.1％(质量比)，优选的，按0.06％(质量比)，与催化裂化装置来的油浆以及回用催化剂富集液一起加入混凝器1中，在100～360℃的条件下，优选300℃条件下，混凝时间1～60分钟，优选混凝时间为30分钟，混凝器操作压力P 混为0.3～0.5MPa，制得混凝油浆。
步骤二：将步骤1制得的混凝油浆按外甩油浆量Q 外的100～400％，优选按150％抽出并从沉降器4的下部注入油浆沉降器4中进行无灰化净化沉降，沉降温度为300℃；油浆在油浆沉降器4中的停留时间为40～540分钟，优选的预沉降时间为20分钟，沉降时间为240分钟；操作压力P 沉为0.3～0.5MPa；
步骤三：将步骤二净化后的油浆从油浆沉降器4的顶部47a溢出至中间罐5，沉降器4内净化后的油浆从取样口47c清空；
步骤四：将步骤二澄清油浆从取样口47c清空后，底部产生的催化剂富集液按0-100％抽出返回混凝器1重新进入无灰化处理程序，优选的，油浆沉降器4下部的催化剂富液分别按0％、或50％、或90％比例返回混凝器1重新进行再利用，做对比试验；操作温度保持在300℃。
经过步骤二后的油浆被分成两部分，上部约85％为无灰油浆，下部约15％为催化剂富集液。
请参阅图2及图3，本发明的实施例，一种催化裂化油浆高温无灰化处理系统，处理系统包括：混凝器1、计量泵2、回流泵3、沉降器4、中间罐5及若干输油管6，混凝器1的下部与计量泵2一端连接，计量泵2另一端与沉降器4的进料口48，沉降器4的出料口49与中间罐5上部连接，沉降器4的底部排出口46连接回流泵3一端，回流泵3另一端通过输油管6连接到混凝器1的混料输入口。
混凝器1中设有均质机7，均质机7用于对加入到混凝器1中的油浆电性中和液、催化裂化外甩油浆、回用富集液进行均匀混凝制得混凝油浆，
沉降器4具有依次从下到上设置的富集段41、沉降段42及澄清段43，富集段41内设有分布器44，分布器44上方设有格栅45，澄清段43内设有集液槽，沉降器4还设有取样口47，取样口47有多个，包括第一取样口47a、第二取样口47b、第三取样口47c及第四取样口47d；分布器为伞形状分布器，也可以是骨排形状、树枝形状等分布器。
混凝器1中设有用于控制温度的第一温控器8及用于测量压力的第一压力表。
沉降器4中设有用于控制温度的第一温控器9和用于测量压力的第二压力表。
进一步说明：
图3所示的取样口47a处取澄清油，取样口47d处取富集液，分别分析灰分。
无灰化处理工艺试验的结果见下表
Figure PCTCN2020141554-appb-000001
Figure PCTCN2020141554-appb-000002
从上表可以看出，本技术方案提供的催化裂化油浆高温无灰化处理方法，净化时间快，净化效果相当显著，净化后的油浆灰分最低可降至30ppm左右。
实施本发明提出的一种催化裂化油浆高温连续无灰化处理方法及系统，具有以下有益的技术效果：
本发明中的催化裂化油浆高温连续无灰化处理方法及系统，可使催化裂化油浆，回炼油或它们的混合物经过无灰化处理工艺后，灰分降低到0.005％以下，其技术新颖，高温状态快速连续净化，净化效果好，可实现连续化动态沉降分离，催化剂环保再利用，节能降耗，工业化操作安全可靠。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种催化裂化油浆高温连续无灰化处理方法，用于高温状态下对所述催化裂化油浆中的催化剂颗粒无灰化处理，其特征在于，包括如下步骤：
    S1.混凝油浆的制备：在温度T 混为100℃～360℃条件下，将油浆电性中和液、催化裂化外甩油浆、沉降器下部回用富集液按重量比且混凝时间t 混为1～60分钟连续在混凝器中均匀混凝制得混凝油浆，其中，所述油浆电性中和液占催化裂化外甩油浆量Q 外的0.003～0.1％，所述回用富集液量Q 回为外甩油浆量Q 外的0～300％，所述催化裂化外甩油浆量Q 外单位为吨/小时，所述混凝器操作压力P 混为0.3～0.5MPa；
    S2.油浆连续动态净化：从混凝器下部按外甩油浆量Q 外的100～400％通过油浆泵抽出所述混凝油浆并注入到沉降器下部，所述沉降器具有依次从下到上设置的富集段、沉降段及澄清段，当沉降器中温度T 沉为100℃～360℃，操作压力P 沉为0.3～0.5MPa时，混凝油浆在所述富集段进行预沉降，预沉降停留时间为10～60分钟，混凝油浆在所述富集段被分离成两部分：一部分为含催化剂颗粒较多的富集液，另一部分为含催化剂颗粒较低的预澄清油，富集液留存于所述富集段，预澄清油溢出所述富集段进入所述沉降段继续进行动态沉降，其动态沉降时间为30～480分钟，所述预澄清油被沉降分离成富集液和澄清油，富集液下沉重回所述富集段，澄清油从所述沉降段顶部溢出进入所述澄清段，为防止预澄清油中的催化剂颗粒被携带进入到澄清油段，其中，所述沉降段中预澄清油液面的上升线速不大于催化剂颗粒的表观沉降速度；
    S3.澄清油收集与输送：将步骤S2中所述澄清油输入到集液槽，所述集液槽的温度T 清为100℃～360℃，操作压力P 清为0.3～0.5MPa条件下，所述澄清油在集液槽的停留时间为10～60分钟后，将所述集液槽中澄清油抽出送往下道工序；
    S4.富集液再利用：将所述富集液按外甩油浆量Q 外的0～300％从设于所述沉降器底部的排出口抽出，一部分按富集液总量的0～100％作为回炼油返回催化装置提升管重新回炼，用于提高催化裂化装置的轻油收率；另一部分按富集液总量的0～100％作循环油与新鲜油浆一起进入所述混凝器重新进入步骤S2及步骤S3进行无灰化过程，用于提高油浆中分散相的浓度，以达到分散的催化剂颗粒更快更完全的絮凝与聚集的目的。
  2. 根据权利要求1所述的催化裂化油浆高温无灰化处理方法，其特征在于，所述步骤S2和S3之间包括步骤S23：
    S23.净化后的澄清油从沉降器顶部溢出并输送至中间罐。
  3. 根据权利要求1所述的催化裂化油浆高温连续无灰化处理方法，其特征在于，所述油浆电性中和液按重量比为催化裂化装置外甩油浆量Q 外的0.03～0.1％，优选为0.06％，催化裂化装置输送的新鲜油浆和所述沉降器的回用催化剂的富集液加入所述混凝器中，在100～360℃的条件下，优选为300℃条件下，混凝时间为1～60分钟，优选为30分钟，制得混凝油浆。
  4. 根据权利要求1所述的催化裂化油浆高温连续无灰化处理方法，其特征在于，所述混凝油浆按外甩油浆量Q 外的100～400％，优选为150％，抽出并从注入沉降器中进行无灰化净化沉降，沉降温度为100℃～360℃，优选为300℃；油浆在油浆沉降器中的停留时间为40～540分钟，优选为260分钟。
  5. 根据权利要求1所述的催化裂化油浆高温连续无灰化处理方法，其特征在于，所述沉降器底部产生的催化剂富集液按0～100％抽出返回所述混凝器重新进入无灰化处理，优选的，所述沉降器下部的催化剂富集液分别按0％、或50％、或90％比例返回所述混凝器重新进行再利用，操作温度保持在300℃。
  6. 一种催化裂化油浆高温连续无灰化处理系统，用于实施上述权利要求1～5中任一项所述的催化裂化油浆高温连续无灰化处理方法，其特征在于，所述处理系统包括：混凝器、计量泵、回流泵、沉降器、中间罐及若干输油管，所述混凝器的下部与计量泵一端连接，所述计量泵另一端与所述沉降器的进料口，所述沉降器的出料口与所述中间罐上部连接，所述沉降器的底部排出口连接所述回流泵一端，所述回流泵另一端通过输油管连接到所述混凝器的混料输入口。
  7. 根据权利要求6所述的催化裂化油浆高温连续无灰化处理系统，其特征在于，所述混凝器中设有均质机，所述均质机用于对加入到所述混凝器中的油浆电性中和液、催化裂化外甩油浆、回用富集液进行均匀混凝制得混凝油浆。
  8. 根据权利要求6所述的催化裂化油浆高温连续无灰化处理系统，其特征在于，所述沉降器具有依次从下到上设置的富集段、沉降段及澄清段，所述富集段内设有分布器，所述分布器上方设有格栅，所述澄清段内设有集液槽，所述沉降器还设有取样口。
  9. 根据权利要求6所述的催化裂化油浆高温连续无灰化处理系统，其特征在于，所述混凝器中设有用于控制温度的第一温控器及用于测量压力的第一压力表。
  10. 根据权利要求6所述的催化裂化油浆高温连续无灰化处理系统，其特征在于，所述沉降器中设有用于控制温度的第二温控器和用于测量压力的第二压力表。
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