阅读说明：本技术 一种加氢催化剂的分离工艺 (Separation process of hydrogenation catalyst ) 是由 过学军 罗利忠 汪太平 杨镭 刘北站 于 2020-07-28 设计创作，主要内容包括：本发明涉及一种加氢催化剂的分离工艺,基于一套分离系统,回收浓缩装置包括有金属烧结管过滤器、压滤釜、碱洗釜、酸洗釜、水洗釜、烘箱、焙烧炉、超声箱和旋风分离器,所述碱洗釜、酸洗釜、水洗釜的底部设置有循环泵,实现洗液洗涤循环；分离工艺包括有：1).过滤；2).洗涤；3).干燥；4).焙烧；5).分离；本发明的分离方法中通过过滤和洗涤对催化剂初步分离,在惰性气体中焙烧炭化处理,再剥离杂质炭,通过旋风分离器实现催化剂与杂质炭的彻底分离,有利于回收再利用催化剂,通过分离回收催化剂而实现催化剂再生活化以降低加氢催化过程的生产成本,有利提高经济效益,最终分离得到的催化剂收率达到80％以上,纯度达到90％以上。(The invention relates to a separation process of a hydrogenation catalyst, which is based on a set of separation system, wherein a recovery and concentration device comprises a metal sintering pipe filter, a filter pressing kettle, an alkaline washing kettle, an acid washing kettle, a water washing kettle, a baking oven, a baking furnace, an ultrasonic box and a cyclone separator, wherein circulating pumps are arranged at the bottoms of the alkaline washing kettle, the acid washing kettle and the water washing kettle to realize washing circulation of washing liquor; the separation process comprises the following steps: 1) filtering; 2) washing; 3) drying; 4) roasting; 5) separating; in the separation method, the catalyst is primarily separated through filtering and washing, roasting and carbonizing treatment is carried out in inert gas, then the impurity carbon is stripped, the catalyst and the impurity carbon are thoroughly separated through the cyclone separator, the recycling of the catalyst is facilitated, the catalyst is separated and recovered, the regeneration and activation of the catalyst are realized to reduce the production cost in the hydrogenation catalysis process, the economic benefit is improved, the yield of the finally separated catalyst reaches more than 80%, and the purity reaches more than 90%.)

1. A separation process of a hydrogenation catalyst is characterized in that: the separation process is based on a set of separation system, the recovery and concentration device comprises a metal sintering pipe filter (1), a filter pressing kettle (2), an alkali washing kettle (3), an acid washing kettle (4), a water washing kettle (5), a drying oven (6), a roasting oven (7), an ultrasonic box (8) and a cyclone separator (9), and circulating pumps are arranged at the bottoms of the alkali washing kettle (3), the acid washing kettle (4) and the water washing kettle (5) to realize washing circulation of washing liquor;

the separation process comprises the following steps:

1) filtering: filtering the mixed solution containing the hydrogenation catalyst by using a metal sintering tube filter (1), collecting filter residues, transferring the filter residues into a filter pressing kettle (2) for filter pressing by using a nanofiltration membrane, and collecting filter cakes;

2) washing: transferring the filter cake into an alkaline washing kettle (3), adding alkaline washing liquid into the kettle until the filter cake is completely immersed, heating to 50-80 ℃, soaking for 2-5 h, stirring at a stirring speed of 500-1000 r/min for 30-60 min, standing for 30-45 min, transferring the material into a filter pressing kettle for filter pressing, and discarding filtrate;

transferring the filter cake into a pickling kettle (4), adding a pickling solution into the kettle until the filter cake is completely immersed, heating to 50-80 ℃, soaking for 2-3 hours, stirring at a stirring speed of 500-1000 r/min for 30-45 min, standing for 20-30 min, transferring the material into a filter pressing kettle for filter pressing, and removing filtrate;

transferring the filtrate into a washing kettle (5), adding deionized water into the kettle until the filter cake is completely immersed, heating to 50-60 ℃, soaking for 1-2 hours, stirring at a stirring speed of 1000-1500 r/min for 30-60 minutes, standing for 30-45 minutes, transferring the materials into a filter pressing kettle for filter pressing, and discarding the filtrate;

3) drying: putting the washed filter cake into an oven (6) with the temperature of 100-150 ℃ for baking for 2-8 h, cooling to 30-80 ℃, keeping the temperature for 2-5 days, and then crushing the filter cake;

4) roasting: transferring the crushed filter cake into a roasting furnace (7), introducing inert gas into the roasting furnace to remove the gas, then starting roasting, wherein the roasting temperature is 500-850 ℃, the roasting time is 2-8 hours, and slowly cooling to room temperature after roasting;

5) separating: and transferring the cooled roasted material into an ultrasonic box (8), performing low-frequency ultrasonic treatment for 10-30 min, transferring into a cyclone separator (9), and separating impurities in the hydrogenation catalyst at a proper separation speed to finally obtain the separated hydrogenation catalyst.

2. The process of claim 1 for separating a hydrogenation catalyst, wherein: and 2-5 layers of metal filter screens are arranged in the metal sintering pipe filter (1) in the separation process step 1, and movable openings capable of filtering the filter residues everywhere are formed in the side wall of the metal sintering pipe filter.

3. The process of claim 2 for separating a hydrogenation catalyst, wherein: the net aperture of metal filters is 80 ~ 450um, reduces to aperture from last in proper order down.

4. The process of claim 1 for separating a hydrogenation catalyst, wherein: the alkaline solution in the alkaline washing kettle (2) in the separation process step 2 is a mixture of 15-30% strong alkaline solution and 50-75% ethanol solution.

5. The process of claim 1 for separating a hydrogenation catalyst, wherein: the pickling solution in the pickling kettle (3) in the separation process step 2 is a mixture of strong acid solution with the concentration of 5-15% and ethanol solution with the concentration of 30-50%.

6. The process of claim 1 for separating a hydrogenation catalyst, wherein: the inert gas in the separation process step 4 is nitrogen, carbon dioxide or a rare gas.

7. The process of claim 1 for separating a hydrogenation catalyst, wherein: and in the separation process step 5, the ultrasonic frequency of the ultrasonic box (8) is 20K-1000 KHz.

Technical Field

The invention relates to the technical field of hydrogenation catalysis, in particular to a separation process of a hydrogenation catalyst.

Background

With the global annual increase of the demand of high-grade lubricating oil base oil and the gradual increase of environmental protection requirements, the high-grade base oil with II and III high viscosity indexes has strong demand. At present, hydrogenation technology is the main means for producing high-grade lubricant base oil, and meanwhile, the technical means also faces serious challenges, and the development of hydrogenation technology with more excellent performance and higher activity and stability is urgently needed to adapt to the trend of processing more inferior raw materials. The core of hydrogenation technology lies in the development of efficient hydrogenation catalysts.

The hydrogenation catalyst is a very important catalyst in the field of petroleum refining, is widely applied to various hydrogenation processes in the field of petroleum refining, and is used for the purposes of producing clean fuel, improving the feeding property of an oil refining process, improving the yield and quality of oil products and the like. The active metals in the hydrogenation catalyst are generally group VIB and group VIII metals and supported on a support having a porous structure, wherein the active metals provide the desired hydrogenation function. Along with the trend of harsh raw material properties in the petroleum refining process, the product quality requirement is continuously improved, and higher requirements are provided for the performance, including activity and stability, of the hydrogenation catalyst. The history of the development and application of hydrogenation catalysts shows that the improvement of the performance of the hydrogenation catalysts is often closely related to the improvement of the preparation technology. This is because the preparation technique firstly affects the strength of the interaction between the active metal and the support, and then affects the dispersion and sulfidability of the active metal in the catalyst, as well as the type of active phase formed, the size of the active phase and the accessibility of the active phase, and finally the hydrogenation performance of the catalyst. Therefore, research on the preparation method of the hydrogenation catalyst has been one of the hot spots in the field.

The traditional hydrogenation catalyst preparation technology mainly adopts an impregnation method to introduce active components into a carrier pore channel, and then the hydrogenation catalyst is obtained through drying and roasting. In the conventional preparation process, whether the impregnation process or the drying and roasting process is performed, precursor species of the active component and the surface of the Al2O3 tend to have strong interaction, so that the active component is easily dispersed unevenly on the surface of the carrier, the accessibility of an active center is poor, and large crystal grain species with low activity are easily formed (see Bergweffet, Catal. Today2008,130: 117). Moreover, the hydrogenation catalyst is easy to mix with materials after being used, and residual materials are inevitably covered on the surface of the hydrogenation catalyst after being simply filtered, washed and dried, so that strict treatment is required, the materials on the surface of the hydrogenation catalyst can be completely removed, the separation and recovery of the catalyst are realized, the reutilization rate of the catalyst is further improved, the economic benefit is improved, and the production cost is reduced.

Disclosure of Invention

The invention aims to provide a separation process of a hydrogenation catalyst, which aims to realize the clean separation and recovery of the catalyst and the reactivation and utilization of the catalyst by technical means of filtration, washing, drying, roasting, separation and the like.

The invention is realized by the following technical scheme:

a separation process of a hydrogenation catalyst is based on a set of separation system, the recovery and concentration device comprises a metal sintering pipe filter, a filter pressing kettle, an alkaline washing kettle, an acid washing kettle, a water washing kettle, an oven, a roasting furnace, an ultrasonic box and a cyclone separator, and circulating pumps are arranged at the bottoms of the alkaline washing kettle, the acid washing kettle and the water washing kettle to realize washing circulation of washing liquor; the ultrasonic box and the cyclone separator form separation circulation, and the hydrogenation catalyst is separated in high purity and high yield through multiple times of separation of the ultrasonic box and the cyclone separator;

the separation process comprises the following steps:

1) filtering: filtering the mixed solution containing the hydrogenation catalyst by using a metal sintering tube filter, collecting filter residues, transferring the filter residues into a filter pressing kettle, performing filter pressing by using a nanofiltration membrane, and collecting filter cakes;

2-5 layers of metal filter screens are arranged in the metal sintering pipe filter, and a movable opening capable of enabling filter residues to be everywhere is formed in the side wall of the metal sintering pipe filter; the mesh aperture of the metal filter screen is 80-450 um, and the apertures are reduced from top to bottom in sequence;

2) washing: transferring the filter cake into an alkaline washing kettle, adding alkaline washing liquid into the kettle until the filter cake is completely immersed, heating to 50-80 ℃, soaking for 2-5 h, stirring at a stirring speed of 500-1000 r/min for 30-60 min, standing for 30-45 min, transferring the material into a filter pressing kettle for filter pressing, and removing filtrate;

the alkaline solution is a mixture of 15-30% strong alkali solution and 50-75% ethanol solution;

transferring the filter cake into a pickling kettle, adding a pickling solution into the kettle until the filter cake is completely immersed, heating to 50-80 ℃, soaking for 2-3 h, stirring at a stirring speed of 500-1000 r/min for 30-45 min, standing for 20-30 min, transferring the material into a filter pressing kettle for filter pressing, and removing the filtrate;

the pickling solution is a mixture of 5-15% of strong acid solution and 30-50% of ethanol solution;

transferring the filtrate into a washing kettle, adding deionized water into the kettle until the filter cake is completely immersed, heating to 50-60 ℃, soaking for 1-2 h, stirring at a stirring speed of 1000-1500 r/min for 30-60 min, standing for 30-45 min, transferring the material into a filter pressing kettle for filter pressing, and discarding the filtrate;

3) drying: putting the washed filter cake into a drying oven with the temperature of 100-150 ℃ for drying for 2-8 h, then cooling to 30-80 ℃, keeping the temperature for 2-5 days, and then crushing the filter cake;

4) roasting: transferring the crushed filter cake into a roasting furnace, introducing inert gas into the roasting furnace to remove the gas, and then, starting roasting, wherein the roasting temperature is 500-850 ℃, the roasting time is 2-8 hours, and the temperature is slowly reduced to the room temperature after roasting;

the inert gas is nitrogen, carbon dioxide or rare gas;

5) separating: and transferring the cooled roasted material into an ultrasonic box, performing ultrasonic treatment at a low frequency of 20K-1000 KHz for 10-30 min, transferring into a cyclone separator, and separating impurities in the hydrogenation catalyst at a proper separation speed to finally obtain the separated hydrogenation catalyst.

The invention has the beneficial effects that: according to the separation method of the hydrogenation catalyst, the hydrogenation catalyst and materials are preliminarily separated through filtering and washing, impurities attached to the catalyst are carbonized through roasting in inert gas, the impurity carbon is stripped from the catalyst, the catalyst and the impurity carbon are thoroughly separated through the cyclone separator, the catalyst is favorably recycled, the activity of the catalyst is ensured, the phenomenon that the impurities are attached to the surface of the catalyst to inhibit the activity of the catalyst is avoided, the catalyst is separated and recovered to realize the regeneration and activation of the catalyst, the production cost in the hydrogenation catalysis process can be reduced, the economic benefit is favorably improved, the yield of the finally separated catalyst is over 80%, and the purity is over 90%.

Drawings

FIG. 1 is a schematic view of the overall structure of a separation system for a hydrogenation catalyst of the present invention.

In the figure: 1. a metal sintered tube filter; 2. a filter pressing kettle; 3. an alkaline washing kettle; 4. pickling kettle; 5. washing the kettle with water; 6. an oven; 7. roasting furnace; 8. an ultrasonic box; 9. a cyclone separator.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.