The method of manufacture of kataloogidele and adsorbents

 

(57) Abstract:

The invention relates to methods for solid sorbents and catalysts carriers, in particular for use in hydrogenation processes for cleaning oil fractions. From the initial mixture is formed into granules. Dried granules. Then calcined in cycles, alternating in each cycle of annealing the period of increasing temperature with a period of isothermal aging. In the first cycle, the increase of annealing temperature from the maximum temperature of the drying up of the first characteristic temperature. The characteristic temperature determine the corresponding extremum of the dependence of the rate of shrinkage of the material temperature. Subsequent isothermal aging is carried out at a maximum temperature of the first cycle of annealing. In each next cycle of annealing perform the temperature increase of the maximum temperature of the previous cycle the ignition to the next characteristic temperature of isothermal exposure at the maximum temperature of the corresponding cycle of annealing. Repeat successive periods of increasing temperature and isothermal aging before reaching Chechevatov and kataloogidele without the use of additional chemical agents. 7 C.p. f-crystals.

The invention relates to the production of catalysts, more specifically, to methods for solid sorbents and catalysts carriers, in particular for use in hydrogenation processes for cleaning oil fractions.

The main requirements as catalysts for hydrogenation refining processes, along with the activity, selectivity, and high productivity are also high thermal stability, a sufficient mechanical strength of the pellet catalysts and their durability.

A method of obtaining the active alumina as a carrier of catalysts, providing maturation or aging of gels of aluminum hydroxide (Nefedov B. K. and other Catalytic processes deep oil processing. - M.: Chemistry, 1992, S. 146). Aging gels occurs when washing the impurities of sodium, iron, sulfate ions, and can last from several hours to several months. During aging of amorphous aluminum hydroxide crystallization occurs with the formation of a mixture of modifications hydroxides. The rate of aging of aluminum hydroxide and its physico-chemical free is italmost aging determines the size of the crystals and porous structure of aluminum hydroxide. By varying the initial reagents, conditions of deposition and the subsequent processing, it is possible to obtain the aluminum oxide with the desired properties. In General, however, the method of obtaining the active aluminum oxide with presidenial characterized by a large metal - and energy-intensive, low productivity, large amounts of wastewater.

A method of obtaining the active alumina as a catalyst carrier by thermal dispersion of three-hydrate of alumina (see ibid., S. 147 - 149), including the preparation of raw materials, thermal dispersion, hydration product, washing hydrated product from impurities, plasticization of nitric acid, forming granules and heat treatment. In this way, there are practically no inefficient and time-consuming wet operation, which makes the process thermodispersion almost closed.

To obtain a product with desired properties, it is necessary to choose the mode of heat treatment given source modification hydroxide and atmosphere annealing, which allows you to adjust the direction and speed of the processes of dehydration of the hydroxide, crystallization and sintering. The heat treatment includes camping aluminum oxide in an atmosphere of air, containing more than 30% (mol) of water vapor (Japan's bid N 52-20117). To obtain alumina with controlled pore size at the stage of deposition of the use of various organic additives, for example, is introduced into the reaction mixture of urea, thiourea or precipitated gel aluminum hydroxide water-soluble aliphatic acid C4-C22such as citric acid (U.S. patent N 4179411). It is known that to increase the specific surface area and the mechanical strength of the granules of aluminum hydroxide treated with ammonia vapour for 6 to 12 h (ed.St. USSR N 384538). However, all these known methods require either the use of controlled composition of the air environment, or the introduction of air, the mixture of additional components, or the matching process is accompanied by formation of large amounts of wastewater and, as a consequence, the increase in environmental load.

The objective of the invention is to provide a method of manufacturing kataloogidele and adsorbents, overcoming the disadvantages of the known solutions. Achievable technical result is the improvement of mechanical properties, increased strength, durability and thermal stability manufacturing is no exception to the controlled input of additional components, and reducing adverse impacts on the environment due to the substantial reduction of the volume of wastewater.

This technical result is achieved in that in the method of manufacturing kataloogidele and adsorbents, based on the preparation of the initial mixture consisting of the active ingredient and a binder, shaping prepared from the mixture of granules and implementation of heat treatment, including drying and calcination, according to the invention the calcination carried out in cycles, alternating in each cycle of annealing the period of increasing temperature with a period of isothermal exposure, while in the first cycle, the increase of annealing temperature from the maximum temperature of the drying up of the first characteristic temperature, which is determined by the functional dependence of the rate of shrinkage of the material initial mixture temperature, subsequent isothermal aging is carried out at a maximum temperature of the first cycle of ignition in a period of time sufficient to complete shrinkage processes in each of the next cycle of annealing perform the temperature increase of the maximum temperature of the previous cycle the ignition to the next characteristics mixture temperature, with the subsequent isothermal exposure at the maximum temperature of the corresponding cycle of annealing and repeat successive periods of increasing temperature and isothermal aging before reaching the end temperature of the heat treatment.

The first characteristic temperature is defined as corresponding to the first extremum of the velocity dependence of the shrinkage temperature or value not exceeding the average value between the initial temperature of the first cycle of annealing and temperature value that corresponds to the first extremum of the velocity dependence of the shrinkage temperature.

In addition, the rate of temperature rise limit value at which the developed thermal stress is less than the limit of destruction of the material in the granules, preferably in the range of 50 - 100oC/h

In addition, the value of the final heat treatment temperature is defined as the smallest group of values comprising the value of the temperature of the beginning of intensive processes of sintering and reduction of the specific surface, the temperature of decomposition of the active material component of the mixture and the temperature value, which is reached from the four consecutive time intervals of duration 1 - 10 hours each at temperatures of, respectively, 20 - 95oC, 95 - 120oC, 120 - 150oC and 150 - 190oC.

And finally, the calcination is preferably carried out for seven cycles, thus carry out the temperature rise in the first cycle from 190 to 250oC and in the second cycle from 250 to 300oC with isothermal aging for 0.5 - 20 hours each, then carry out the temperature rise in the third cycle from 300 to 350oC and in the fourth cycle of 350 to 400oC with isothermal aging for 0.5 - 20 hours each, and then carry out the temperature rise in the fifth cycle of 400 to 500oC, in the sixth cycle - from 500 to 600oC and in the seventh cycle - from 600 to 700oC with isothermal aging for 0.5 - 30 hours each.

The achievement of the technical result provided by the invention, is justified as follows. Making dried prefabricated elevated mechanical characteristics is achieved by a special regime stage of annealing. The dried semi-finished product is dispersed body, consisting of individual grains separated by then. At grain boundaries may remain adsorbed water or residual solution used on PressTV the ale is a series of processes of different physical nature. First, remove the remnants of moisture from the surface of the grains, and the grains begin to communicate directly between each other. Secondly, when the temperature in the grains begin to occur phase transitions and chemical transformations, for example the decomposition of crystalline. In addition, begin the process of sintering of individual grains. These processes are accompanied by changes of volume of the substance, its porous structure, specific surface area, physical and mechanical characteristics.

Due to volumetric changes of the grains at the boundaries between grains are developing mechanical stress. If the magnitude of these stresses is higher than the tensile strength of individual grains, the grain destruction, i.e., occurs a local defect of the material. When a significant volume changes of such local destruction, together, can form cracks of various sizes and to determine the low mechanical properties of the material.

It is known that the mechanical characteristics of individual grains is improved with increasing heat treatment temperature, and therefore, to ensure high strength of the material, you must choose the treatment is thus to increase the strength characteristics of hotcelebrities.

As a result of research and experimentation it has been found that the above requirement can be satisfied through cyclic mode calcination, namely alternating periods of temperature increase with periods of isothermal aging. The temperature increase from the previous value achieved for the subsequent manufactured with speed, eliminating the possibility of cracking of the material due to uneven heating. Cyclic mode of annealing with a characteristic zones of increasing temperature and isothermal exposure required to achieve a stable material at specific values of temperature and time condition. As a result, the proposed invention is the mode of heat treatment, forming a solid skeleton of the porous body due to the strong growth of the individual grains of the material among themselves without any significant internal stresses between grains.

As you know, there are a number of sources of internal stresses: temperature difference across the sample, causing uneven thermal expansion of the material; due to volumetric changes of the grains in the sample, leading to the displacement of the mass inside Matara), if the gas does not have time to go through the fine pores and then begins to increase the pressure. Research and experiments have shown that the first and third of the above sources of internal stresses fending off slow temperature rise during annealing, and the second slow temperature rise between adjacent critical temperatures and the corresponding isothermal exposure. It was found that the most critical, prevailing over the others are the requirements for the heat treatment associated with the last of the above factors. I.e., when the mode of heat treatment with regard to internal stresses that may occur due to volumetric changes of the grains in the material are automatically satisfied the requirements of other sources of internal stresses.

To determine the temperature and time parameters of heat treatment was experimental curve shrinkage of the material depending on the temperature. Heating of the samples was carried out in a tubular furnace with a controlled rate of heating. The values of the shrinkage of the samples was measured precision quartz dilatometer. The obtained curve allowed us to determine the characteristic values are characteristic temperature, the corresponding local minima and local maxima on the curve shrinkage, namely 200, 300oC, etc.

The obtained values of the characteristic temperatures were used to build the isothermal curves of shrinkage, which allowed to determine the time during which the processes of shrinkage.

Temperature, defined on the basis of the dependency of the shrinkage rate on temperature, and the time intervals are determined from isothermal curves of shrinkage, has allowed to establish the mode of ignition in a cycle consisting of a period of increasing temperature and period of isothermal aging.

The invention is illustrated below with specific examples of its implementation.

Made three versions of products: sorbent on the basis of natural raw materials (clay, diatomite); sorbent-based synthetic natural zeolite and a binder; the carrier of the catalyst for Hydrotreating. The manufacturer was made by technological schemes used in industry.

Example 1. The manufacture of the sorbent on the basis of natural raw materials.

Material - natural aluminosilicate got wet from the career; it was attended by the fraction with a particle size less than 100 microns (dust who/SUB>O3- 7,63

Na2O - 0,11

Fe2O3was 2.25

CaO - 5,3

The first stage of processing was drying. The dried material was grinded in a jaw crusher, then in a ball mill and sieved through a sieve with an opening size of 150 μm. The resulting powder was kneaded with water and was stirred smailey car for 1 h the resulting paste was extrudible on the extruder with a diameter of Spinneret 3 mm Wet extrudates were dried to constant weight in accordance with the following regime: 50oC - 2 h; 100oC - 2 h; 150oC - 2 h; 190oC - 3 hours After that, the dried extrudate was loaded into a tube furnace and was progulivali in accordance with the following regime: 200oC - 2 h; 250oC - 2 h; 300oC - 2 h; 350oC - 0.5 h; 400oC - 0.5 h; 500oC - 2 h; 550oC - 1 h; 600oC - 2 h

Studies have found that when the temperature of annealing above 800oC there was a decrease in the specific surface area of sorbent (deterioration technological properties), so above 700oC search modes were not carried out. Since the desired result was obtained by stepwise heating, it was possible to abandon previously acids, i.e., to improve the environmental component of the M-2, averaged 18 kg/pellet, which corresponds to the index of strength of 6 kg/mm

Example 2. The manufacture of the sorbent on the basis of synthetic zeolite.

To synthetic zeolite, which represents a crystalline substance, to enable forming of the manufactured product was added to the binder to provide the necessary plasticity. As a binder used clay as before baking they are plastic and after calcination gain significant strength characteristics. Zeolite NaX (85 mass%) and binder - clay (15% by weight) in the powdered state was mixed and loaded into emailnow machine, kneaded with water (20 mass%) and was stirred for 1 h the mixture was extrudible on the extruder with a diameter of the nozzle 3 mm, and then dried in a drying Cabinet in accordance with the mode: 50oC - 1 h; 100oC - 2 h; 150oC - 2 h; 190oC - 3 hours After this was carried out by calcining the dried extrudate in accordance with the mode: 200oC - 2 h; 250oC - 2 h; 300oC -2 h; 350oC - 0.5 h; 400oC - 0.5 h; 500oC - 2 h; 550oC - 1 h; 600oC - 2 h

The crushing force, defined on the device PM-2 averaged 11 atora Hydrotreating.

Used cooked pasta of aluminum hydroxide (Bamana paste) production Ryazan refinery, which was extrudible on the extruder with a diameter of a die of 2.1 mm extrudates were dried and then the dried extrudates were hot according to the mode: 200oC - 2 h; 250oC - 2 h; 300oC - 2 h, 350oC - 0.5 h; 400oC - 0.5 h; 500oC - 2 h; 550oC - 1 h; 600oC - 2 h

Originally used an additive a minor amount of phosphoric acid, referring to the formation of aluminum phosphate, which is a good binder, which is also possible sorption. However, ultimately, from the use of acid refused, because the increase in strength due to the speed of heating is significantly higher than from the use of acid, use of which is also entail additional complexity of the process.

The average crushing force, defined on the device PM-2, was 8.3 kg/pellet, which corresponds to the index of strength of 3.9 kg/mm

Considering the fact that, according to the prior art, the average index of strength for typical adsorbents and kataloogidele is about 1.1 kg/mm and only in some cases, under special conditions obratno higher the efficiency of the method, corresponding to the invention, which can greatly enhance the strength characteristics of the adsorbents and kataloogidele without the use of additional chemical agents, weighting the environmental component of the process.

1. The method of manufacture of kataloogidele and adsorbents, which prepare the initial mixture consisting of the active ingredient and a binder, formed from the prepared mixture of granules and perform thermal processing, including drying and calcination, wherein the annealing carried out in cycles, alternating in each cycle of annealing the period of increasing temperature with a period of isothermal exposure, while in the first cycle, the increase of annealing temperature from the maximum temperature of the drying up of the first characteristic temperature, which is determined by the functional dependence of the rate of shrinkage of the material initial mixture temperature, subsequent isothermal aging is carried out at a maximum temperature of the first cycle of annealing in the course of time, sufficient to complete shrinkage processes in each of the next cycle of annealing perform the temperature increase of the maximum temperature Pradyumna the dependence of the rate of shrinkage of the material initial mixture temperature, with the subsequent isothermal exposure at the maximum temperature of the corresponding cycle of annealing and repeat successive periods of increasing temperature and isothermal aging before reaching the end temperature of the heat treatment.

2. The method according to p. 1, wherein the first characteristic temperature is defined as corresponding to the first extremum of the velocity dependence of the shrinkage temperature.

3. The method according to p. 1, wherein the first characteristic temperature select value not exceeding the average value between the initial temperature of the first cycle of annealing and temperature value that corresponds to the first extremum of the velocity dependence of the shrinkage temperature.

4. The method according to p. 2 or 3, characterized in that the rate of temperature rise limit value at which the developed thermal stress is less than the limit of destruction of the material in the granules.

5. The method according to p. 4, characterized in that the rate of temperature rise is chosen in the range of 50 - 100oC/h

6. The method according to any of the preceding items, wherein the final temperature of the heat treatment determines the project and reduce the specific surface area, the temperature of decomposition of the active material component of the mixture and the temperature value at which attained the required level of properties of the manufactured product.

7. The method according to any of paragraphs.1 - 6, characterized in that the drying is carried out in four consecutive time intervals of duration 1 - 10 hours each at temperatures of, respectively, 20 - 95oC, 95 - 120oC, 120 - 150oC, 150 - 190oC.

8. The method according to any of paragraphs.1 to 7, characterized in that the annealing is carried out for seven cycles, thus carry out the temperature rise in the first cycle from 190 to 250oC and in the second cycle - from 250 to 300oC with isothermal aging for 0.5 - 20 hours each, then carry out the temperature rise in the third cycle from 300 to 350oC and in the fourth cycle of 350 to 400oC with isothermal aging for 0.5 - 20 hours each, then carry out the temperature rise in the fifth cycle of 400 to 500oC, in the sixth cycle - from 500 to 600oC and in the seventh cycle from 600 to 700oC with isothermal aging for 0.5 - 30 hours each.

 

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