RU2479619C2 - Pulsation apparatus for delignification of cellulose-containing plant material and method for operation thereof - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: material is fed into a mixer 1 and treated with steam from a pipe 10. The treated material is then fed into a screw feeder 2 which is provided with valve locking device. The reactor 3 is in form of a vertical cylindrical vessel which is provided with means of loading and unloading material and a means of intensifying agitation of the reaction mass, having a pulsation chamber 4, which encloses the reactor 3, and a pulsator - pulse generator 12. Cooking liquor is fed into the reactor 3 through pipe 5. Spent cooking liquor is removed from the reactor 3 through pipe 6. Steam is fed into the reactor 3 through pipe 7, which is fitted with steam injectors. The reaction mass is subjected to acoustic energy pulses with frequency of 5-70 pulsations per minute with energy density of 3-100 MJ/mol. The pulsator - pulse generator 12 consists of a compressor 13, a receiver 14, a pipe 16 and a pulse generator 15. The reaction mass is moved into the top part of the reactor 3 and, using a blade or scrapping device 8 of a screw device 9, the ready product is separated from the cooking liquor to obtain the end product - edible cellulose.

EFFECT: simple reactor design and delignification technology, low power consumption, while improving quality of the cellulose mass.

3 cl, 3 dwg

Description

The claimed technical solution relates to pulsating devices and continuous technologies for the delignification of cellulose-containing plant materials. It can be most effectively used for processing predominantly one-year plant materials with the production of pulp intended for the manufacture of predominantly dietary fiber and other cellulose-containing materials, which can significantly simplify the design of the reactor and the technology of delignification, reduce unit energy costs while improving the quality of the pulp. Technical results are provided due to changes in the design of the reactor, the use of a new pulsating device that provides high-energy acoustic impact on the reaction medium by water hammer.

From the studied prior art, plants for the delignification of plant materials of periodic and continuous action are widely known. In particular, for delignification of wood raw materials, periodic pressure boilers are used that operate under excessive pressure (Pulp and paper production equipment. M: Publishing House "Lesnaya Industriya", 1981, under the editorship of V.A.Chichaev p.58-65, analogue 1).

Known cooking devices (boilers) in connection with the design features have the following disadvantages:

- work at excess pressure (8-12 atm);

- have low safety and environmental performance due to the operation of devices (boilers) under excessive pressure.

- have low productivity;

- have low maintainability.

- also have high metal consumption.

The known devices described in analogue 1 (digesters) are batch apparatuses and, due to their design features, have drawbacks characteristic of these apparatuses in the method for implementing the cooking process, i.e., have a low specific productivity per 1 m ^{3 of} useful volume of the device and, as a consequence of this, is characterized by the above disadvantages.

Widely known multitube cooking installations of horizontal type continuous operation. For example, the installation shown in analogue 2 consists of cooking tubes equipped with screw conveyors. Pipes are located horizontally one above the other in a vertical plane. The number of cooking tubes depends on the type of semi-finished product and the installation capacity and is 2-8 pcs. The diameter of the pipes is 0.6-1.2 m, the length is 6-12 m. These plants are designed for processing wood chips into paper and paperboard in pulp and paper production. In these installations, wood chips from the hopper, having passed the dispenser, are fed by a screw type high pressure feeder into the impregnation pipe. The screw feeder is narrowed towards the loading nozzle of the impregnating pipe, due to which the chips are compacted and excludes the breakthrough of steam from the pipe into the feeder. Compressed wood chips (cork) fall into the impregnation pipe, where, moving to the opposite end of the pipe, under the influence of a screw, steam, pressure, temperature and liquor, the wood chips mix well with the liquor, impregnate and turn into the target cellulose product. After passing successively the cooking tubes, the chips are boiled and then blown through the discharge device into the blowing tank. The cooking temperature in all cooking tubes is maintained at 160-180 ° C, the cooking time is 15-60 minutes (Equipment for pulp and paper production. M: Publishing house "Lesnaya industry", 1981, under the editorship of V.A. Chichaev p.71 -76) (analog 2).

The disadvantages of these settings include:

- high specific heat consumption;

- excessive pressure inside the apparatus;

- the device operates at high temperatures.

Known multi-tube, horizontal horizontal cooking plants described in analogue 2, due to their design features, have drawbacks typical for these devices in the way the cooking process is implemented, that is, they have lower productivity per unit useful volume of the device 1 m ³ , compared with the claimed technical solution, as a result of this, the known method implemented on the known device is characterized by the above disadvantages in obtaining pulp for zvodstva paper and board for the needs of the pulp and paper industries.

Vertical type devices for two-stage continuous pulping are widely known. Cooking equipment consists of two vertical boilers, the upper parts of which are connected by a bypass pipe. From the high-pressure feeder, wood chips and liquor are fed into the lower neck of the digester, in which it moves from bottom to top. The second boiler is also equipped with a circulation system for indirect heating, and the liquor is taken from the lower part of the boiler and, after heating, enters its upper part. From the lower neck of the second boiler, the mass is blown through a concentrator into a blow tank. Cellulose cooking in continuously operating boilers is carried out with a full boiling pot filled with liquor and excessive hydraulic pressure (0.1-0.2 MPa more than the pressure corresponding to the boiling point of the cooking solution)

The working pressure in the boiler, therefore, is equal to 1-1.2 MPa. The applied technique allows to prevent boiling of liquor and thereby create different temperature zones along the height of the boiler (Pulp and paper production equipment. M .: Publishing house "Lesnaya industry", 1981, under the editorship of V.A. Chichaev p.76-77) (analogue 3).

A disadvantage of the known devices is that a high consumption of thermal energy is required, an overpressure inside the apparatus, the apparatus operates at high temperatures, this equipment is intended for the production of industrial pulp for the production of paper and cardboard.

Known vertical-type devices for two-stage continuous pulping, described in analogue 3, due to their design features, have disadvantages characteristic of these apparatuses in the method of implementation of the cooking process, i.e., they have lower productivity per 1 m ^{3 of} useful volume of the device compared to by the claimed technical solution, as a result of this, the known method implemented on the known device (analogue 3) is characterized by the above-mentioned disadvantages in the production of cellulose purpose for the production of paper and cardboard.

The known design of the pulsation apparatus for oxygen-alkaline delignification of plant materials (see analogue 4, p. 61-64, respectively), which is closest to the claimed technical solution in terms of the number of matching features of both structural and process features, and the achieved technical result, except this, the well-known technical solution is intended to implement similar tasks (goals), namely, for the delignification of plant materials.

The device (pulsation apparatus) is a vertical cylindrical vessel with a fixed nozzle (nozzle type "KRIMZ see page 55, Fig. 2 and 3), which has rectangular holes with guide vanes (blades) with periodic loading of raw materials.

The pulsation apparatus for delignification of plant materials is equipped with a pulsator (see page 55 Fig. 2) located outside the cooking apparatus, which is actually a pulsation apparatus, a pulsator and a pulsator piston, which creates fluid oscillations in the vertical direction. Passing the nozzle openings, the fluid acquires a rotational movement due to the direction of the blades (blades). The apparatus operates at a pressure of 1.9-2.1 MPa, at a temperature of 150 ° C (Delignification of plant materials in pulsating apparatus. L.O. Ioffe [et al.] / Chemistry of wood. - 1984. - No. 6. - C. 54-57; and also Ivanov Yu.S., Ioffe L.O., Vorobyov Yu.P., Dvoskin Sh.F. Cellulose production with continuous fiber separation in a pulsation apparatus // Express-Inform. Cellulose, paper, cardboard; issue 5. - M .: VNIPIEIlesprom, 1987. - p. 5-9, analogue 4).

The method of operation of the pulsating apparatus for oxygen-alkaline delignification of plant materials with periodic loading of raw materials consists in the continuous supply of cooking liquid to the reactor by spraying and recycling the cooking solution through the holes of the annular tube. The process is carried out at high (their) overpressure and temperature in a batch reactor with oxygen supply (see analogue 4, p. 55, paragraphs 2-5, respectively) with repeated (35 times) recirculation of the cooking solution and the gas phase (20 times oxygen recirculation), while it is indicated that: “delignification under these conditions proceeded extremely unevenly. Liquid and gas found paths with minimal hydraulic resistance. In these places, the chips turned out to be light and overcooked, while in other areas there was a lot of lack of penetration, and cellulose had a low average degree of polymerization and a dark color. These experiments showed how difficult it is to evenly distribute the liquid and gas throughout the entire volume of the cooking apparatus, even with its small size. In addition, with any mixing system with a cooking solution, single-stage cooking of wood chips will give unsatisfactory results, since the delignification process occurs only on the surface of the wood material. Naturally, under these conditions, the fibers of the surface layers of wood chips will boil much earlier than the fibers of the middle layers, which leads to cellulose of a heterogeneous quality ”(see pages 55, 56, paragraph 3.4). Design and technological disadvantages of this installation include:

- high hydraulic module (1:40);

- the frequency of loading the device;

- low specific productivity per 1 m ³ apparatus;

- small working volume;

- high energy consumption to create a pulsation process;

- overpressure;

- high temperatures;

- this unit is intended solely for the oxygen-alkaline method of delignification;

- the use of a pulsation apparatus is designed to cleave cellulose fragments from the surface of the chip and thereby provide oxygen access to the surface of the chip to oxidize lignin, this process can be implemented with a high hydraulic module (up to 1:40), this requires higher specific energy consumption for creating a pulsation process , which leads to a complication of both the design of the device and the technology of delignification.

The disadvantage of this pulsating device is its low efficiency for intended use, because pulsations are a low-frequency (not more than 5-6 hertz) reciprocating pulse, which is supplied to the liquid phase from the generator (pulsator). The ripple is characterized by an intensity I equal to the product of the oscillation frequency and their amplitude 2A (double amplitude in mm). I is usually 1000-4000 mm / min. Pulsation mixing is more effective than bubble and mechanical mixing, as the entire contents of the autoclave is in motion, and there are no “dead” zones in the reactor (see the description of the pulsation apparatus and the principle of its operation on page 56. Fig. 2 of analogue 4).

Known pulsating cooking apparatus for the delignification of plant materials, described in analogue 4, due to its design features is characterized by the following disadvantages of the method (process):

- the device operates at an overpressure (1.9-2.1 MPa or a pressure of 19-21 atmospheres, respectively), which provides greater metal consumption;

- the device operates under the influence of high temperature (150 ° C);

- the device uses a periodic method of loading;

- the apparatus requires high energy costs to create a pulsating process in the reactor;

- the apparatus has a high explosion and fire hazard due to the use of both high temperatures, pressure, and the use of oxygen in the delignification process.

The claimed technical solution is intended for the processing of predominantly annual plant materials with the production of pulp intended for the manufacture of mainly dietary fiber and other cellulose-containing materials.

The essence of the claimed technical solution is as follows. A pulsation device for the delignification of cellulose-containing vegetable raw materials, made in the form of a vertical cylindrical vessel of the reactor, equipped with means for loading and unloading of raw materials made by means for intensifying mixing of the reaction mass, made in the form of an annular tube placed in the upper part of the reactor, equipped with a spray gun for. the filing of the cooking solution and pulsation device, characterized in that the means for loading the raw material is made in the form of a mixing device consisting of a housing, a rotor, which is a horizontal tubular shaft with mixing spiral turns and bills located on it, a rotor drive connected to a screw feeder, made in the form of a cylindrical body, equipped at the end with a pipe of cylindrical or conical shape with flanges for fastening to the reactor, a screw placed coaxially with the body, and an aporno device, made in the form of a sliding device, means for squeezing and unloading the target product, made in the form of a blade or scraper device connected to a screw device, and the means for intensifying and mixing the reaction mass contains a pulsation chamber and a pulsator-pulse generator, providing the possibility of generation in a pulsating chamber of energy acoustic pulses with a frequency in the range of 5-70 pulsations per minute with a density of energy impact on raw materials, varying from 3 to 100 MJ / mol.

The pulsator-pulse generator according to claim 1, characterized in that it is made in the form of a compressor, receiver, and a pulse generator containing a spool-distributing mechanism, or an intake and exhaust valve system. The method of operation of the pulsating device for the delignification of cellulose-containing vegetable raw materials, which consists in pre-grinding the raw materials, feeding the raw materials to the reactor through the loading device, sealing the reactor, continuously feeding the cooking liquid into the reactor by spraying the circulation liquid through the openings of the annular tube, processing the raw materials in the reactor, and selecting cellulose from cooking solution with the supply of cellulose for washing with subsequent extraction of cellulose, characterized in that the raw materials are fed continuously into the mixer, in which the first is carried out - preliminary compression and loosening of the raw materials by means of a rotor, which is a shaft with coils located on it, with beats with a reverse coil at the end of the rotor at the outlet pipe, with a parallel or sequential supply of cooking solution to the loosening zone in the mixer and steam, then the raw materials are loosened by means of a turn of the screw of the reverse direction and fed to a screw feeder, in which the second compression of the raw materials is carried out by means of a screw of a screw feeder, d Then the raw material is fed into the nozzle of the screw feeder-cork former, in which an additional third compression of the raw material is performed, bringing the density of the raw material to a state that prevents the cooking liquor from flowing out of the reactor, with the possibility of parallel feeding of the cooking liquor into the nozzle of the screw feeder; the reactor due to the one-time impact of the flotation effect and pulsation effects and delignification in the entire reactor volume due to the pulsation device, ensuring creating (generating) energy (acoustic) pulses to the processed raw materials located in the reactor with a frequency in the range of 5-70 pulsations per minute and exposure density (energy pulse) in the range from 3 to 100 MJ / mol, with parallel exposure to steam on raw materials, then loosening (mixing) the raw materials with a blade or scraper device to ensure the movement of raw materials in the screw device, then compressing the raw materials in order to release it from the cooking liquor on a screw device, then additional compression of the raw material is performed at the exit of the screw device in its conical part with the possibility of more efficiently squeezing the pulp from the cooking solution and creating a tube of cellulose at the exit of the device to ensure the possible discharge of steam and or cooking solution from the reactor, followed by unloading product from the pulsating device, with the receipt of the target product of food pulp.

The claimed technical solution in comparison with the prototype is devoid of the above structural and technological disadvantages, is illustrated in figures 1-3, which show respectively:

Figure 1 is a schematic diagram of the claimed device;

Figure 2 shows a diagram of an example of a specific implementation of the device;

Figure 3 shows the basic operational block diagram of the delignification process in the claimed device.

The claimed technical solution ensures the implementation of the following technical tasks (goals) achieved due to the design features of the claimed device, in combination with the features of the method, which are given separately below in relation to the device and method (technological process).

The claimed technical solution in comparison with the prototype ensures the implementation of the following goals (tasks), realized, according to the applicant, mainly due to the design features of the claimed technical solution;

1 - the device has a low hydraulic module 4 times smaller than that of the prototype due to the design features of the device - due to the lack of moving parts and fixed elements in the reaction zone of the apparatus, preventing the movement of raw materials in the device;

2 - the device has a high specific productivity per unit working volume of 1 m ³ due to the absence of moving parts in the reaction zone of the apparatus;

3 - the device ensures the effective operation of the device (reactor) at atmospheric pressure due to the superposition of the countercurrent effect of the reagents (raw materials and cooking liquor) and the pulsating effect (effect) on the reaction mass;

4 - the device ensures the operability of the apparatus at lower temperatures (up to 95 ° С-100 ° С) due to the superposition of the countercurrent effect of the reagents (raw materials and cooking liquor) and the pulsating effect (effect) on the reaction mass;

5 - the device provides a lower comparable consumption of reagents due to the implementation of the process of regeneration of the cooking solution;

6 - the device provides a low energy consumption due to the occurrence of a synergistic effect arising from the structural and technological features of the claimed device and its operation;

7 - the device provides high reliability of the device due to the exclusion of moving parts and elements in the reaction zone of the apparatus (reactor);

8 - the device provides the ability to implement simplified remote maintenance by minimizing the use of the necessary for the process of delignification of instrumentation and apparatus;

9 - the device provides high maintainability due to the absence of moving parts and fixed elements in the reaction zone of the apparatus (reactor);

10 - the device provides the possibility of using ceramics and plastics for the manufacture of structural elements of the reactor mainly by simplifying the design of the reactor and its elements in contact with the cooking solution).

The claimed technical solution in relation to the claimed method (technology) provides the following advantages compared to the method used in the prototype, the advantages are created due to the interaction and combination of features of the device and method implemented in the claimed technical solution:

1 - the method ensures the effective operation of the device (reactor) at atmospheric pressure due to the superposition of the countercurrent effect of the reagents (raw materials and cooking liquor) and the pulsating effect (effect) on the reaction mass;

2 - the method ensures the operability of the apparatus at lower temperatures (up to 95 ° C), this result is achieved by superimposing the countercurrent effect of the reagents (raw materials and cooking liquor) and the pulsating effect (effect) on the reaction mass;

3 - the method provides a low consumption of reagents due to the implementation of the process of regeneration of the cooking solution;

4 - the method provides low energy consumption due to the occurrence of a synergistic effect - the mutual influence of the structural and technological features of the claimed device (method of operation);

5 - the method provides the possibility of using ceramics and plastics for the manufacture of structural elements of the device (mainly the reactor) by eliminating the need to install moving parts and fixed elements in the reaction zone of the apparatus (reactor) in contact with the cooking solution;

6 - the method ensures the operability of the device in principle and the implementation of the stated goals due to the original combination of structural elements and the method, which consists in ensuring the tightness of the device by creating an impervious to the cooking solution tube from raw materials in the lower part of the device (at the input of raw materials to the reactor) and the same a kind of impermeable plug at the outlet of the target product from the reactor, which prevents the release of both steam and cooking liquor from the device.

In addition, in addition to the listed technical advantages of the claimed technical solution, the following can be attributed:

- conducting the delignification process in countercurrent (as opposed to the prototype) with pulsating or energy (acoustic) effects on the raw materials, which significantly increases the efficiency of the process, which makes diffusion of the cooking solution into raw materials in the reactor and subsequent extraction of lignin from raw materials into cooking solution.

The applicant draws attention to the fact that in both figures well-known devices, for example, mixers, etc., are shown conditionally (schematically) to avoid unnecessary clutter of the figures, and text descriptions are given in more detail.

The technical solution is a column mass transfer apparatus with countercurrent movement of the reaction masses and is intended for delignification of mainly plant materials.

The device depicted in figure 1 (General view of the claimed device) consists of a mixer 1, consisting of a housing, a rotor and a rotor drive (in figures 1, 2 the elements are not detailed in order not to clutter the drawing). The mixer rotor is a horizontal tubular shaft with mixing screw-like coils and bills located on it; at the mixer inlet, the rotor is equipped with 1.5–2 turns, then a series of mixing beats follows, then again 1.5–2 mixing coils, a reverse coil is placed at the end of the rotor at the outlet directions for intensification of the process of unloading of raw materials due to its loosening. This design provides the most effective process of preliminary preparation of the reaction mass (preferably at least twice) by compressing the reaction mass with turns of the mixer and then loosening it with bills, then loosening it with a mixing coil with a reverse spiral direction, which ensures intensive mixing of the reaction mass with the cooking solution , in the mixer 1 there is further placed a screw feeder 2, made in the form of a cylindrical body, equipped at the end with a pipe a single or conical shape with flanges for fastening to the reactor before the raw material enters the reactor 3, a screw placed coaxially to the housing, a locking device made, for example, in the form of a slide device (in Fig. 1, 2, the locking device is made in the form of a slide, which is presented conditionally and not indicated by the position number to prevent clutter of Fig. 1, 2).

It should be noted that as a locking device, any other device (means) can be installed that is functionally designed to control the overlap of the cross section of the screw feeder at the beginning of the declared pulsating device, which serves to create a plug after the screw feeder, which ensures the operability of the pulsating device in whole since in the absence of this plug, all raw materials with a cooking solution at a temperature of about 100 ° C and a mass of several tons will inevitably pour out of the reactor through a screw feeder 2.

Given the above, it can be stated that the locking device, made in the form of a gate, can be made in any design, while the purpose of the locking device is to create a plug of raw materials at the end of a screw feeder (feeder pipe), made in the form of a cylindrical or conical pipe with flanges for fastening to the reactor, placed in front of the input of raw materials into the reactor 3 in the form of compressed raw materials (in the form of a cork). The design of the locking device can be made, for example, in the form of a pair of cone-saddle or other similar device with a manual or mechanized (automated) drive, designed, firstly, to create a plug at the time the device is put into operation, to conduct the delignification process (cooking ) cellulose, secondly, to overlap the cross section of the screw feeder, if necessary, stop the delignification process or to carry out preventive (repair) work on the pulsating device.

Next, there is a screw feeder tube (cork former), made in the form of a cylindrical or conical pipe with flanges for fastening to the reactor, which is a cork former itself (in figure 1, 2 the cork former is not shown as a separate position to prevent clutter of the drawings), it is intended to create corks from raw materials and cooking liquor, provides additional compression of the reaction mass, which:

- prevents the leakage of cooking liquid from the device into the mixer during the start-up of the device, thereby ensuring the operability of the device both at the initial stage when the installation starts and during the operation of the device when it enters the operating mode and ends work, and when the declared pulsating device stops;

- provides additional intensification of the mixing of the reaction mass, because after passing the locking device, the reaction mass (raw materials) under the influence of a pneumatic pulsator (pulse generator) and the flotation effect is again loosened.

A nozzle is placed in the nozzle of the feeder (not shown in FIGS. 1, 2 to prevent clutter of the drawings), intended (if necessary) to provide the possibility of supplying an impregnating liquid (for example, cooking solution) to it. The reactor 3 is made in the form of a predominantly hollow cylindrical tank, a coaxial pulsation chamber 4, covering the reactor 3, from the outside, a pipe 5 for supplying the cooking solution to the reactor located in the upper part of the reactor, a pipe 6 for draining the spent cooking solution from the reactor located in the upper part a pulsation chamber 4, a steam line 7 installed in the lower part of the reactor, mainly along or coaxially with its (reactor) vertical axis, which is a pipe equipped with steam injectors, located mainly radially on the steam line 7 (not shown in FIGS. 1, 2 to prevent clutter of the drawings), a blade or scraper device 8, a screw device 9 for squeezing and unloading pulp, a pipe 10 for draining the spent cooking solution, device 11 for separating lignin from spent cooking liquor, a pulsator-pulse generator 12, designed to transmit a hydraulic pulse (hydraulic shock) to the raw materials in the reactor 3 by means of action on the surface of the cooking liquor present in the pulsation chamber 4, pneumatic pulses generated by pulse generator 12 pulsator.

The device shown in Fig. 1 consists of the following elements: a mixer 1, a screw feeder 2, a reactor 3, a pulsation chamber 4, a pipe 5 for supplying a cooking solution to the reactor, a pipe 6 for draining the spent cooking solution from the reactor, a steam pipe 7, a blade or a scraper device 8, a screw device 9, a pipeline 10 for removing the spent cooking solution, a device 11 for separating lignin from the spent cooking solution, a pulsator-pulse generator 12, designed to transmit hydra influential or energy (acoustic) impulse (water hammer) on the raw materials in the reactor 3 by exposing the surface of the cooking solution in the pulsation chamber 4 to pneumatic pulses generated by the pulsator-pulse generator 12.

The claimed device operates as follows.

The raw material (crushed straw) is fed into the mixer 1, in which it is subjected to steam treatment (in Figs. 1, 2, the steam supply is indicated arbitrarily by the arrow "steam"), while in the mixer 1 and in the screw feeder 2 at the same time the cooking solution is fed by means of a pipe 10 equal or unequal shares, depending on the characteristics of the state of the feedstock. In the mixer 1 and the feeder 2, the raw material is pre-impregnated with the cooking liquor coming from the pipeline 10, while in order to intensify the delignification process, the coolant is supplied to the mixer 1 and to the central part of the reactor 3 through the steam pipe 7 (for example, steam injectors) (for example steam, hot steam, hot or superheated water).

Next, the pre-prepared raw material impregnated with the cooking solution and processed with a coolant (for example, steam) from the mixer 1 enters the screw feeder 2, from which, due to the rotation of the screw located in the feeder 2, the raw material is transferred to the reactor 3. At the same time, to ensure the process temperature in the Central part of the reactor 3 through the steam line 7 additionally, through, for example, steam injectors, serves coolant (for example, steam, hot or superheated water).

Further, when the reaction mass (raw materials and cooking liquor) is exposed to hydraulic (acoustic) pulses (directed upward) generated by the pulsator-pulse generator 12 simultaneously, through the pulse conduit (pulse conduit not shown in Fig. 1), the reaction mass is exposed to the cooking liquor in countercurrent and moves to the upper part of the reactor, from which, by means of a blade or scraper device 8 and a screw device 9 for pressing and unloading, the pulp is subjected to extraction from the cooking solution and ygruzke for future use.

Thus, the processed raw materials (see figure 3), starting with the receipt of the mixer is subjected to the following influences that characterize the essential features of the claimed method of operation of the device, necessary and sufficient for the implementation of the claimed method in the claimed device. Figure 3 shows the basic operational block diagram of the process of delignification.

The following is a detailed operational description of the processing of raw materials at each of the component nodes (elements) of the claimed device.

Mixer 1

Operation No. 1 - the first compression with a simultaneous supply of the cooking solution and steam into the mixer with raw materials under the influence of the rotational movement of the rotor on the raw materials, equipped with mixing coils and bills, while the mixing coils of the rotor provide the first compression of the raw material.

Operation No. 2 - the beater located on the rotor provides loosening of raw materials, and if necessary, operations No. 1 and No. 2 can be repeated by installing additional sections of mixing turns and beats on the rotor shaft, while parallel to mixer 1 and screw feeder 2 is provided supply of cooking solution and steam.

Screw feeder 2

Operation No. 3 - in a screw feeder equipped with a screw and a locking device, the raw material is subjected to repeated compressive action by means of a screw, which is necessary for more effective wetting and mixing of the reaction mass with the cooking solution.

Operation No. 4 - the raw materials for creating the cork are fed into the feeder pipe (cork former), this operation is fundamentally important for the implementation of the claimed process, because it allows you to eliminate the breakthrough of the cooking solution in the feeder and mixer from the reactor, because the height of the reactor is at least 5 m, and the volume of the reactor is at least 4 m ^{3 of} solution at temperatures up to 100 ° C (it should be noted that a breakthrough of the cooking solution in the screw feeder is fraught with unpredictable consequences).

Reactor 3

Operation No. 5 - further in the reactor 3, the raw material is subjected to the next mixing (loosening) due to the effect of the flotation effect.

Operation No. 6 is a pulsating (acoustic) effect on the reaction mass due to the action of a pulse generator 12 on the raw materials, and the vector of these forces directs the reaction mass to the upper part of the reactor, while reducing the necessary force on the shaft of the screw feeder and increasing the overall efficiency of the device, respectively.

Operation No. 7 - on the raw materials, in parallel with the effects of operations No. 5 and 6, the steam is affected by supplying it preferably to the central part of the reactor through the steam line 7. Thus, in the reactor three operations No. 5, No. 6, No. 7 are simultaneously affected by the raw materials.

Paddle or scraper device 8

Operation No. 8 - further, the raw materials from the upper part of the reactor, by means of a blade or scraper device 8, are again subjected to loosening.

Screw device 9

Operation No. 9 - in a screw device 9, the raw material is subjected to the next squeezing (compression) in order to free it from the cooking solution, by means of a screw.

Operation No. 10 - the raw material at the exit of the screw device 9 is displaced by the screw for unloading, creating at the exit of the screw device 9 (in its conical part) a cork from the finished pulp, which is then fed to for further processing.

It should be noted that the lower loading of the reactor with raw materials is not obvious to a person skilled in the art both technological and constructive solution and is due to the need to realize the goals. The claimed solution is dictated both by the need to provide preliminary preparation of raw materials for feeding into the reactor, and by the need to increase the productivity of the device while simplifying the design and improving the quality of the resulting product — food pulp.

The flotation properties of raw materials (in this case straw), due to the presence of air bubbles in it, were used by the applicant to intensify the delignification process, taking into account the additional effect of the hydraulic (acoustic) impulse on the raw material.

Thus, in the inventive device, the raw material during the implementation of the inventive method is subjected to at least ten times the mechanical action of compressive and loosening forces by exposing the raw materials to various parts and elements of the inventive device, which are additionally superimposed with a chemical (cooking solution), thermal effect (temperature as a solution, and steam) throughout the entire process of processing raw materials into edible cellulose. Moreover, in the reactor 3, the feedstock is subjected to an additional pulsating energy (acoustic) effect, which creates the most favorable conditions for the extraction of lignin from the feedstock and to obtain the target product — food pulp.

An example of a preferred embodiment of the actual pulsator-pulse generator

Actually the pulsator-pulse generator 12, shown in figure 2 and limited by a dash-dot line, consists of (made) of:

- a source of compressed gas 13 (compressor);

- receiver 14;

- pipeline 16;

- a pulse generator 15 (made of a spool-distributing mechanism or of a valve system (intake and exhaust valves) manufactured by ADL (Netherlands) or domestic manufacturers (for example, ISTA fast-acting valves, brands KB-35D UHL2 or KB-40 UHL2 ™, opening time 0.001 sec, closing time 0.002 sec, operating pressure range from 0.1 to 1 MPa).

The applicant draws attention to the fact that the selection of the above devices with the specified parameters of the speed of opening and closing most effectively ensures the implementation of the tasks (technical results).

An example of a preferred embodiment of the claimed device and implementation of the method on the claimed device is shown in Fig.2.

The device shown in figure 2, consists of the following elements: mixer 1, screw feeder 2, reactor 3, pulsation chamber 4, pipe 5 for feeding the cooking solution into the reactor, pipe 6 for draining the spent cooking solution from the reactor, steam pipe 7, paddle or scraper device 8, screw device 9, pipe 10 for draining spent cooking liquor, device 11 for separating lignin from spent cooking liquor, pulsating pipe 12, designed to transmit a hydraulic impulse a (water hammer) at the feedstock in the reactor 3 by acting on the surface of the cooking liquor present in the pulsation chamber 4, pneumatic pulses generated by the pneumatic pulsator pulse generator 12 which consists of the following elements:

- a source of compressed gas 13 (compressor);

- receiver 14;

- pipeline 16;

- pulse generator 15.

The embodiment of the pulsating device shown in Fig. 2 (pulsator-pulse generator 12) is the most preferred particular embodiment of the claimed technical solution (device and method), which is practically manufactured and tested by the applicant in the form of a pilot installation; the present technical solution of the goal (task), namely, the modes of conducting the process and the most effective values of the technological parameters of the cooking process of raw materials, those temperature, concentration of cooking liquids, hydromodule, process duration.

The feedstock (for example, crushed straw) is fed into the mixer 1, after filling the mixer, the reactor with raw materials into the space between the turns of the screw and the beater, steam is supplied, this place of steam supply and time (after filling the mixer) are selected in order to exclude the possibility steam breakthrough from the mixer in both directions: towards the loading of raw materials and towards feeding into the screw feeder 2.

In this case, after filling the raw materials with mixer 1 and the screw feeder 2, the cooking liquor is supplied in equal or unequal proportions, depending on the characteristics of the feedstock, in which the raw material is preliminarily impregnated with the cooking solution coming from pipeline 5, with the aim of intensifying the process delignification in the mixer 1 and in the Central part of the reactor 3 through the steam pipe 7 is supplied coolant (for example steam, hot or superheated water).

Next, the raw material impregnated with the cooking solution and processed with the coolant from the mixer 1 enters the screw feeder 2, from which, due to the rotation of the screw of the feeder 2, it is transferred to the reactor 3, then, when the reaction mass (raw material and cooking solution) is exposed to hydraulic pulses generated by the generator pulses (pulsator-pulse generator 12) transmitted through the pipeline (pulse conduit) 16, the reaction mass is subjected to intense action of the cooking solution in countercurrent and moves to the upper part of the reactor, from which, by means of a blade or scraper device 8, a screw device 9 for unloading and squeezing the pulp, the finished product — food pulp — is supplied for further processing for bleaching or is supplied for further processing if necessary.

The pneumatic pulsation system shown in figure 2, indicated by the general position of the pulsator-pulse generator 12, is limited from the other elements of the device by a dot-dash line, is a spool-distributing mechanism and a valve system described above, structurally associated with a compressed air source - receiver and compressor .

The pulsation system operates as follows.

A pulsator-pulse generator 12 (limited by a dash-dot line), consisting of a spool-distributing mechanism or a system of valves - inlet and outlet valves, a source of compressed gas, remotely generates hydraulic pulses in a pulsation chamber 4 through a pipeline (pulse pipeline) 16 (energy impact of a certain power ) with a frequency of 5-70 vibrations per minute (corresponding to a frequency of 0.83-1.1666 Hz) and a specific power of 3 to 100 MJ / mol. As a source of energy (acoustic) impact - a pulse generator, any device (means) known in science and technology can be used that provides the creation of energy (acoustic) impact (pulse generation) on the processed raw materials in the reactor, in the frequency range of 5-70 vibrations per minute and with a specific power of 3 to 100 MJ / mol, for example, a mechanical vibrator generator made in the form of an eccentric mechanism, for example, like an electric hammer drill, electromagnetic a generator made in the form of a vibrating device used in electric spray guns, a hydraulic vibrating apparatus, the working element of which is a membrane, when a stream of liquid or gas breaks, vibration is transmitted to the membrane, and from it to the processed medium of the piezoelectric vibrating element, the working element of which is a piezocrystal and etc., since the technical result of this effect on the raw material is the creation of a cavitation effect in the reaction mass of the raw material, leading to ifikatsii delignification process due to the fact that the influence appears at both the macro and the microbubbles of air, steam, cooking liquor being in the reaction mass reactor. By analogy with the claimed device for delignification, in which a pneumatic pulse generator is used, we can give a classic example of a device for pulling a cable under a roadway or embankments without stripping, working under the influence of an elastic element (invention according to the a.s. of the USSR), made in in the form of a steel spring, which, as you know, has been successfully circumvented by a patent issued by Japanese applicants, in which, instead of the elastic element stated in the formula, made of a steel spring, other elastic elements were used in the formula, for example, pneumatic, electromagnetic, elastic elements that perform the equivalent function of a steel spring - vibration, which, acting on the ground, provided the device under the ground in a given direction. Given the foregoing, the sign of a pneumatic pulse generator (pulsator-pulse generator) 12, shown in the distinctive part of the claimed claims, is formulated at the level of a generic term (concept), namely, the pulse generator is made in the form of a source of energy (acoustic) impact on the reaction medium and is characterized the parameters declared in the formula.

The above formulation of the sign, according to the applicant, will provide a wider scope of patent protection and may reduce the likelihood of negative consequences when the applicant delivers food pulp equipment and technology to one of the large enterprises of the Russian Federation, which plans to start production of its own food pulp in exchange for purchased abroad leading manufacturing companies. At the same time, it can be assumed that the refusal to purchase raw materials from the Russian consumer for import (import substitution) can cause (or provoke) not only claims of foreign suppliers (loss of part or all of the Russian market), but also their desire to circumvent or invalidate a patent granted according to this application, if there is an appropriate expert decision, because according to the information available to the applicant on the filing date of this application, the lion's share of food pulp is currently supplied to enterprises of the Russian Federation from abroad. Moreover, the absurdity of the situation lies in the fact that having their own colossal resources of raw materials (straw, sawdust, etc.), enterprises of the Russian Federation purchase food pulp for import, because in the Russian Federation, according to the applicant, at the filing date of this application, there is no competitive equipment and technology for the production of food cellulose, the share of food cellulose and other additives in food products, for example in sausage, reaches up to 50% or more, the volume of purchases on import in the Russian Federation for needs, including the food industry, reaches enormous amounts.

According to the applicant, this kind of energy (acoustic) effect on the processed raw materials in the reactor causes an extremely effective effect on the processed raw materials both at the macro and micro levels, and the effectiveness of the impact is explained by the following reasons:

- with a sharp interruption of the air flow in the pulse conduit 12 by means of a spool-distributing mechanism or from a system of valves (inlet and outlet valves) that are triggered in thousandths of a second (from 0.001 sec - opening the valve, from 0.002 sec - closing the valve), a significant vacuum is created behind the valve, which instantly in the form of a shock energy (acoustic) wave propagates throughout the reactor volume, tearing (exploding from the inside) macro- and microbubbles of air contained in the raw material, and then the presence of a shock wave of the opposite direction, which ensures the collapse of macro- and microbubbles in the reaction mass, as a result of this there is a cavitation effect (cavitation from lat. cavitas - void) - the formation in the liquid of cavities (cavitation bubbles, or caverns) filled with gas, steam or a mixture thereof. Cavitation occurs as a result of a local decrease in pressure in the liquid, which can occur either with an increase in its velocity (hydrodynamic cavitation), or with the passage of a high-intensity acoustic wave during the rarefaction half-cycle (acoustic cavitation), and there are other reasons for the effect to occur. Moving with the flow to a region with a higher pressure, or during a half-period of compression, the cavitation bubble closes, emitting a shock wave. Cavitation destroys the surface of the impact of the shock wave on the raw material, which provides the occurrence of the cavitation effect and the resulting chaotic imposition of various kinds of physical, chemical, hydrodynamic effects, which result in phenomena occurring in the reactor due to the action of the pulse generator on the raw materials with a frequency of 5 to 70 once per minute, with an exposure power in the range from 3 to 100 MJ / mol, which has an effective effect on the entire heterogeneous system located in factor, which ultimately ensures the implementation of the results stated in this technical solution, namely, the temperature of the process is reduced (up to 100 ° C), there is no need to use excess pressure in the reactor (up to 100% or more), the specific productivity of the device during the process is increased delignification (2-5 times) while improving the quality of food pulp obtained, there are no cases of lack of penetration of raw materials and its destruction, because, according to the applicant, in the claimed technical solution, the process lignification conducted due to mass-transfer processes (effects) occurring at both macro (minced raw element) and micro (cell level) levels. Based on the information studied, it can be assumed that as a result of a pulsating (acoustic) effect on the raw materials, when the spool device 12 or valves are suddenly shut and open, the pressure in the reactor instantly decreases, and this leads to the process of explosive boiling and subsequent collapse of air microbubbles in the raw material in the entire volume of the reactor.

It should be noted that a pneumatic or hydraulic shock in most cases is an undesirable phenomenon in technology, the appearance of which they try to avoid, which can lead to the destruction of structures (equipment) or to emergency situations due to the high destructive potential known from the prior art.

In the claimed technical solution, the applicant used this well-known negative effect of pneumatic or hydraulic shock to intensify the chemical-technological process of delignification of raw materials, which leads to non-obvious technical results for the specialist in the claimed field of technology.

Thus, the energy (acoustic) effect of a certain power created by the pulse generator, passing through the cooking solution located in the pulsation chamber 4, with a power of shock (hydraulic shock) from 3 to 100 MJ / mol provides the formation of many dynamically developing bubbles that can be considered as a kind of microtransformers that convert the potential energy accumulated in the system into the kinetic energy of a liquid, distributed discretely in space and in time.

The claimed technical solution meets the criterion of "novelty" presented to the invention, because from the investigated prior art, no technical solutions have been identified that match the design features of the device and the technology used.

The claimed technical solution meets the criterion of "inventive step" presented to the invention, because The claimed technical solution is not obvious to a specialist in the selected field of technology, because leads to the implementation of seemingly mutually exclusive technical results for the specialist, namely, the claimed technical solution provides an increase in the specific productivity of the installation while reducing energy costs - temperature, pressure, simplifying the design and technology of the cooking process (due to the use of a pulsating device as well) while eliminating the need for additional reagents (such as oxygen - the prototype) in the claimed technical solution, leads to considerably increase the target product quality while increasing environmental friendliness and safety of the process as a whole.

Thus, for a person skilled in the art, the obtained technical results, significantly superior to those known to a person skilled in the art, are not obvious in the art, this is an additional confirmation of the conformity of the claimed solution to the criterion of "inventive step".

The claimed technical solution meets the criterion of "industrial applicability" presented to the invention, because The claimed technical solution was implemented in the form of a pilot installation at one of the enterprises of the Russian Federation, and all the declared technical results (goals) were obtained that far exceed the known indicators of installations of a similar purpose known at the filing date of this application.

Information sources

1. Processes and apparatuses of chemical technology. Transport phenomena, macrokinetics, similarity, modeling design. In 5th vol. T.2: Mechanical and hydromechanical processes. / Ed. A.M. Kutepova. - M .: Logos, 2001 .-- 600 p.

2. M.A. Promtov. "Machines and apparatus with pulsed energy effects." Textbook "Publishing House Engineering-1", 2004).

3. Equipment for pulp and paper production. M .: Publishing house "Forest industry", 1981, under. Ed. V.A. Chichaeva, p. 58-65, analogue 1.

4. Equipment for pulp and paper production. M .: Publishing house "Forest industry", 1981, under. Ed. V.A. Chichaeva, p. 71-76, analogue 2.

5. Equipment for pulp and paper production. M .: Publishing house "Forest industry", 1981, under. Ed. V.A. Chichaev, p. 76-77, analog 3.

6. Delignification of plant materials in pulsating equipment L.O. Ioffe [et al.] / Chemistry of wood. - 1984. - No. 6. - S. 54-57; and also Ivanov Yu.S., Ioffe L.O., Vorobyov Yu.P., Dvoskin Sh.F. Cellulose production with continuous fiber separation in a pulsating apparatus // Express-inform. swelling. production experience. Cellulose, paper, cardboard; issue 5. - M.: VNIPIEIlesprom, 1987.- P.5-9, analog 4.

Claims (3)

1. A pulsation device for the delignification of cellulose-containing vegetable raw materials, made in the form of a vertical cylindrical vessel-reactor, equipped with means for loading and unloading raw materials, means for intensifying the mixing of the reaction mass, made in the form of an annular tube placed in the upper part of the reactor, equipped with a sprayer for feeding cooking solution and a pulsator-pulse generator, characterized in that the means for loading raw materials is made in the form of a mixing device, consisting it from the housing, the rotor, which is a horizontal tubular shaft with mixing screw-like coils and bars located on it, the rotor drive connected to a screw feeder, made in the form of a cylindrical housing, equipped at the end with a pipe of cylindrical or conical shape with flanges for fastening to the reactor, a screw placed coaxially to the housing and a locking device made in the form of a slide device, the means for pressing and unloading the target product is made in the form of a blade or scraper a device connected to a screw device, and the means for intensifying the stirring of the reaction mass contains a pulsation chamber and a pulsator-pulse generator, which makes it possible to generate energy-acoustic pulses in the pulsation chamber with a frequency in the range of 5-70 pulsations per minute with an energy density on the raw material, ranging from 3 to 100 MJ / mol. 2. The pulsation device according to claim 1, characterized in that the pulsator-pulse generator is made in the form of a compressor, receiver and pulse generator containing a spool-distributing mechanism, or an intake and exhaust valve system. 3. The method of operation of the pulsating device for the delignification of cellulose-containing vegetable raw materials, which consists in pre-grinding the raw materials, feeding the raw materials to the reactor through the loading device, sealing the reactor, continuously feeding the cooking liquid into the reactor by spraying the circulation liquid through the openings of the annular tube, processing the raw materials in the reactor, and selecting cellulose from the cooking liquor with the supply of pulp for washing, followed by the extraction of pulp, characterized in that the raw material is fed discontinuously into the mixer, in which the first preliminary compression and loosening of the raw material is carried out by means of a rotor, which is a shaft with coils and bills located on it with a reverse screw at the end of the rotor at the outlet pipe, with a parallel or sequential supply of cooking solution to the loosening zone in the mixer and steam, then the raw material is loosened by means of a turn of the screw of the reverse direction and fed to a screw feeder, in which the second compression of the raw material is carried out by means of a screw of a screw feeder, Further, the raw material is fed into the nozzle of the screw feeder - cork former, in which an additional third compression of the raw material is performed, bringing the density of the raw material to a state that prevents the cooking liquor from flowing out of the reactor, with the possibility of parallel feeding of the cooking liquor into the nozzle of the screw feeder, then the next loosening of the raw material is carried out when entering the reactor due to the one-time effect of the flotation effect and pulsation effect and delignification in the entire reactor volume due to the pulsator-pulse generator providing the creation (generation) of energy - acoustic pulses to the processed raw materials in the reactor, with a frequency in the range of 5-70 pulsations per minute and energy density (energy pulse) in the range from 3 to 100 MJ / mol, with parallel exposure to steam on raw materials, then loosening (mixing) the raw materials with a blade or scraper device to ensure the movement of raw materials in the screw device, then compressing the raw materials in order to release them - squeezing them from varo solution on the screw device, then additionally compress the raw materials at the exit of the screw device in its conical part with the possibility of more efficient extraction of cellulose from the cooking solution and create a tube of cellulose at the exit of the device to exclude the possible discharge of steam and / or cooking solution from the reactor with subsequent unloading of the product from the pulsating device, with the receipt of the target product is food pulp.

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