Multitubular reactor, the method of the catalytic oxidation in the vapor phase with usage of the multitubular reactor, and the method of the multitubular reactor start-up

IPC classes for russian patent Multitubular reactor, the method of the catalytic oxidation in the vapor phase with usage of the multitubular reactor, and the method of the multitubular reactor start-up (RU 2309794):

C07C45/35 - in propene or isobutene

B01J8/06 - in tube reactors; the solid particles being arranged in tubes

Another patents in same IPC classes:

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FIELD: chemical industry; other industries; methods of production of the glued woodwork.

SUBSTANCE: the invention provides, that the multitubular reactor consists of the set of the reaction tubes containing the placed in them catalyst, and the housing supplied with the reaction tubes located inside it, in which the heat-carrier passing in the inter-tubular space is introduced. The reaction tubes are selected from the tubes having the equal nominal outer diameter and the wall thickness. The tolerance of the outer diameter is selected from ±0.62 % and the tolerance of the wall thickness - from ±19 % up to -0 %. The tolerance of the outer diameter - from ±0,56 % and the tolerance of the wall thickness - from ±17 % up to -0 %. The method of the catalytic oxidation in the vapor-phase consists in the usage of the multitubular reactor, circulation of the heat carrier in the reaction tubes inter-tube space and feeding of the source gas into the reaction tubes filled with the catalyst, for production of the gaseous product of the reaction, including the determination of the performance specification on the catalyst packing into the reactionary tubes. The multitubular reactor additionally includes the deflectors connected with the reaction tubes through the positions of the joints, for the change of the directions of the passage of the heat-carrier medium introduced into the housing. It is possible to use the heat-exchange reactor with the immovable layer of the catalytic agent additionally containing the set of the reaction tubes, in the inter-tube space of which the heat carrier is passing. The specification is determined by means of provision in one of the reaction tube of at least two catalytic layers with the different specifications of packaging of the catalyst and the change of the lengths of the reaction zones of the reaction tube for relocation of the places of the maximal temperatures of the catalytic layer along the reaction tube or formation of the layer containing the thinning agent in the reaction tube disposed in the places of the joints for determination of the specification on the catalyst packaging to provide the control of the reaction temperature in the places of joints. The version of realization the method of the catalytic oxidation use oxidation of propylene, propane or isobutylene and-or (metha) acrolein by the catalytic oxidation in the vapor phase with the help of the gas containing the molecular oxygen, for production of the (metha)acrolein and-or the(metha)acrylic acid including the packaging of the Mo-Bi catalyst and-or Sb-Mo catalyst in the reaction tubes so, that activity is increasing from the inlet of the process gas into the reaction tubes up to the outlet of the process gas from the reaction tubes and ensures the possibility for the heat-transfer medium and the process gas to pass through as the counter current. The multitubular reactor used in the method contains: the cylindrical housing, the set of the annular tubes, the circulation device, the set of the reaction tubes limited by the set of the of tube plates of the reactor and containing the catalyst, and the set of the deflectors. According to the method of the start-up of the shell-and-tube reactor having the circulating system of the heat-exchange medium, which is the solid substance at the room temperature, the heating of reaction tubes takes place by introduction of the gas with the temperature from 100 up to 400°С into the inter-tube space of the reaction tubes and circulation of the heated heat carrier. The shell-and-tube reactor has the reaction tubes and the inlet and the outlet for the liquid passing in the inter-tube space of the reaction tubes for withdrawal of the heat formed inside the reaction tubes. Due to the method of the catalytic oxidation the invention ensures prevention of formation of the local overheating and the clogging of the reaction tubes, the increased outlet of the gaseous product of the reaction and the increased service life of the catalyst and also the stable operation of the multi-tube reactor for the long time.

EFFECT: the invention ensures prevention of formation of the local overheating and the clogging of the reaction tubes, the increased outlet of the gaseous product of the reaction and the increased service life of the catalyst and also the stable operation of the multi-tube reactor for the long time.

17 cl, 14 dwg

The text descriptions are given in facsimile form.

1. Novotrubny reactor that includes many of the reaction tubes containing the filled catalyst, and the casing is supplied inside the reaction tubes, in which is held in the annular space of the coolant, while the reaction tube is selected from the pipes that have the same nominal outside diameter and the same nominal wall thickness, the tolerance of the outer diameter is from ±0,62% and the tolerance of the wall thickness from ±19 to -0%.

2. Novotrubny reactor according to claim 1, which ensures obtaining (meth)acrolein and/or (meth)acrylic acid by oxidation of propylene, propane, isobutylene, Isobutanol or tert-butanol gas containing molecular oxygen.

3. Novotrubny reactor that includes many of the reaction tubes containing the filled catalyst, and the casing is supplied inside the reaction tubes, in which is held in the annular space of the coolant, while the reactionary labor is s selected from the pipes, having the same nominal outside diameter and the same nominal wall thickness, the tolerance of the outer diameter is from ±0,56% and the tolerance of the wall thickness from ±17 to -0%.

4. Novotrubny reactor according to claim 3, which provides obtaining (meth)acrolein and/or (meth)acrylic acid by oxidation of propylene, propane, isobutylene, Isobutanol or tert-butanol gas containing molecular oxygen.

5. Method of catalytic oxidation in the vapor phase, including the use of novotrubnogo reactor according to claim 1 or 3 which further includes a deflector connected to the reaction tube through the junction, for changing the direction of passage of the fluid introduced into the casing, the circulation of coolant in the annular space of the reaction pipe and supply the source gas into the reaction tubes filled with catalyst, to obtain a gaseous reaction product, including the definition of technical specifications of the packing of the catalyst in the reaction tubes by providing in a single reaction tube at least two catalytic layers with different specifications of the packing of the catalyst and of a length change of the reaction zones of the reaction tube to move seats the maximum temperature catalytic layer along the reaction tube, or forming the layer containing the diluent reaktsionnoi pipe, located at the joints to determine the technical specifications of the packing of the catalyst to control the heat of reaction in the joints.

6. Method of catalytic oxidation in the vapor phase according to claim 5, in which position to determine the technical specifications of the packing of the catalyst include the type of catalyst, amount of catalyst, the shape of the catalyst, the method of dilution of the catalyst and the length of the reaction zones.

7. Method of catalytic oxidation in the vapor phase according to claim 5, comprising the gasket reaction tubes Mo-Bi catalyst and/or Sb-Mo catalyst so that the activity increases from the inlet process gas in the reaction tube to the exit process gas from the reaction tube, enabling the fluid and process gas to pass countercurrent and oxidation of propylene, propane or isobutylene and/or (meth)acrolein catalytic oxidation in the vapor phase with a gas containing molecular oxygen.

8. Method of catalytic oxidation in the vapor phase according to claim 5 or 7, comprising heating the reaction tube by introducing into the tube space of the reaction pipe gas having a temperature of from 100 to 400°and the circulation of the heat carrier which is solid at room temperature, in the annular space of the reaction pipe to start megatr the service of the reactor.

9. Method of catalytic oxidation in the vapor phase, including the use of novotrubnogo heat exchange reactor with a fixed catalyst bed containing many reaction tubes and baffles are connected to the reaction tube through the junction, for changing the direction of passage of the fluid flowing in the annular space of the reaction pipe, the circulation of coolant in the annular space of the reaction pipe, the supply of the source gas in the reaction tubes filled with catalyst, to obtain a gaseous reaction product, including the definition of technical specifications of the packing of the catalyst in the reaction tubes.

10. Method of catalytic oxidation in the vapor phase according to claim 9, in which layers with different specifications of the packing of the catalyst include two or more catalyst in one reaction tube.

11. Method of catalytic oxidation in the vapor phase according to claim 9, in which position to determine the technical specifications of the packing of the catalyst include the type of catalyst, amount of catalyst, the shape of the catalyst, the method of dilution of the catalyst and the length of the reaction zones.

12. Method of catalytic oxidation in the vapor phase according to claim 10, in which position to determine the technical specifications of the packing of the catalyst include a catalyst type, the number is utilizator, the shape of the catalyst, the method of dilution of the catalyst and the length of the reaction zones.

13. Method of catalytic oxidation in the vapor phase according to claim 11 or 12, further comprising the oxidation of propane, propylene and/or isobutylene with molecular oxygen to produce (meth)acrylic acid.

14. Method of catalytic oxidation in the vapor phase, including the use of novotrubnogo reactor, which comprises a cylindrical casing having an aperture of input raw material and the hole in the unloading of products, many ring-shaped tubes arranged on the outer periphery of the cylindrical casing, coolant to enter into the cylindrical casing or discharge of fluid therefrom, the circulation device that connects multiple annular tubes with each other, many reaction tubes limited by many tube grates reactor containing the catalyst, and plenty of vents placed in the longitudinal direction of the reactor, for changing the direction of passage of the coolant introduced into the cylindrical casing, the oxidation of propylene, propane or isobutylene and/or (meth)acrolein catalytic oxidation in the vapor phase through a gas containing molecular oxygen, to obtain a (meth)acrolein and/or (meth)acrylic acid, comprising the gasket Mo-Bi catalyst and/or Sb-Mo catalyst in reactio the main pipe so that that activity increases from the inlet process gas in the reaction tube to the exit process gas from the reaction tube, and enabling the fluid and process gas to pass counter-current.

15. Method of catalytic oxidation in the vapor phase through 14, in which the Mo-Bi catalyst represented by following General formula (I) and Sb-Mo catalyst represented by following General formula (II)

(where Mo represents molybdenum; W is tungsten; Bi represents bismuth; Fe represents iron; And represents at least one element selected from Nickel and cobalt; In represents at least one element selected from the group comprising sodium, potassium, rubidium, cesium and thallium; C is at least one element selected from alkaline-earth metals; D represents at least one element selected from the group comprising phosphorus, tellurium, antimony, tin, cerium, lead, niobium, manganese, arsenic, boron and zinc; E represents at least one element selected from the group comprising silicon, aluminum, titanium and zirconium; O represents oxygen; a, b, C, d, e, f, g, i and j represent the atomic relations of Mo, W, Bi, Fe, a, b, C, D, E, and O respectively; and e is if a=12, 0≤b≤10, 0<C≤10, 0<d≤10, 2≤e≤15, 0<f≤10, 0≤g≤10, 0≤h≤4 and 0≤i≤30; and j represents a value determined of oxidation States of elements present); and

(where Sb represents antimony; Mo represents molybdenum; V is vanadium; Nb represents niobium; X represents at least one element selected from the group comprising iron (Fe), cobalt (Co), Nickel (Ni) and bismuth (Bi); Y represents at least one element selected from copper (Cu) and tungsten (W); Si represents silicon; O represents oxygen; (V/Nb) represents V and/or Nb; k, l, m, n, p, q and r are atomic relations Sb, Mo, (V/Nb), X, Y, Si and O, respectively; and 1≤k≤100, 1≤l≤100, 0,1≤m≤50, 1≤n≤100, 0,1≤R≤50, 1≤q≤100; and r is a value determined from oxidation States of the respective elements).

16. The way you start shell-and-tube reactor having a circulation system of the heat carrier which is solid at room temperature, and shell-and-tube reactor has a reaction tube and the insertion and opening of the discharge fluid flowing in the annular space of the reaction pipe to exhaust heat generated inside the reaction the pipe, includes heating the reaction tubes through the introduction of a gas with a temperature of 100 to 400°in the annular space of the reaction pipe and the circulation of heated fluid into the annular space of the reaction pipe.

17. The method according to item 16, wherein the heat carrier which is solid at room temperature, has a solidification point in the range from 50 to 250°C.

Priorities for items:

09.04.2002 according to claims 1-8;

11.01.2002 at p-13;

14.02.2002 on PP,15;

14.03.2002 on PP,17.