WO2018174075A1 - Réacteur à lit fluidisé et procédé de production d'une résine de poly(chlorure de vinyle) chloré - Google Patents

Réacteur à lit fluidisé et procédé de production d'une résine de poly(chlorure de vinyle) chloré Download PDF

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Publication number
WO2018174075A1
WO2018174075A1 PCT/JP2018/011133 JP2018011133W WO2018174075A1 WO 2018174075 A1 WO2018174075 A1 WO 2018174075A1 JP 2018011133 W JP2018011133 W JP 2018011133W WO 2018174075 A1 WO2018174075 A1 WO 2018174075A1
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raw material
gas
solid raw
gas supply
fluidized bed
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PCT/JP2018/011133
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English (en)
Japanese (ja)
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慧 岩上
廣田　淳一
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株式会社カネカ
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Priority to JP2019507699A priority Critical patent/JP7080874B2/ja
Publication of WO2018174075A1 publication Critical patent/WO2018174075A1/fr

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  • the present invention relates to a fluidized bed reactor and a method for producing a chlorinated vinyl chloride resin using the fluidized bed reactor.
  • a chlorinated vinyl chloride resin (hereinafter also referred to as CPVC) obtained by chlorinating vinyl chloride resin (hereinafter also referred to as PVC) is heat resistant without substantially impairing the mechanical and chemical properties of PVC. Is known to improve. Therefore, CPVC is also used for applications such as heat-resistant pipes, heat-resistant joints, heat-resistant valves, and heat-resistant sheets that cannot be used with PVC.
  • Patent Documents 1 and 2 a production method by a gas phase chlorination method is known (for example, Patent Documents 1 and 2).
  • the method for producing CPVC in Patent Document 1 is to put PVC powder in an eggplant-shaped flask, circulate chlorine gas in the eggplant-shaped flask, irradiate the PVC powder with ultraviolet rays, and rotate the eggplant-shaped flask. Let By doing so, the PVC powder reacts with chlorine gas, and CPVC is formed together with hydrochloric acid gas.
  • a reaction vessel having a dispersion mechanism such as a perforated bottom plate is used, and the chlorination reaction is continuously performed by ultraviolet irradiation while keeping the PVC particles in a fluid state by a chlorine stream. .
  • JP 2002-275213 A Japanese Patent Publication No. 52-15638
  • Patent Document 1 In order to industrially produce CPVC, it is necessary to uniformly react a large amount of PVC with chlorine gas. However, the manufacturing method disclosed in Patent Document 1 has a problem that it is difficult to increase the size of the PVC powder because the powder is rotated and mixed. In the chlorination method of Patent Document 2, an experiment was performed using a gas inflow port provided with a filter cloth as a dispersion mechanism, but industrial durability cannot be expected.
  • a reactor 501 of the prototype reaction apparatus 500 includes a gas dispersion plate 505 having a gas supply hole 503, a generator 506 for irradiating ultraviolet rays, and a heat transfer tube 507 in a housing 502.
  • the PVC powder 510 as a raw material is introduced into the casing 502, the PVC powder 510 is placed on the gas dispersion plate 505, and chlorine gas is supplied from each gas supply hole 503 to the PVC powder 510. This was performed by irradiating ultraviolet rays from the generator 506 while forming a fluidized bed by spraying.
  • the inventor stirs the CPVC and the PVC powder 510 generated in the vicinity of the ultraviolet generator 506 by the injected chlorine gas, and the CPVC and the unreacted PVC powder 510 are replaced. It was considered that the reaction PVC powder 510 could be reacted efficiently and mass production was possible.
  • the PVC powder 510 when the PVC powder 510 is irradiated with ultraviolet light to cause a photoreaction, CPVC is generated by an exothermic reaction, and the reaction field is within the ultraviolet irradiation range. Therefore, in order to advance the CPVC reaction and improve the CPVC reaction efficiency, it is necessary to irradiate the PVC powder 510 flowing in the housing 502 with ultraviolet rays while removing the reaction heat generated by the reaction. Therefore, in the prototype reactor 500, the generator 506 and the heat transfer tube 507 are arranged close to each other, and the temperature in the vicinity of the generator 506 is adjusted. By doing so, the reaction efficiency of the PVC powder 510 was improved.
  • the prototype reactor 500 has not been able to efficiently generate CPVC having quality above a certain level.
  • the present invention has an object to provide a fluidized bed reactor capable of efficiently mixing solid raw materials and efficiently producing a reaction product of a certain level or more and a method for producing a chlorinated vinyl chloride resin as compared with the prior art.
  • the present inventors diligently examined the results of the above-mentioned trial manufacture, and paid attention to the distance between the generator that generates ultraviolet rays and the heat transfer tube for cooling, and examined the distance between the generator and the heat transfer tube.
  • the distance between the generator and the heat transfer tube is closer than a certain distance, the presence of the heat transfer tube becomes a steric hindrance near the generator, and the generated CPVC and the raw material PVC powder are not sufficiently stirred, and the raw material PVC. It was discovered that the powder was less likely to flow near the generator. It was also discovered that if the distance between the generator and the heat transfer tube is longer than a certain distance, the heat generated in the vicinity of the generator cannot be sufficiently cooled by the heat transfer tube and the quality deteriorates.
  • One aspect of the present invention derived from this discovery has a reactor filled with a powdery or granular solid raw material, gas is supplied to the reactor filled with the solid raw material, A fluidized bed reaction apparatus for obtaining a reaction product by reacting the solid raw material with the gas while fluidizing the solid raw material with a gas, comprising a light emitting member and a temperature adjusting member, wherein the light emitting member comprises the reactor A light-emitting side rod-shaped portion that is disposed inside and irradiates the solid raw material with light, and the temperature adjustment member has an adjustment-side rod-shaped portion that is disposed in the reactor and adjusts the temperature of the solid raw material,
  • the shortest distance between the outer peripheral surface of the light emitting side rod-shaped portion and the outer peripheral surface of the adjustment side rod-shaped portion closest to the light emitting side rod-shaped portion is 1.9 cm to 15 cm.
  • “closest” means a relationship in which the shortest distance is closest.
  • the “state filled with the solid raw material” here includes not only a state where the reactor is completely filled with the solid raw material but also a state where a part of the reactor is filled with the solid raw material.
  • the temperature adjusting member has a plurality of adjusting side bar-like parts arranged in the reactor to adjust the temperature of the solid raw material, and the shortest distance between the outer peripheral surfaces of the two closest adjusting side bar-like parts is 1.9 cm or more and 15 cm or less.
  • a more preferable aspect is that one of the two adjustment-side rod-like portions is closest to the light-emitting side rod-like portion among the plurality of adjustment-side rod-like portions.
  • a preferred aspect has a gas dispersion part having a plurality of gas supply holes for injecting the gas into the reactor, and at least one of the plurality of gas supply holes includes the light emitting member and the gas supply hole. It is separated from the temperature control member, and the gas dispersion part is placed when the solid material is loaded when the solid material is filled.
  • a more preferred aspect is that the gas injection direction of the gas supply hole intersects with a direction orthogonal to the longitudinal direction of the light emitting side rod-shaped portion or the adjustment side rod-shaped portion.
  • the light-emitting side rod-shaped part has a light source part and a surrounding part surrounding an outer periphery of the light source part, and the surrounding part transmits light from the light source part, and the light source part And the surrounding portion constitutes an outer peripheral surface of the light emitting side rod-shaped portion.
  • the adjustment-side rod-like portion is a hollow body, and a temperature-adjusting liquid or gas is allowed to pass through to adjust the temperature of the solid raw material.
  • a preferred aspect is that the light emitting side bar-like portion is arranged at a position away from the inner wall of the reactor when viewed from the longitudinal direction of the light emitting side bar-like portion.
  • the temperature adjusting member includes a plurality of adjusting side bar-like portions arranged in the reactor to adjust the temperature of the solid raw material, has at least two adjusting side bar-like groups, and the two adjusting side members
  • the rod-shaped group has an adjustment-side rod-like row in which two or more of the adjustment-side rod-like portions are arranged in a straight line at intervals, and the light-emitting side rod-like portion can irradiate light in at least two directions
  • the light emission side bar-shaped portion is disposed between the adjustment side bar-shaped rows of the two adjustment side bar-shaped groups, and can emit light toward the adjustment side bar-shaped row side of the two adjustment side bar-shaped groups. is there.
  • a more preferable aspect is that, when the temperature adjusting member is viewed in plan, the adjusting side bar-shaped portion in the adjusting side bar-shaped group is arranged at the apex position of the regular plane filling type.
  • the “regular plane filling form” here is a regular polygon structure that can fill a plane with one type of figure, and for example, a plane filling form consisting of any one of a regular triangle, a square, and a regular hexagon.
  • the “planar filling type” here means a shape when a plane is filled with a figure without a gap.
  • a preferred aspect includes a plurality of unit units each including a gas dispersion part, the light emitting member, and the temperature adjustment member, and the gas dispersion part is configured to place the solid raw material, Is provided with a gas supply hole for injecting the gas into the reactor, and the unit units are arranged in a plane and spread in parallel.
  • the present inventor also prototyped a reactor 600 as shown in FIG. 32 in order to industrially produce CPVC. That is, the prototype reaction apparatus 600 is provided with a metal plate 602 made of Hastelloy C22 provided with a number of gas supply holes 605 and a generator (not shown) for irradiating ultraviolet rays in a reaction vessel 601. .
  • the CPVC is manufactured by placing the PVC powder 610 on the metal plate 602, injecting chlorine gas from each gas supply hole 605 to the PVC powder 610, and irradiating with ultraviolet rays while forming a fluidized bed. went. By carrying out like this, PVC and chlorine gas were made to react uniformly with the prototype reactor 600, and it was tried to mass-produce CPVC.
  • Hastelloy C22 is a corrosion-resistant alloy and is supposed to have resistance to acidic gas.
  • the metal plate 602 made of Hastelloy C22 was corroded by chlorine gas or hydrochloric acid gas. Therefore, even if it was made of Hastelloy C22, there was a problem that the metal plate 602 could not be used for a long time.
  • a preferable aspect for making the fluidized bed reactor capable of suppressing the fall of the solid raw material from the gas supply hole is that the reactor includes a gas dispersion member and a solid raw material filling unit, and the solid raw material Is filled in the solid raw material filling part in a state of being in contact with the upper surface of the gas dispersion member, the gas is supplied to the solid raw material filling part via the gas dispersion member, and the gas in the solid raw material filling part is supplied by the gas.
  • the solid raw material and the gas are reacted while fluidizing the solid raw material to obtain a reaction product
  • the gas dispersion member is a plate-like body having resistance to the gas
  • the gas dispersion member includes a plurality of gas dispersion members.
  • the first gas supply hole has an opening on the solid raw material filling part side that opens upward, has a non-vertical part having at least a horizontal component, and further includes the following: ( ) Is a fluidized bed reactor according to any one of claims 1 to 11, wherein the condition is satisfied or (2). (1)
  • the non-vertical portion is horizontal or inclined at an inclination angle of less than 45 degrees with respect to a horizontal plane.
  • the circumscribed diameter of the opening on the solid raw material filling part side is less than 10 times the median diameter of the solid raw material.
  • “With gas resistance” as used herein means changes in mass, dimensions, appearance, and physical properties (mechanical properties, electrical properties, thermal properties, optical properties, etc.) when a reaction product is produced. Substantially does not occur, and deterioration that affects the quality of the reaction product produced does not occur.
  • the first gas supply hole is an inclined hole that extends linearly and penetrates the gas dispersion member obliquely.
  • a preferable aspect is that most of the opening of the first gas supply hole on the solid raw material filling portion side overlaps with an inner wall surface constituting the first gas supply hole when viewed in plan.
  • a preferable aspect is that the non-vertical portion is inclined with respect to a horizontal plane, and the inclination angle of the non-vertical portion is smaller than the angle of repose of the solid raw material according to ISO902: 1976.
  • a preferred aspect is that the circumscribed diameter of the first gas supply hole is not less than 5 times and not more than 20 times the median diameter of the solid raw material.
  • a preferred aspect is that the first gas supply holes have at least three, and the intervals between the first gas supply holes in the three first gas supply holes are all equal.
  • a preferred aspect is that the first gas supply hole has a circular opening shape on the side of the solid material filling portion.
  • the solid raw material filling portion has an inner wall portion that rises with respect to the gas dispersion member, and there is a discharge port that can be opened and closed on the inner wall portion, and the non-vertical portion is the first gas supply hole.
  • One aspect of the present invention includes a reactor having a gas dispersion member and a solid material filling portion, and the solid material filling portion is in a state where a powdery or granular solid material is in contact with the upper surface of the gas dispersion member. Gas is supplied to the solid raw material filling part through the gas dispersion member, and the solid raw material and the gas are reacted while fluidizing the solid raw material in the solid raw material filling part by the gas, thereby producing a reaction product.
  • the gas dispersion member is a plate-like body having resistance to the gas, the gas dispersion member has a plurality of first gas supply holes, and the first gas supply
  • the hole is characterized in that the opening on the solid raw material filling part side opens upward, has a non-vertical part having at least a horizontal component, and further satisfies the following condition (1) or (2): It is a fluidized bed reactor. (1) The non-vertical portion is horizontal or inclined at an inclination angle of less than 45 degrees with respect to a horizontal plane. (2) The circumscribed diameter of the opening on the solid raw material filling part side is less than 10 times the median diameter of the solid raw material.
  • One aspect of the present invention includes a reactor having a gas dispersion member and a solid material filling portion, and the solid material filling portion is in a state where a powdery or granular solid material is in contact with the upper surface of the gas dispersion member.
  • Gas is injected from the gas dispersion member to the solid raw material filling part, and the solid raw material and the gas are reacted while fluidizing the solid raw material in the solid raw material filling part by the gas to obtain a reaction product
  • the solid raw material filling portion includes an inner wall portion that rises with respect to the gas dispersion member, and a guide wall portion that faces the gas dispersion member with a predetermined interval therebetween.
  • the guiding wall portion is a fluidized bed reaction apparatus that blocks the gas injected from the gas dispersion member and guides the gas along at least the inner wall portion.
  • One aspect of the present invention includes a reactor having a gas dispersion member and a solid material filling portion, and the solid material filling portion is in a state where a powdery or granular solid material is in contact with the upper surface of the gas dispersion member.
  • Gas is injected from the gas dispersion member to the solid raw material filling part, and the solid raw material and the gas are reacted while fluidizing the solid raw material in the solid raw material filling part by the gas to obtain a reaction product
  • the solid raw material filling part includes a first inner wall part that rises with respect to the gas dispersion member, and a second inner wall part that is continuous with a step through the first inner wall part and the guide wall part.
  • the guide wall portion is opposed to the gas dispersion member at a predetermined interval in the vertical direction, and the guide wall portion blocks at least the gas injected from the gas dispersion member.
  • On the second inner wall A fluidized bed reactor for guiding the gas to Migihitsuji.
  • One aspect of the present invention includes a reactor having a gas dispersion member and a solid material filling portion, and the solid material filling portion is in a state where a powdery or granular solid material is in contact with the upper surface of the gas dispersion member.
  • a fluidized bed reaction apparatus comprising a guide wall facing the gas dispersion member at a predetermined interval, the gas dispersion member having a first gas supply hole, and the first gas supply
  • the hole has a non-vertical part having at least a horizontal component, and the non-vertical part constitutes an opening on the solid material filling part side of the first gas supply hole, and the non-vertical part is the guide wall part In a fluidized bed reactor extending towards That.
  • One aspect of the present invention includes a reactor having a gas dispersion member and a solid material filling portion, and the solid material filling portion is in a state where a powdery or granular solid material is in contact with the upper surface of the gas dispersion member.
  • a fluidized bed reaction apparatus comprising a light emitting member and a temperature adjusting member, wherein the light emitting member has a light emitting side rod-like portion arranged in the solid raw material filling portion for irradiating light to the solid raw material, and the temperature adjusting The member has an adjustment-side rod-like portion that is arranged in the solid raw material filling portion and adjusts the temperature of the solid raw material, and the solid raw material filling portion is in a middle portion in the vertical direction as compared with the portion on the gas dispersion member side. There is a narrowed part The temperature adjusting member and the light emitting side rod-shaped portion to the narrowed portion is a fluidized bed reactor is located.
  • One aspect of the present invention includes a reactor having a gas dispersion member and a solid material filling portion, and the solid material filling portion is in a state where a powdery or granular solid material is in contact with the upper surface of the gas dispersion member.
  • Gas is supplied to the solid raw material filling part through the gas dispersion member, and the solid raw material and the gas are reacted while fluidizing the solid raw material in the solid raw material filling part by the gas, thereby producing a reaction product.
  • the solid raw material filling portion has an inner wall portion that rises with respect to the gas dispersion member, and there is a discharge outlet that can be opened and closed on the inner wall portion.
  • a plurality of first gas supply holes wherein the first gas supply hole has a non-vertical portion having at least a horizontal component, and the non-vertical portion is on a solid material filling portion side of the first gas supply hole;
  • the non-opening Straight section is a fluidized bed reactor which extends toward the dispensing port side.
  • One aspect of the present invention is a method for producing a chlorinated vinyl chloride resin using the fluidized bed reactor described above, wherein the reactor is filled with the vinyl chloride resin. And a method for producing a chlorinated vinyl chloride resin in which chlorine gas is supplied to the reactor to react the vinyl chloride resin with chlorine gas.
  • vinyl chloride resin refers to not only a vinyl chloride resin but also a resin in which only a part of the vinyl chloride resin is substituted with other substituents while maintaining the skeleton structure of the vinyl chloride resin. Copolymers with other monomers are also included.
  • chlorinated vinyl chloride resin as used herein means that not only the chlorinated vinyl chloride resin but also the basic skeleton structure of the chlorinated vinyl chloride resin is maintained, and only a part thereof is substituted with other substituents. Also includes products and copolymers.
  • One aspect of the present invention is a method for producing a chlorinated vinyl chloride resin in which a vinyl chloride resin is produced using the fluidized bed reactor described above, wherein the particle diameter is larger than the outer diameter of the first gas supply hole.
  • a powder or granular vinyl chloride resin having a small diameter is filled in the solid raw material filling portion, and chlorine gas is supplied to the solid raw material filling portion through the gas dispersion member to react the vinyl chloride resin and chlorine gas.
  • This is a method for producing a chlorinated vinyl chloride resin formed.
  • solid raw materials can be mixed more efficiently than before, and a reaction product of a certain level or more can be produced efficiently.
  • FIG. 3 is a vertical sectional view of the reactor of FIG. 2, and (a) and (b) are seen from different directions. It is the horizontal direction sectional view which looked at the reactor of FIG. 2 from the gas dispersion member side. It is a cross-sectional perspective view of the principal part of the reactor of FIG.
  • FIGS. 3A and 3B are explanatory views of the gas dispersion member of FIG. 2, in which FIG. 2A is a perspective view of the gas dispersion member, and FIG.
  • 1 is a perspective view conceptually showing Example 1 of the present invention. It is explanatory drawing of the measurement point of the mixing degree measurement test of Example 1, 2, Comparative example 1, and Reference example 1, (a) when each measurement point is planarly viewed, (b) is a cross section of each measurement point. It is a figure at the time of seeing.
  • FIG. It is a graph which shows the result of the mixing degree measurement test of Example 1, 2, the comparative example 1, and the reference example 1.
  • FIG. It is explanatory drawing which shows typically the reactor of the reactor which this inventor made as an experiment, (a) is a perspective view, (b) is sectional drawing. It is explanatory drawing of the reactor which this inventor made as an experiment, (a) is a perspective view, (b) is sectional drawing.
  • the fluidized bed reactor 1 (hereinafter also simply referred to as the reactor 1) of the first embodiment of the present invention is a chemistry that causes a chemical reaction between the source gas and the solid source 100 while stirring the solid source 100 with the source gas. It is a reactor.
  • the reaction apparatus 1 is an apparatus for producing a chlorinated vinyl chloride resin (hereinafter also simply referred to as CPVC).
  • CPVC chlorinated vinyl chloride resin
  • the reactor 1 reacts while stirring a vinyl chloride resin (hereinafter simply referred to as PVC) as a solid raw material 100 with chlorine gas as a raw material gas, to obtain CPVC as a reaction product and hydrochloric acid gas as a reaction product gas. is there.
  • the reactor 1 includes a circulation circuit 7 including a reactor 2, a deaeration device 3, a deaeration path 5, and a supply path 6 as main components.
  • the reactor 1 of the embodiment has a main feature in the reactor 2.
  • the reactor 2 is a reaction tank that actually generates a chemical reaction using the solid raw material 100 as a reaction product. As shown in FIGS. 1 and 2, the reactor 2 includes a light emitting member 11, a temperature adjusting member 12, and a gas dispersion member 15 in a housing 10.
  • the casing 10 has a vertically long rectangular parallelepiped shape, and includes a top surface side wall portion 40, side wall portions 41 to 44, and a bottom surface side wall portion 45, and is surrounded by these wall portions 40 to 45.
  • a Go space 50 is provided.
  • the casing 10 is mainly composed of a solid material filling unit 51 (hereinafter also simply referred to as a filling unit 51) and a gas supply unit 52 in the vertical direction.
  • the side wall portions 41 to 44 are composed of filling side wall portions 141 to 144 belonging to the filling portion 51 and supply side wall portions 161 to 164 belonging to the gas supply portion 52.
  • the light emitting member 11 is a device that applies light energy to the solid material 100.
  • the light emitting member 11 is an ultraviolet irradiation device that generates ultraviolet rays and irradiates the solid material 100 with ultraviolet rays.
  • the light emitting member 11 extends in a bar shape in the vertical direction (height direction, vertical direction, vertical direction), and the outer shape of the cross section orthogonal to the extending direction is circular.
  • the “outer shape” refers to the contour shape that forms the contour, and refers to the shape of the outer surface that forms the outer shape.
  • the light emitting member 11 includes a light source side 20 and a light emitting side rod-like portion 22 constituted by an encircling portion 21 surrounding the outer periphery of the light source portion 20.
  • the light source unit 20 functions as a light source for irradiating ultraviolet light, and is a part extending in a bar shape in the vertical direction.
  • the light source unit 20 has a cylindrical shape, and the LEDs 23 are scattered on the side surfaces thereof.
  • the light source unit 20 is capable of irradiating ultraviolet rays in the radial direction, and is preferably capable of irradiating ultraviolet rays in at least two directions when viewed in plan.
  • the light source of the light source unit 20 is not limited to the LED 23.
  • the light source of the light source unit 20 may be another light source such as a high pressure mercury lamp.
  • the light source of the light source unit 20 may be not only a point light source such as the LED 23 but also a surface light source such as an organic EL or an inorganic EL.
  • the surrounding part 21 is a protective member having translucency, transmits the ultraviolet rays irradiated from the light source part 20, can disperse the ultraviolet rays substantially uniformly, and can be taken out to the outside (solid material 100 side). It has become.
  • the surrounding portion 21 is a cylindrical hollow body, and the light source portion 20 is inserted therein.
  • a gap 25 is formed between the outer peripheral surface of the light source unit 20 and the inner peripheral surface of the surrounding portion 21.
  • the gap 25 may be a gap, or the gap 25 may be filled with a light-transmitting medium such as gas or liquid other than air.
  • the temperature adjustment member 12 is a temperature adjustment device that can adjust the inside of the housing 10 to a predetermined temperature and maintain the inside of the housing 10 at a constant temperature.
  • the temperature adjusting member 12 of the present embodiment is an air-cooled or water-cooled cooling device that suppresses a temperature rise caused by reaction heat between the solid raw material 100 and the raw material gas.
  • the temperature adjustment member 12 is mainly composed of heat transfer tubes and has a lattice shape.
  • the temperature adjustment member 12 includes an outflow portion 30, an inflow portion 31, and an adjustment-side bar group 32 that connects the outflow portion 30 and the inflow portion 31.
  • the inflow part 31 is a part for allowing a cooling gas or a cooling liquid (cooling medium) to flow into the adjustment-side rod group 32 from the outside.
  • the outflow part 30 is a part which flows out the cooling gas or the cooling liquid heat-exchanged by the adjustment side rod-shaped group 32 to the outside.
  • the adjustment-side rod-shaped group 32 includes one or more adjustment-side rod-like rows 33 in which a plurality of adjustment-side rod-like portions 35 are arranged in a straight line at intervals.
  • the adjustment-side rod-shaped portion 35 is a cylindrical body that connects the outflow portion 30 and the inflow portion 31 and extends in a bar shape in the vertical direction.
  • the adjustment side rod-shaped portion 35 of the present embodiment is a cylindrical hollow body. The inside can pass cooling gas or cooling liquid.
  • the adjustment-side rod-like portions 35 belonging to one adjustment-side rod-like row 33 are parallel to each other.
  • the shortest distance D2 between the side surfaces of the two adjustment-side rod-like portions 35, 35 closest to the vertical direction Y shown in FIG. 4 is preferably 1.9 cm or more, and more preferably 2.0 cm or more.
  • the shortest distance D2 is preferably 15 cm or less, more preferably 10 cm or less, and particularly preferably 5 cm or less. If it is these ranges, the flow of the solid raw material 100 will be hard to be inhibited by the adjustment
  • the adjustment-side bar-like group 32 includes two or more adjustment-side bar-like rows 33 in the lateral direction X, and the adjustment-side rod-like portion 35 constitutes the apex of the regular plane filling type. Therefore, the temperature distribution of the solid raw material 100 can be reduced.
  • the adjustment-side bar-shaped group 32 of the present embodiment the adjustment-side bar-shaped portions 35 are arranged at the apex positions of the squares.
  • the shortest distance D3 between the side surfaces of the adjustment-side rod-like portions 35, 35 of the two rows of adjustment-side rod-like rows 33, 33 closest to the horizontal direction X is the side surface of the two adjustment-side rod-like portions 35, 35 closest to the vertical direction Y.
  • the shortest distance D3 is preferably 1.9 cm or more, and more preferably 2.0 cm or more.
  • the shortest distance D3 is preferably 15 cm or less, more preferably 10 cm or less, and particularly preferably 5 cm or less.
  • the gas dispersion member 15 is a plate-like body that is provided in the housing 10 in a horizontal posture and partitions the surrounding space 50 of the housing 10 into the filling unit 51 side and the gas supply unit 52 side. As shown in FIG. 6, the gas dispersion member 15 includes a main body plate portion 55 and a plurality of gas supply holes 56.
  • the main body plate portion 55 is a quadrangular plate body, and connects the intermediate portions in the vertical direction (vertical direction) of the side wall portions 41 to 44 of the housing 10 as shown in FIG. It is a part.
  • the “intermediate portion” refers to a portion other than the end portion in one direction and between the end portions.
  • the main body plate portion 55 is made of resin and is a plate-like body having resistance to the source gas and the reaction product gas. Therefore, even in an acidic atmosphere, corrosion like a metal plate hardly occurs, stable equipment operation is possible, and the same gas dispersion member 15 can be used over a long period of time.
  • the material of the main body plate portion 55 is not particularly limited as long as it has resistance to the source gas and the reaction product gas.
  • the main body plate portion 55 can be made of, for example, a fluororesin typified by polytetrafluoroethylene (PTFE), a hard chlorinated vinyl chloride resin, an unsaturated polyester resin, a vinyl ester resin, or the like.
  • the thickness of the main body plate portion 55 is preferably 0.3 cm or more and 10 cm or less, and more preferably 0.5 cm or more and 3 cm or less. If it is this range, while ensuring sufficient intensity
  • the gas supply hole 56 is a hole that allows the filling unit 51 and the gas supply unit 52 to communicate with each other, and is a through hole that penetrates the main body plate portion 55.
  • the opening ratio of the gas supply holes 56 is preferably 0.1% or more and 5% or less. Within this range, it is possible to supply the source gas stably while maintaining the rigidity of the main body plate portion 55.
  • the gas supply hole 56 includes a first gas supply hole 150 (first gas vent hole) and a second gas supply hole 151 (second gas vent hole).
  • the first gas supply hole 150 includes a non-vertical portion 152 having at least a horizontal component, and is a hole having a horizontal component and a vertical component as a whole.
  • the first gas supply hole 150 of the present embodiment is an inclined hole that is configured by only the non-vertical portion 152 and is inclined at a predetermined angle with respect to the horizontal plane. That is, the first gas supply hole 150 is an inclined hole that extends linearly and penetrates the main body plate portion 55 in an oblique direction as shown in FIG. Therefore, formation of the first gas supply hole 150 is easy.
  • the first gas supply hole 150 has a filling side opening 145, which is an opening on the filling part 51 side, opened upward, and the upper part of the filling side opening 145 is not blocked by other portions.
  • the filling side opening 145 of the first gas supply hole 150 overlaps with the inner wall surface constituting the first gas supply hole 150 when the main body plate portion 55 is viewed in plan as shown in FIG. Yes. That is, the center of the filling side opening 145 is shifted from the center of the supply side opening 146 when viewed in plan. It is preferable that 90% or more of the filling side opening 145 overlaps with the inner wall surface constituting the first gas supply hole 150.
  • the filling side opening 145 completely overlaps the inner wall surface constituting the first gas supply hole 150, and the supply side opening 146 that is the opening on the gas supply part 52 side from the filling part 51 side is invisible. It has become. Therefore, the solid raw material 100 can be further prevented from falling from the first gas supply hole 150.
  • the inclination angle ⁇ 1 of the first gas supply hole 150 with respect to the surface (horizontal plane) of the main plate 55 of the first gas supply hole 150 shown in FIG. 6B is ISO902: 1976 (corresponding to JIS R 9301-2-2). Is preferably smaller than the angle of repose of the solid raw material 100, and more preferably smaller than the angle of repose of the solid raw material 100 by 3 degrees or more. If it is this range, it can prevent that the solid raw material 100 falls along the inclined surface of the 1st gas supply hole 150.
  • the inclination angle ⁇ 1 is preferably less than 45 degrees.
  • the solid raw material 100 can suppress that the solid raw material 100 falls to the gas supply part 52 side from the 1st gas supply hole 150 compared with the past, and can stir the solid raw material 100 efficiently. Therefore, the solid raw material 100 can be uniformly reacted with the gas, and a high-quality fluidized bed can be formed.
  • the opening shape of the filling side opening 145 is preferably circular, and the opening shape of the supply side opening 146 is also preferably circular. By setting it as such an opening shape, gas tends to spread
  • FIG. The first gas supply hole 150 of the present embodiment has the same opening shape in the entire depth direction.
  • the inner diameter (the circumscribed diameter, the diameter of the minimum inclusion circle) of the first gas supply hole 150 is preferably 5 times or more, more preferably 7 times or more the median diameter of the solid raw material 100. Further, the inner diameter (the circumscribed diameter, the diameter of the minimum inclusion circle) of the first gas supply hole 150 is preferably not more than 20 times the median diameter of the solid raw material 100, and more preferably less than 10 times. Within these ranges, the number of the first gas supply holes 150 per unit area should be increased while suppressing the falling of the solid raw material 100 toward the gas supply unit 52 and the clogging of the first gas supply holes 150. Can do.
  • the inner diameter of the first gas supply hole 150 of the present embodiment is less than 10 times the median diameter of the solid raw material 100.
  • the solid raw material 100 can be prevented from dropping from the first gas supply hole 150 to the gas supply unit 52 side compared to the conventional case, and the solid raw material 100 can be efficiently stirred. Therefore, a high quality fluidized bed can be formed, and the solid raw material 100 can be reacted with the gas evenly.
  • the second gas supply hole 151 is a vertical hole extending linearly in the vertical direction (vertical direction), and the opening shape is preferably circular.
  • the inner diameter of the second gas supply hole 151 (the circumscribed diameter, the diameter of the smallest inclusion circle) is preferably smaller than the inner diameter of the first gas supply hole 150 (the circumscribed diameter, the diameter of the smallest inclusion circle). More preferably, it is less than 10 times the diameter. If it is this range, the fall of the solid raw material 100 from the 2nd gas supply hole 151 to the gas supply part 52 side can be suppressed.
  • the opening area on the filling part 51 side of the second gas supply hole 151 is preferably smaller than the opening area of the filling side opening 145 of the first gas supply hole 150.
  • the filling unit 51 is a solid material storage unit that can store the solid material 100, and is a housing that is opened downward. As shown in FIG. 3, the filling portion 51 includes a top side wall portion 40 and filling side wall portions 141 to 144 rising from the gas dispersion member 15. As shown in FIG. 3B, one filling-side side wall portion 141 is provided with a payout opening 170 that can be opened and closed by an opening / closing member 171. The discharge outlet 170 is used to discharge the solid raw material 100 and the reaction product to a housing member (not shown), and is an opening that communicates the inside and outside of the filling unit 51.
  • the opening / closing member 171 is a lid that changes its posture between a closed posture and an open posture by a power source (not shown) and opens and closes the payout opening 170. That is, the opening / closing member 171 is a member that is flush with the inner wall surface of the filling side wall portion 141 in the closed posture and closes the discharge outlet 170, and is separated from the filling side wall portion 141 in the open posture to open the discharge outlet 170. It is.
  • the gas supply unit 52 is a casing opened upward, and mainly includes supply side wall portions 161 to 164 and a bottom side wall portion 45 as shown in FIG.
  • the gas dispersion member 15 divides the interior of the housing 10 in the vertical direction and constitutes a boundary between the filling unit 51 and the gas supply unit 52.
  • the axis of the gas supply hole 56 of the gas dispersion member 15 intersects the direction perpendicular to the longitudinal direction of the light emitting side rod-like portion 22 of the light emitting member 11 or the adjustment side rod-like portion 35 of the temperature adjusting member 12.
  • the light emitting member 11 and the temperature adjusting member 12 are partly or wholly arranged in the filling portion 51, located above the gas dispersion member 15, and extend with a height in the vertical direction. Yes.
  • the light emitting side rod-like portion 22 of the light emitting member 11 has a vertical posture extending in the vertical direction, and the surrounding portion 21 surrounds the outside of the light source portion 20.
  • the temperature adjustment member 12 has a horizontal posture in which the outflow portion 30 and the inflow portion 31 extend in the horizontal direction, and an adjustment-side rod-like portion 35 that connects the outflow portion 30 and the inflow portion 31 has a vertical posture in the vertical direction.
  • the light-emitting side rod-like portion 22 is positioned between the adjustment-side rod-like groups 32 and 32 when viewed in plan, and is sandwiched between the adjustment-side rod-like groups 32 and 32.
  • the shortest distance D1 between the outer peripheral surface of the light emitting side bar 22 and the side surface of the adjustment side bar 35 closest to the light emitting side bar 22 shown in FIG. 5 is 1.9 cm or more and 2.0 cm or more. It is preferable.
  • the shortest distance D1 is preferably 15 cm or less, more preferably 10 cm or less, and further preferably 5 cm or less.
  • the solid raw material 100 can fully be mixed, the reaction heat which generate
  • the reaction product can be produced in large quantities.
  • each of the light emitting member 11 and the temperature adjusting member 12 with respect to the gas dispersion member 15 is preferably 1.9 cm or more and 50 cm or less, and more preferably 1.9 cm or more and 20 cm or less.
  • the gas supply hole 56 is not blocked by the light emitting member 11 and the temperature adjusting member 12, and is in the space between the gas dispersing member 15 and the light emitting member 11 and the space between the gas dispersing member 15 and the temperature adjusting member 12. Gas becomes easy to flow. Therefore, a good quality fluidized bed can be formed.
  • the first gas supply holes 150 are evenly arranged so as to be closest packed when viewed in plan, and the distance between the first gas supply holes 150 and 150 is equal. It has become. That is, the first gas supply holes 150 are evenly arranged so as to constitute the apex of the regular plane filling type.
  • the distance D11 between the first gas supply hole 150b adjacent to one first gas supply hole 150a shown in FIG. 8 is the distance D12 between the first gas supply hole 150a adjacent to the other first gas supply hole 150c. Is equal to The distance D11 is also equal to the distance D13 between the first gas supply hole 150b and another adjacent first gas supply hole 150c.
  • the first gas supply holes 150 are uniformly arranged.
  • the first gas supply holes 150 gather on the center side to form a first gas supply hole group.
  • the second gas supply hole 151 is disposed so as to surround at least a part or all of the periphery of the first gas supply hole group.
  • the second gas supply hole 151 is arranged in the vicinity of one filling side wall portion that is the inner wall of the filling portion 51 along the edge of the main body plate portion 55.
  • the distance between the adjacent second gas supply holes 151 and 151 is equal. That is, the second gas supply hole 151 is disposed closer to the one filling side side wall than the first gas supply hole 150 and is arranged along the one filling side side wall. For example, as shown in FIG.
  • the second gas supply hole 151 is disposed at least in the vicinity of the filling side wall 143 opposite to the filling side wall 141.
  • the second gas supply hole 151 is provided at least in a portion where the opening density (opening area per unit area) of the first gas supply hole 150 is small when the gas dispersion member 15 is viewed from the filling part 51 side. It has been.
  • the second gas supply holes 151 are provided along all four filling side wall portions 141 to 144 as shown in FIG.
  • the discharge outlet 170 is disposed at a position slightly higher than the gas dispersion member 15 as shown in FIG. In this case, a damming portion is formed by this step, and when cleaning the inside of the housing 10, the cleaning liquid is dammed and is difficult to leak outside, and the inside of the housing 10 is easy to clean.
  • the non-vertical portion 152 of the first gas supply hole 150 faces the discharge outlet 170 side as shown in FIG. 3B and opens toward the filling side wall portion 141 where the discharge outlet 170 is provided.
  • the degassing device 3 is a device that degass the reaction product gas from the mixed gas of the material gas and the reaction product gas, and extracts the material gas.
  • the degassing path 5 is a forward flow path that connects the degassing device 3 from the reactor 2 and the mixed gas or the like goes to the degassing device 3.
  • a trap device 60 is provided in the middle flow direction of the raw material gas, a first path 61 that connects the reactor 2 and the trap apparatus 60, and a second path 62 that connects the trap apparatus 60 and the degassing apparatus 3. It has.
  • the trap device 60 is a separation device that separates the mixed gas of the raw material gas and the reaction product gas from the scattered solid raw material 100.
  • the trap device 60 is formed separately from the first path 61, and a return path 63 connected to the reactor 2 is connected to the bottom. Therefore, the trap device 60 can send the mixed gas from the second path 62 to the degassing device 3 side, and return the solid raw material 100 from the return path 63 into the housing 10 of the reactor 2.
  • the return path 63 is a flow path for returning the solid material 100 separated by the trap device 60 to the reactor 2.
  • the return path 63 includes a return side valve 65 in the midstream of the solid raw material 100 in the flow direction.
  • the supply path 6 is a return channel that connects the degassing device 3 and the reactor 2 as shown in FIG. 1 and returns the source gas from which impurities and the like have been removed by the degassing device 3 to the reactor 2.
  • a blower 80 is provided in the middle flow direction of the raw material gas.
  • the supply path 6 is downstream of the blower 80 and upstream of the reactor 2, and an introduction flow path 81 is connected.
  • the blower 80 is a device that pressurizes the source gas and pushes the source gas toward the reactor 2, and can introduce the source gas into the gas supply unit 52 of the reactor 2.
  • the introduction flow path 81 is a flow path for introducing fresh source gas into the supply path 6 from the outside.
  • the introduction flow path 81 includes an introduction valve 82 in the middle flow direction of the source gas.
  • the solid raw material 100 is a solid raw material of a reaction product, and is powdery or granular and has fluidity.
  • the solid raw material 100 of this embodiment is a fine powder of PVC that is a raw material of CPVC.
  • the median diameter of the solid raw material 100 is preferably 40 ⁇ m or more and 500 ⁇ m or less, and preferably 100 ⁇ m or more and 200 ⁇ m or less.
  • the median diameter of the solid raw material 100 of this invention means the median value of the particle size distribution in the volume reference
  • the solid raw material 100 is filled in the filling portion 51 in the reactor 2 in a state of being in direct contact with the upper surface of the gas dispersion member 15 in the reactor 2, and the solid raw material 100 is placed on the gas dispersion member 15. Is placed. At this time, it is preferable to fill the solid raw material 100 with 5% to 70% of the capacity of the filling part 51. If it is this range, it will be easy to form a fluidized bed at the time of stirring.
  • the blower 80 is driven to circulate the gas in the circulation circuit 7, and the introduction valve 82 and an exhaust valve (not shown) are opened.
  • the gas in the circulation circuit 7 is exhausted to the outside while introducing the chlorine gas as the raw material gas, the gas in the circulation circuit 7 is replaced with the chlorine gas, and the inside of the reactor 2 is in a chlorine gas atmosphere.
  • an exhaust valve (not shown) is closed, and a circulation operation is performed in which chlorine gas circulates in the circulation circuit 7.
  • the solid-state raw material 100 is irradiated with ultraviolet rays by the light emitting side rod-like portion 22 of the light emitting member 11 while driving the temperature adjusting member 12 and controlling the temperature in the housing 10 to be within a certain range. Then, the solid raw material 100 is mixed and fluidized by the blower 80 while stirring with the chlorine gas injected from the gas supply hole 56. By doing so, in a state where the solid raw material 100 is suspended and suspended in the raw material gas, that is, in a fluidized bed state, the chlorine group of the chlorine gas is replaced with the hydrogen group of PVC, and the reaction product CPVC Hydrochloric acid gas is generated as a reaction product gas.
  • the generated hydrochloric acid gas flows into the first path 61 together with chlorine gas as the raw material gas and a part of the solid raw material 100 by injection of the raw material gas from the gas supply hole 56 or the like.
  • the trap device 60 separates the solid raw material 100 into a mixed gas of hydrochloric acid gas and chlorine gas. Then, the solid raw material 100 is returned to the reactor 2 by gravity from the return path 63, and the mixed gas flows from the second path 62 to the deaerator 3.
  • the mixed gas When the mixed gas reaches the deaerator 3, it is separated into a hydrochloric acid gas as a reaction product gas and a chlorine gas as a raw material gas in the deaerator 3, and the hydrochloric acid gas is absorbed by a liquid such as water and discharged from a discharge port (not shown). It is discharged outside.
  • chlorine gas flows through the supply path 6, is introduced into the gas supply unit 52 of the reactor 2 by the blower 80, and is injected from the gas dispersion member 15 onto the solid raw material 100.
  • the internal pressure of the circulation circuit 7 decreases, so that chlorine gas is continuously supplied from the introduction flow path 81 so as to maintain the internal pressure of the circulation circuit 7.
  • the gas supply hole 56 of the gas dispersion member 15 is separated from the light emitting member 11 and the temperature adjustment member 12, so that a solid is formed on the gas dispersion member 15.
  • a raw material 100 is placed. Therefore, the solid raw material 100 blown up by the raw material gas can be stirred using the gravity drop, and the solid raw material 100 and the reaction product can be mixed more easily. Moreover, the solid raw material 100 and the reaction product in the housing 10 are easily soaked by convection.
  • the gas injection direction from the gas supply hole 56 is orthogonal to the longitudinal direction of the light emitting side bar 22 of the light emitting member 11 or the adjustment side bar 35 of the temperature adjusting member 12. It has a relationship that intersects the direction. Therefore, the source gas hardly hits the side surface of the light emitting side rod-shaped portion 22 or the adjustment side rod-shaped portion 35 at a right angle, and is not easily blocked by the side surface.
  • the reaction apparatus 1 of the present embodiment as shown in FIG. 5, there is a gap 25 between the light source part 20 and the surrounding part 21, and the light irradiated from the light source part 20 diffuses in the gap 25, and the surrounding part 21. Is transmitted through the surrounding portion 21 while being refracted or the like. Therefore, the substantially uniform light leveled by the surrounding portion 21 can be irradiated to the solid raw material 100 in the filling portion 51.
  • the cooling liquid or gas passes through the adjustment-side rod-like portion 35 to adjust the temperature of the solid raw material 100. Therefore, heat exchange can be performed without exposing the solid raw material 100 to the temperature adjusting liquid or gas.
  • the light emitting side rod-shaped portion 22 when viewed from the longitudinal direction of the light emitting side rod-shaped portion 22 of the light emitting member 11, the light emitting side rod-shaped portion 22 is a side wall portion 41 to the inner wall of the housing 10. It is arranged at a position away from 44. Therefore, ultraviolet rays can be irradiated in a plurality of directions.
  • the light emitting member 11 can irradiate ultraviolet rays in a plurality of directions, and the light emitting side rod-like portion 22 of the light emitting member 11 is formed of the adjustment side rod-like rows 33 and 33. Arranged in between. Therefore, it is possible to simultaneously irradiate ultraviolet rays toward the adjustment-side rod-like rows 33, 33, and a wide range of solid raw materials 100 can be reacted.
  • the first gas supply holes 150 are all inclined in the same direction, and the openings on the side of the filling part 51 are all one side wall part. It faces the 141 side.
  • the opening on the filling portion 51 side is provided in one direction (direction toward one filling-side side wall portion 141), and the source gas is concentrated and supplied in one direction. Therefore, in the case where the supply hole 56 of the gas dispersion member 15 is configured only by the first gas supply hole 150 that is an inclined hole, the filling side side wall part 143 (hereinafter referred to as the opposing side side wall part 143) facing the one filling side side wall part 141. Also, it is difficult for the source gas to flow in the vicinity.
  • the second gas supply hole 151 is provided at least in the vicinity of the opposing side wall portion 143. Therefore, fluidity can be ensured even in the vicinity of the opposite side wall portion 143 having low gas fluidity as compared with the one side wall portion 141 side (see FIG. 3B). Therefore, generation
  • the second gas supply holes 151 may be further provided in the vicinity of the filling side wall portions 141, 142, and 144 other than the facing side wall portion 143.
  • the outlet 170 that can be opened and closed by the opening / closing member 171 is provided, and the non-vertical portion 152 faces the outlet 170 side. Therefore, for example, the non-reactive gas that does not react with the reaction product and the solid raw material 100 is injected from the gas supply holes 150 and 151 in a state where the outlet 170 is closed as shown in FIG. Thus, the discharge outlet 170 is opened while the non-reactive gas injection state is maintained.
  • the reaction product and / or the solid raw material 100 in the filling portion 51 is pushed out to the discharge outlet 170 side by the non-reactive gas, and between the gas supply holes 150 and 150 and between the gas supply holes 150 and 151, That is, the reaction product and / or the solid raw material 100 is fluidized even in a portion where the gas supply holes 150 and 151 are not provided. Therefore, all or most of the reaction product and / or the solid raw material 100 in the filling unit 51 can be easily dispensed to a housing member (not shown), and maintenance such as cleaning of the filling unit 51 is easy.
  • the solid raw material 100 and the reaction product are constantly fluidized. Therefore, the fresh solid raw material 100 is supplied to the vicinity of the light emitting member 11, and a high quality CPVC can be manufactured compared with the past. Moreover, CPVC can be manufactured with a high yield.
  • reaction apparatus 200 according to the second embodiment of the present invention will be described.
  • the structure similar to the reactor 1 of 1st Embodiment attaches
  • the reaction apparatus 200 of the second embodiment includes a plurality of unit units 202 (202 a to 202 i) composed of a light emitting member 11, a temperature adjustment member 12, and a gas dispersion member 15.
  • the unit units 202 are arranged in a plane in the vertical and horizontal directions when viewed in a plan view.
  • unit units 202 made of the same constituent elements are repeatedly arranged vertically and horizontally.
  • nine unit units 202a to 202i of 3 ⁇ 3 are arranged in the horizontal direction X and the vertical direction Y.
  • the gas dispersion members 15a and 15b of the unit units 202a and 202b adjacent to each other in the longitudinal direction Y shown in FIG. 12 constitute one plane and are flush with each other, and the end surfaces of the gas dispersion members 15a and 15b are opposed to each other. Connected.
  • the intervals between the light emitting side bar portions 22 of the light emitting members 11 of the unit units 202 arranged in parallel in the vertical direction Y shown in FIG. 11 are equal. That is, the interval between the light emitting side rod-like portions 22 and 22 of the unit units 202a and 202b adjacent in the vertical direction Y is equal to the interval between the light emitting side rod-like portions 22 and 22 of the unit units 202b and 202c adjacent in the vertical direction Y.
  • the gas dispersion members 15a and 15d of the unit units 202a and 202d adjacent to each other in the horizontal direction X shown in FIGS. 11 and 12 constitute a single plane and are flush with each other.
  • the end faces of 15d are opposed to each other and connected.
  • the intervals between the light emitting side rod-like portions 22 of the light emitting members 11 of the unit units 202 arranged in parallel in the horizontal direction X shown in FIG. 11 are equal. That is, the interval between the light emitting side rod-like portions 22 and 22 of the unit units 202a and 202d adjacent in the horizontal direction X is equal to the interval between the light emitting side rod-like portions 22 and 22 of the unit units 202d and 202g adjacent in the horizontal direction X.
  • the adjusting side rod-like rows 33, 33, 33 of the temperature adjusting members 12, 12, 12 of the unit units 202a, 202d, 202g arranged in parallel in the horizontal direction X are parallel to each other.
  • the light emitting member 11, the temperature adjusting member 12, and the gas dispersion member 15 constitute the unit unit 202, and the same unit units 202a to 202i are arranged in parallel. The Therefore, the capacity can be easily expanded and the equipment cost at the time of expansion can be reduced.
  • one heat transfer tube of the temperature adjustment member 301 is bent in a wave shape to form an adjustment-side rod-like row 302.
  • the adjustment-side bar-shaped row 302 is configured by repeating a top surface-side folded portion 303, an adjustment-side rod-shaped portion 305, and a bottom surface-side folded portion 306 in this order.
  • the top surface side folded-back portion 303 is a portion that is folded back into a “U” shape by connecting the upper ends of the adjacent adjustment-side rod-shaped portions 305 and 305.
  • the adjustment-side rod-shaped portion 305 is a rod-shaped portion that connects the folded portions 303 and 306 and extends linearly.
  • the bottom-side folded portion 306 is a portion that is folded back into a “U” shape by connecting lower ends of the adjacent adjustment-side rod-shaped portions 305 and 305. Adjacent adjustment-side rod-like portions 305 and 305 have the cooling gas or the cooling liquid flowing in the opposite directions.
  • the shortest distance D1 between the outer peripheral surface of the adjustment-side rod-shaped portion 305 and the outer peripheral surface of the light emitting member 11 shown in FIG. 14, and the shortest distance between the outer peripheral surfaces of the adjustment-side rod-shaped portions 305 and 305 that belong to the same adjustment-side rod-shaped row 302 D2 and the shortest distance D3 between the outer peripheral surfaces of the adjustment-side rod-like portions 305 and 305 of the adjacent adjustment-side rod-like rows 302 and 302 are the relationship between the adjustment-side rod-like portion 35 of the first embodiment and the light emitting member 11, and the closest adjustment. Since it is the same as the relationship between the side bar-shaped portions 35 and 35 and the relationship between the adjacent adjustment-side bar-shaped rows 33 and 33, description thereof will be omitted.
  • the housing 701 of the reaction device 700 of the fourth embodiment is divided into a filling part 703 and a gas supply part 52 by a gas dispersion member 702 as shown in FIG.
  • the filling side wall portions 741 to 744 of the filling portion 703 include a first inner wall portion 710, a second inner wall portion 711, and a connection wall portion 712.
  • the first inner wall portion 710 and the second inner wall portion 711 are continuous with a step through the connection wall portion 712 as shown in FIG.
  • the connection wall portion 712 is a guide wall portion that guides the gas along the second inner wall portion 711 while blocking the gas injected from the gas dispersion member 702.
  • a discharge outlet 725 that can be opened and closed by an opening and closing member 726 is provided in one filling-side side wall 741.
  • the payout opening 725 is formed across the first inner wall portion 710, the second inner wall portion 711, and the connection wall portion 712.
  • the gas dispersion member 702 includes a main body plate portion 55 (see FIG. 2) and a plurality of gas supply holes 720.
  • the gas supply hole 720 includes only the first gas supply hole 150 and does not include the second gas supply hole 151.
  • connection wall portion 712 is opposed to the gas dispersion member 702 with an interval in the vertical direction.
  • the connection wall portion 712 is located on the projection surface of the gas supply hole 720 in the injection direction. That is, the gas supply hole 720 extends toward the connection wall portion 712.
  • the inflow space 715 is a space where the load from the solid raw material 100 is small and the pressure loss is small compared to other parts, and the gas easily flows in.
  • the height of the connection wall portion 712 with respect to the gas dispersion member 702 is preferably 0.1 cm or more, and is 5 cm or less. It is preferable. If it is this range, the gravity load to the gas from the solid raw material 100 can be suppressed, and it is easy to maintain the flow of the gas in the inflow space 715.
  • the filling portion 703 is provided with a constricted portion 730 from the middle portion to the upper portion in the vertical direction as shown in FIG.
  • the narrowed portion 730 is a portion having a smaller cross-sectional area as compared with the upstream side (the gas dispersion member 702 side) in the gas flow direction, and the gas flow velocity varies depending on the vertical direction when gas is injected.
  • the light emitting member 11 and the temperature adjusting member 12 are arranged.
  • the gas dispersion member 702 according to the present embodiment is composed of only gas supply holes 720 that are inclined holes. Therefore, as described above, there is a possibility that the powder retention part 180 (see FIG. 9) may occur in the vicinity of the opposite side wall part 143. Therefore, in the reaction apparatus 700 of the present embodiment, there is a connection wall portion 712 at a position that blocks the gas injected from the gas supply hole 720 of the opposite side wall portion 743 as shown in FIG. 17, and the gas supply hole 720 and the connection wall portion are provided. An inflow space 715 exists between 712 and 712.
  • the gas supply hole 720 extends toward the connection wall portion 712, and the gas injected from the gas supply hole 720 flows into the inflow space 715 where the gravity load due to the solid material 100 is small. Therefore, gas easily enters the inflow space 715, and gas easily flows along the second inner wall portion 711. Therefore, the powder staying portion 180 is hardly formed in the vicinity of the second inner wall portion 711 of the filling side wall portion 743, and generation of burnt resin or the like can be suppressed.
  • the light emitting member 11 and the temperature adjusting member are provided in the constricted portion 730 having a small cross-sectional area and a high gas flow rate as compared with the upstream side in the gas flow direction. 12 is arranged. Therefore, a larger amount of the solid raw material 100 can be reacted.
  • reaction apparatus 800 of the fifth embodiment will be described.
  • the reaction device 800 of the fifth embodiment is provided with a guiding member 801 in the filling unit 51 in addition to the light emitting member 11 and the temperature adjusting member 12.
  • the guide member 801 is provided in the vicinity of the specific filling side wall portion 143 and spaced apart from the gas dispersion member 702 in the vertical direction, and the gas dispersed by blocking the gas ejected from the gas dispersion member 702 is specified. It is a member that guides the gas along the filling side wall portion 143.
  • the guide member 801 is a triangular prism-shaped member whose bottom surface is a right triangle, and whose side surfaces include wall portions 802 to 804.
  • the first wall portion 802 is a guide wall portion that blocks the gas injected from the gas dispersion member 702 and guides the gas to the space between the second wall portion 803 and the specific filling side wall portion 143.
  • the second wall portion 803 is an upright wall portion that is orthogonal to the first wall portion 802 and faces a specific filling side wall portion 143.
  • the third wall portion 804 is an inclined wall portion that is inclined with respect to the first wall portion 802, and is a wall portion that forms one corner with the second wall portion 803.
  • the guide member 801 is made of resin and has resistance to the source gas and the reaction product gas.
  • the size of the guide member 801 when the gas dispersion member 702 is viewed in plan is larger than the opening area of the filling side opening 145 of the first gas supply hole 150.
  • the guide member 801 has substantially no recess in the portion where the solid raw material 100 and the reaction product are placed. That is, the second wall portion 803 and the third wall portion 804 are substantially free of recesses.
  • the term “substantially free of recesses” as used herein is not limited to a completely smooth case, but allows a recess that does not catch the solid raw material 100 and the reaction product. It means that the size is 1/10 or less of 100.
  • the guide member 801 is arranged such that the first wall portion 802 is opposed to the gas dispersion member 702 with a support member (not shown).
  • the corner formed by the second wall portion 803 and the third wall portion 804 forms the top portion.
  • a narrowed portion 830 is formed by the presence of the guide member 801 from the middle portion to the upper portion in the vertical direction.
  • the first wall portion 802 forms an inflow space 806 between the first wall portion 802 and the gas dispersion member 702, and is positioned on the extension of the gas injection direction of the first gas supply hole 150.
  • the second wall part 803 is opposed to the specific filling side wall part 143 with a space therebetween, and a flow path space 805 is formed between the second wall part 803 and the specific filling side wall part 143.
  • the shortest distance D21 between the gas dispersion member 702 and the first wall portion 802 shown in FIG. 18 is preferably 0.1 cm or more, and more preferably 0.5 cm or more.
  • the shortest distance D21 is preferably 5 cm or less, and more preferably 1 cm or less. If it is this range, the gravity load to the gas from the solid raw material 100 can be suppressed, and it is easy to maintain the flow of the gas in the inflow space 806.
  • the guiding member 801 is provided in the filling portion 51, and there is the first wall portion 802 that blocks in the injection direction from the first gas supply hole 150.
  • An inflow space 806 is formed between the one wall portion 802 and the gas dispersion member 702. Therefore, a part of the gas blocked by the first wall portion 802 easily flows into the flow path space 805, and the powder retention portion 180 is not easily formed in the vicinity of the opposing side wall portion 143. Therefore, generation
  • the corner formed by the second wall portion 803 and the third wall portion 804 constitutes the top portion. Therefore, the gravity load received from the solid material 100 on the guide member 801 is dispersed along the second wall portion 803 and the third wall portion 804. Therefore, the gravitational load applied to the guide member 801 from the solid raw material 100 can be suppressed.
  • the light emitting member 11 has a circular outer shape in cross section perpendicular to the extending direction, but the present invention is not limited to this.
  • the adjustment-side rod-like portion 35 of the temperature adjustment member 12 is cylindrical and has a circular outer shape in cross section perpendicular to the extending direction, but the present invention is not limited to this.
  • the outer shape of the cross section orthogonal to the extending direction of the light emitting member 11 and the adjustment-side rod-like portion 35 may be a shape other than a circle, for example, a polygonal shape such as a triangular shape, a quadrangular shape, a hexagonal shape, It may be oval or oval.
  • the adjustment-side rod-like group 32 is configured by two adjustment-side rod-like rows 33, but the present invention is not limited to this.
  • the adjustment side rod-shaped group 32 may be constituted by one row of adjustment side rod-like rows 33 or may be constituted by three or more rows of adjustment side rod-like rows 33.
  • the adjustment-side rod-shaped group 32 is arranged on both sides of the light emitting member 11 when viewed in plan, but the present invention is not limited to this.
  • the adjustment-side rod-shaped group 32 may be disposed only on one side of the light emitting member 11.
  • the adjustment-side rod-like rows 33 are arranged in a straight line when viewed in plan, but the present invention is not limited to this.
  • the adjustment-side rod-like rows 33 may be arranged in a curved shape or an annular shape.
  • the adjustment-side rod-like rows 33 may be arranged in the circumferential direction so as to surround the light emitting member 11 with the light emitting member 11 as the center as shown in FIG.
  • the adjustment-side rod-like portion 35 extends linearly, but the present invention is not limited to this. As shown in FIG. 22, the adjustment-side rod-like portion 35 may be bent in a wave shape as long as it extends linearly as a whole.
  • the adjustment-side rod-shaped group 32 has a square arrangement in which the four adjustment-side rod-like portions 35 constitute a square apex, but the present invention is not limited to this.
  • the adjustment side rod-shaped group 32 may be, for example, an arrangement in which the three adjustment side rod-like portions 35 constitute the vertices of an equilateral triangle.
  • the light emitting member 11 includes the single light emitting side rod-shaped portion 22, but the present invention is not limited to this.
  • the light emitting member 11 may include a plurality of light emitting side rod-like portions 22.
  • the temperature adjustment member 12 has a posture in which the inflow portion 31 is located on the bottom surface side with respect to the outflow portion 30 in the top-down direction, but the present invention is not limited to this.
  • the temperature adjustment member 12 may be turned upside down. That is, the temperature adjustment member 12 may be in a posture in which the inflow portion 31 is located on the top surface side with respect to the outflow portion 30 in the top-down direction.
  • the nine unit units 202a to 202i are provided, but the present invention is not limited to this. As long as it is composed of a plurality of unit units 202, it may be composed of eight or less unit units 202, or may be composed of ten or more unit units 202. In the second embodiment described above, the nine unit units 202a to 202i are arranged vertically and horizontally, but the unit units 202 may be arranged in a line.
  • the filling side opening 145 and the supply side opening 146 are shifted, but the present invention is not limited to this.
  • the filling side opening 145 and the supply side opening 146 may coincide with the thickness direction (vertical direction).
  • the first gas supply hole 150 and the second gas supply hole 151 have the same inner diameter in the depth direction, but the present invention is not limited to this.
  • the first gas supply hole 150 and the second gas supply hole 151 may have different inner diameters in the depth direction.
  • the first gas supply hole 150 may have an inner diameter that increases in the depth direction as shown in FIG. 23B, and the opening area of the filling side opening 145 may be smaller than the opening area of the supply side opening 146.
  • the reverse may be sufficient. That is, the inner diameter may be reduced in the depth direction, and the opening area of the filling side opening 145 may be larger than the opening area of the supply side opening 146.
  • each first gas supply hole 150 is inclined so that the central axes are parallel to each other, but the present invention is not limited to this.
  • the axial direction of each first gas supply hole 150 may be random as shown in FIG.
  • each first gas supply hole 150 is inclined such that the central axis faces the same direction, but the present invention is not limited to this.
  • Each first gas supply hole 150 may be directed in a direction with a different central axis.
  • the central axis may be directed toward the center as shown in FIG.
  • the first gas supply holes 150 are arranged so as to be the vertices of an equilateral triangle, but the present invention is not limited to this.
  • the first gas supply holes 150 may be arranged in a grid shape so as to have a square apex as shown in FIG. That is, the distance D14 between the first gas supply hole 150a and the first gas supply hole 150b adjacent in the horizontal direction is equal to the distance D15 between the first gas supply hole 150a and the first gas supply hole 150c adjacent in the vertical direction. May be.
  • the opening shapes of the first gas supply hole 150 and the second gas supply hole 151 are circular, but the present invention is not limited to this.
  • the opening shapes of the first gas supply hole 150 and the second gas supply hole 151 may be other than circular, for example, may be elliptical, polygonal, oval, It may be a long hole.
  • the gas supply hole 56 includes the two types of supply holes, the first gas supply hole 150 and the second gas supply hole 151, but the present invention is not limited to this. .
  • the gas supply hole 56 may be configured with only the first gas supply hole 150 as in the fourth and fifth embodiments, or may be configured with only the second gas supply hole 151.
  • other types of supply holes may be mixed in the gas supply hole 56.
  • the casing 10 has a vertically long rectangular parallelepiped shape, but the present invention is not limited to this.
  • the shape of the housing 10 may be other than a vertically long rectangular parallelepiped shape, and may be, for example, a cylindrical shape or a prism shape having a polygonal bottom surface.
  • the outer shape of the gas supply unit 52 is a rectangular parallelepiped shape is illustrated, but the present invention is not limited to this.
  • the outer shape of the gas supply unit 52 may be, for example, an inverted polygonal pyramid shape such as an inverted triangular pyramid, an inverted quadrangular pyramid, or an inverted hexagonal pyramid, or an inverted conical shape.
  • the inside of the gas supply unit 52 may have a tapered shape that spreads from the gas inlet 880 toward the gas dispersion member 15 as shown in FIG.
  • the shape of the main body plate portion 55 constituting the skeleton of the gas dispersion member 15 is a square shape, but the present invention is not limited to this.
  • the case 10 can be changed as appropriate depending on the shape of the part (the boundary part between the filling part 51 and the gas supply part 52) partitioned by the gas dispersion member 15.
  • the shape of the main body plate portion 55 may be a circular shape.
  • the direction of the first gas supply hole 150 of the gas dispersion member 15 of each unit unit 202 may be adjusted so that the solid material 100 faces the discharge outlet 170 side.
  • the inclination direction of the first gas supply hole 150 of the gas dispersion member 15 of the unit unit 202 adjacent to the filling side wall 141 to which the discharge outlet 170 belongs is directed toward the discharge outlet 170, and other units. You may make it the inclination direction of the 1st gas supply hole 150 of the gas dispersion member 15 of the unit 202 face the filling side wall part 141 side.
  • the wall portions 712 and 802 that block the gas injected from the gas dispersion member 702 are spread in a planar shape, but the shape of the wall portions 712 and 802 is not limited to this.
  • the wall portions 712 and 802 may extend in a curved shape or a wave shape.
  • the guide member 801 has a triangular prism shape, but the present invention is not limited to this. Other polygonal column shapes such as a quadrangular column, pentagonal column, hexagonal column, etc., or a curved surface such as a cylindrical shape may be used.
  • the guide member is preferably configured such that the portion on which the solid raw material 100 and the reaction product are placed is a downwardly inclined surface or a downwardly inclined surface. By doing so, the gravitational load received from the solid material 100 on the guide member 801 can be dispersed by the downward inclined surface or the downward inclined curved surface.
  • the light emitting member 11 is disposed in the filling portion 51, but the present invention is not limited to this.
  • the light emitting member 11 may be provided outside the filling unit 51 as long as the solid material 100 in the filling unit 51 can be irradiated with ultraviolet rays.
  • the solid material 100 in the filling portion 51 can be irradiated with ultraviolet rays even if the light emitting member 11 is provided outside the filling portion 51.
  • the main body plate portion 55 and the guide member 801 are made of resin, but the present invention is not limited to this.
  • the main body plate portion 55 and the guide member 801 may be made of ceramics such as glass or rubber such as fluoro rubber as long as they are resistant to the reaction gas.
  • each constituent member can be freely replaced or added between the embodiments.
  • the guide member 801 of the reaction device 800 of the fifth embodiment may be inserted into the filling portion 703 of the reaction device 700 of the fourth embodiment.
  • Example 1 In Example 1, as shown in FIG. 28, cylindrical heat transfer tubes 402 are arranged in a row in the vertical direction in a container 401 having a gas dispersion member 400 of 25 cm long ⁇ 25 cm wide as a bottom plate and arranged in the center in the horizontal direction. Further, each heat transfer tube 402 was inserted into the container 401 in a vertical posture so that the shortest distance D between the side surfaces of the heat transfer tubes 402 and 402 that were closest to each other was 2.4 cm.
  • the heat transfer tube 402 used was a cylindrical tube having an outer diameter of 3.2 cm and a length of 110 cm, and was arranged in a vertical posture at a position 10 cm above the gas dispersion member 400.
  • Example 2 In Example 2, it inserted in the vertical attitude
  • each heat transfer tube 402 was inserted in a vertical posture so that the shortest distance D between the side surfaces of the closest heat transfer tubes 402 and 402 was 1.5 cm.
  • FIG. 30 a graph derived from the results of Table 1 is shown in FIG. As shown in FIG. 30, when the wall distance between the heat transfer tubes is approximately 1.9 cm or more, the standard deviation of the tracer concentration is 0.20% by weight or less (that is, the difference in standard deviation from the case where no heat transfer tube is used). It was estimated that it was within the range of 0.06% by weight or less.
  • the solid raw material 100 and the reaction product can be uniformly mixed if the gap between obstacles when the solid raw material 100 flows is 1.9 cm or more.
  • Example 3 In Example 3, a first gas supply hole having a diameter of 0.15 cm and an inclination angle ⁇ 1 of 30 degrees is formed on a flat plate made of Teflon (registered trademark) (manufactured by Kurimoto Steel Corporation) with a pitch (center-to-center). The gas dispersion member was formed so that the distance) was 0.7 cm, and the second gas supply holes having a diameter of 0.1 cm were formed in two rows around the first gas supply holes.
  • Teflon registered trademark
  • Example 4 In Example 4, the diameter of the first gas supply hole was 0.1 cm, and other than that was the same as Example 3.
  • Example 5 (Example 5) In Example 5, the inclination angle ⁇ 1 of the first gas supply hole was set to 45 degrees, and other than that was the same as Example 4.
  • Comparative Example 2 In Comparative Example 2, the diameter of the first gas supply hole was 0.15 cm, and the inclination angle ⁇ 1 was 45 degrees. Otherwise, it was the same as Example 3.
  • the solid raw material to be used was PVC powder having a particle diameter of 40 ⁇ m or more and 500 ⁇ m or less and a median diameter of 150 ⁇ m.
  • the angle of repose according to JIS R 9301-2-2 (corresponding to ISO 902: 1976) was measured for this solid raw material, and it was 35 ° to 40 °.
  • Table 1 shows the results of the drop measurement test. “C” represents that the solid raw material does not substantially drop. “D” indicates that the solid raw material falls, but the raw material has a slow dropping speed and can be ignored in the manufacturing process. “E” represents a case where the solid raw material is dropped and the solid raw material has a high falling speed and cannot be ignored in the manufacturing process.
  • Non-flow measurement test The same solid material as described above was placed on the gas dispersion members of Examples 3 and 5 and Comparative Example 2, and colored particles were added to the solid material. And the non-flowing part after making it flow with the gas of 0.125 m / s of linear velocity in the state was confirmed visually, and the quantity of the resin raw material used as non-flowing was measured. As described above, in Comparative Example 2, when the solid raw material was placed, it dropped from the gas supply hole. Therefore, fluid at the fluidization start speed was always flowed from the gas supply hole, and measurement was performed in a state where the fall was prevented.
  • Example 4 As a result of the non-flow amount measurement test, in Example 4 and Comparative Example 2, the colored particles were well mixed with the solid raw material, and no non-flow portion was observed. In Example 5, although there was a minute amount of non-flowing colored particles, the amount was substantially negligible in terms of quality and was mixed with the solid raw material almost uniformly.
  • the inclination angle of the first gas supply hole is less than 45 degrees.
  • the diameter of the first gas supply hole is less than 10 times the median diameter of the solid raw material.

Landscapes

  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

L'invention aborde le problème consistant à fournir un réacteur à lit fluidisé susceptible de mélanger une matière première solide plus efficacement que la technique antérieure, et susceptible de produire efficacement un produit de réaction à un niveau donné, ou plus élevé. L'invention concerne également un procédé de production d'une résine de poly(chlorure de vinyle) chloré. A cette fin, l'invention concerne un réacteur à lit fluidisé comprenant un réacteur qui contient une matière première solide dans un état pulvérulent ou granulaire, un gaz étant introduit dans ledit réacteur chargé de ladite matière première solide, et la matière première solide étant fluidisée au moyen du gaz, tout en subissant une réaction avec le gaz, dans le but d'obtenir le produit de la réaction. Le réacteur à lit fluidisé contient un élément électroluminescent et un élément de réglage de la température, l'élément électroluminescent présentant un segment en forme de barre sur le côté électroluminescent, qui est disposé à l'intérieur du réacteur et irradie la matière première solide avec une lumière, et l'élément de réglage de la température présente un segment en forme de barre sur le côté réglage, qui est disposé à l'intérieur du réacteur et règle la température de la matière première solide. En les points où le segment en forme de barre devient adjacent au segment en forme de barre côté réglage, les surfaces périphériques extérieures desdits segments présentent une distance la plus courte de 1,9 cm ou plus.
PCT/JP2018/011133 2017-03-24 2018-03-20 Réacteur à lit fluidisé et procédé de production d'une résine de poly(chlorure de vinyle) chloré WO2018174075A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7458815B2 (ja) 2019-02-19 2024-04-01 大阪瓦斯株式会社 触媒容器

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5215638B1 (fr) * 1965-01-15 1977-05-02
JPS56166204A (en) * 1980-05-27 1981-12-21 Chisso Corp Continuous fluorination of polyvinyl chloride and unit therefor
JPS6079541U (ja) * 1983-11-08 1985-06-03 三井造船株式会社 気相流動層反応器
JPH03153703A (ja) * 1989-11-13 1991-07-01 Showa Denko Kk 流動層型気相重合装置のガス分散板
JPH03153704A (ja) * 1989-11-13 1991-07-01 Showa Denko Kk 流動層型気相重合装置のガス分散板
JP2002275213A (ja) * 2001-01-15 2002-09-25 Kanegafuchi Chem Ind Co Ltd 塩素化塩化ビニル系樹脂の製造方法および装置

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5215638B1 (fr) * 1965-01-15 1977-05-02
JPS56166204A (en) * 1980-05-27 1981-12-21 Chisso Corp Continuous fluorination of polyvinyl chloride and unit therefor
JPS6079541U (ja) * 1983-11-08 1985-06-03 三井造船株式会社 気相流動層反応器
JPH03153703A (ja) * 1989-11-13 1991-07-01 Showa Denko Kk 流動層型気相重合装置のガス分散板
JPH03153704A (ja) * 1989-11-13 1991-07-01 Showa Denko Kk 流動層型気相重合装置のガス分散板
JP2002275213A (ja) * 2001-01-15 2002-09-25 Kanegafuchi Chem Ind Co Ltd 塩素化塩化ビニル系樹脂の製造方法および装置

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7458815B2 (ja) 2019-02-19 2024-04-01 大阪瓦斯株式会社 触媒容器

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