Polyester reaction device and method

Abstract

The invention discloses a polyester reaction device and method. The polyester reaction device comprises: a reactor having a reaction chamber, and a feed port, a discharge port and a gas phase outlet which are communicated with the reaction chamber; the isolation part comprises a sleeve arranged in the reaction chamber, the bottom of the sleeve is connected to the bottom wall of the reaction chamber in a sealed mode, a gap is formed between the top of the sleeve and the top wall of the reaction chamber, a gap is formed between the outer side wall of the sleeve and the inner side wall of the reaction chamber to form a feeding area, and the feeding area is communicated with the feeding port; a reaction area is defined by the inner side wall of the sleeve and the bottom wall of the reaction chamber, and the reaction area is communicated with the discharge port and the gas phase outlet; the stirring part is mounted in the reactor and extends to the reaction area to stir reaction materials in the reaction area; and the temperature control component is connected with the sleeve so as to control the temperature of the reaction area. According to the invention, high-efficiency production of esterification or ester exchange reaction of polyester can be realized.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical industry, in particular to a polyester reaction device and method. BACKGROUND

[0002] Polyesters are a class of polymers obtained by polycondensation of polyols and polyacids, and the polymer long chains are connected by intermolecular ester bonds. Polyester materials have excellent mechanical properties, chemical resistance, heat resistance and weather resistance, and are easy to process and shape, so they are widely used in textiles, electronics, construction and packaging and other fields.

[0003] Polyester industrial production is divided into two technical routes of direct esterification and ester exchange. The direct esterification route is that the carboxyl group of diacid and the hydroxyl group of diol undergo esterification to generate diester oligomers and water, and the esterification effect directly affects the molecular weight, color phase, mechanical properties and other indicators of polyester products; the ester exchange route uses dimethyl ester corresponding to diacid to react with diol to generate diester oligomers and byproduct methanol, and the reaction conditions are more consistent compared with direct esterification. In polyester industrial production, a full-mixing reactor is usually used. The full-mixing reactor in the traditional technology includes a shell and a stirring device. The top of the shell is provided with a feed inlet, the bottom of the shell is provided with a discharge outlet, and the stirring device is arranged in the shell. The material is sent into the shell at a constant rate through the feed inlet, the stirring device fully mixes the mixed raw materials, and then the fully reacted material is transported to the next unit at a constant rate. In actual production, the unreacted monomers in the full-mixing reactor are mixed with the materials that have reacted to a certain extent in real time, and there are many shortcomings such as low single-pass conversion rate, low production efficiency and uneven distribution of material concentration. It is usually necessary to connect multiple full-mixing reactors in series or prolong the residence time to improve the conversion rate of raw materials, which will reduce the production efficiency of polyester. SUMMARY

[0004] Therefore, it is necessary to provide a polyester reaction device capable of realizing high-efficiency production.

[0005] An embodiment of the present application provides a polyester reaction device.

[0006] A polyester reaction device comprises:

[0007] A reactor having a reaction chamber and a feed inlet, a discharge outlet and a gas phase outlet communicating with the reaction chamber;

[0008] The isolation component comprises a sleeve arranged in the reaction chamber, the bottom of the sleeve is sealingly connected to the bottom wall of the reaction chamber, the top of the sleeve is spaced from the top wall of the reaction chamber, the outer wall of the sleeve is spaced from the inner wall of the reaction chamber to form a feeding area, the feeding area is communicated with the feeding port, the inner wall of the sleeve and the bottom wall of the reaction chamber form a reaction area, the reaction area is communicated with the discharging port and the gas phase outlet;

[0009] The stirring component is installed in the reactor and extends into the reaction area to stir the reaction material in the reaction area along a first direction and a second direction;

[0010] In addition, the temperature control component is used to control the temperature of the reaction area.

[0011] In some embodiments, the feeding area is provided with annular flow guiding baffles.

[0012] In some embodiments, the number of flow guiding baffles is multiple, and a part of the flow guiding baffles are connected to the outer wall of the sleeve, and another part of the flow guiding baffles are connected to the inner wall of the reaction chamber.

[0013] In some embodiments, the flow guiding baffles connected to the outer wall of the sleeve and the flow guiding baffles connected to the inner wall of the reaction chamber are distributed in a staggered manner to form flow channels capable of allowing the reaction material to flow in a meandering manner.

[0014] In some embodiments, the lowermost flow guiding baffle in the feeding area is located at a position of 20% to 30% of the height of the feeding area.

[0015] In some embodiments, the uppermost flow guiding baffle in the feeding area is located at a position of 60% to 80% of the height of the feeding area.

[0016] In some embodiments, the reaction chamber has a cylindrical structure, and the sleeve has a cylindrical structure.

[0017] In some embodiments, the central axis of the sleeve coincides with the central axis of the reactor, and the inner diameter of the sleeve is 40% to 70% of the inner diameter of the reactor.

[0018] In some embodiments, the feeding port and the discharging port are respectively located at the bottom of the reactor, and the gas phase outlet is located at the top of the reactor.

[0019] In some embodiments, the isolation component further comprises a first partition plate and a second partition plate, and the first partition plate and the second partition plate are arranged at different height positions of the reaction area.

[0020] In some embodiments, the first partition plate and the second partition plate are each independently in a ring shape.

[0021] In some embodiments, the first partition plate is located at a height of 50% to 70% of the reaction zone.

[0022] In some embodiments, the second partition plate is located at a height of 20% to 40% of the reaction zone.

[0023] In some embodiments, the width of the first partition plate is equal to the width of the second partition plate along the direction of advancement of the polyester raw material.

[0024] In some embodiments, the isolation component further comprises a flow guide plate, which is disposed in the reaction zone and connected to the inner side wall of the sleeve.

[0025] In some embodiments, the flow guide plate is located between the first partition plate and the second partition plate.

[0026] In some embodiments, the flow guide plate is in a ring shape.

[0027] In some embodiments, the width of the flow guide plate is less than the width of the first partition plate along the direction of advancement of the polyester raw material.

[0028] In some embodiments, the stirring component comprises a stirring shaft, a stirring paddle, and a stirring drive component, one end of the stirring shaft extends into the reaction zone, the stirring paddle is connected to the stirring shaft, the stirring drive component is installed on the reactor and connected to the stirring shaft, and the stirring drive component is used to drive the stirring shaft to rotate to drive the stirring paddle to rotate.

[0029] In some embodiments, the stirring paddle comprises a spaced apart paddle stirring paddle and a propelling stirring paddle.

[0030] In some embodiments, the paddle stirring paddle is located above the propelling stirring paddle along the height direction.

[0031] In some embodiments, the paddle stirring paddle is located at a height of 45% to 55% of the reaction zone along the height direction.

[0032] In some embodiments, the propelling stirring paddle is located at a height of 10% to 20% of the reaction zone along the height direction.

[0033] In some embodiments, the temperature control component comprises a heating coil, which is disposed in the reaction zone.

[0034] In some embodiments, the temperature control component further comprises a heat preservation layer connected to the outer wall of the reactor.

[0035] An embodiment of the present application provides a polyester reaction method.

[0036] A polyester reaction method comprises the following steps:

[0037] The polyester raw material is mixed by first direction stirring and second direction stirring; the temperature during mixing is controlled to be 150-300°C, and the pressure during mixing is controlled to be 0.03-0.3 MPaA.

[0038] In some embodiments, the first direction is the forward direction of the polyester raw material, and the second direction is the direction intersecting the forward direction of the polyester raw material.

[0039] In some embodiments, the temperature during mixing is controlled to be 230-270°C.

[0040] In some embodiments, the pressure during mixing is controlled to be 0.1-0.2 MPaA.

[0041] In some embodiments, the stirring speed during stirring along the first direction is controlled to be 10-100 rpm.

[0042] In some embodiments, the stirring speed during stirring along the first direction is controlled to be 30-70 rpm.

[0043] In some embodiments, the stirring speed during stirring along the second direction is controlled to be 10-100 rpm.

[0044] In some embodiments, the stirring speed during stirring along the second direction is controlled to be 30-70 rpm.

[0045] In some embodiments, the polyester raw material comprises diacid and / or corresponding dimethyl ester thereof, and dihydric alcohol, the diacid and / or corresponding dimethyl ester thereof is selected from C4-C20 diacid and / or corresponding dimethyl ester thereof, and the dihydric alcohol is selected from C2-C20 aliphatic dihydric alcohol and / or aromatic dihydric alcohol.

[0046] In some embodiments, the diacid and / or corresponding dimethyl ester thereof comprises one or more of succinic acid, adipic acid, terephthalic acid, isophthalic acid, phthalic acid, diphenic acid, naphthalic acid, furan dicarboxylic acid, thiophene dicarboxylic acid, and cyclohexane dicarboxylic acid.

[0047] In some embodiments, the diacid and / or its corresponding dimethyl ester include one or more of succinic acid, adipic acid, and terephthalic acid.

[0048] In some embodiments, the diol includes one or more of 1,4-cyclohexanedimethanol, 2,2,4,4-tetramethyl-1,3-cyclobutanediol, isosorbide, ethylene glycol, neopentyl glycol, 1,3-propanediol, 2-methyl-1,3-propanediol, 1,2-propanediol, 1,4-butanediol, 2,3-butanediol, 1,2-pentanediol, 1,4-pentanediol, 1,5-pentanediol, 3-methyl 1,5-pentanediol, 2,2,4-trimethyl-1,3-pentanediol, diethylene glycol, 1,6-hexanediol, 1,8-octanediol, 1,10-decanediol, spiro glycol, and tricyclodecane dimethanol.

[0049] In some embodiments, the diol includes one or more of neopentyl glycol, 1,4-cyclohexanedimethanol, and 2,2,4,4-tetramethyl-1,3-cyclobutanediol.

[0050] In some embodiments, the feed temperature of the polyester feedstock is controlled to be 150°C to 300°C.

[0051] In some embodiments, the feed temperature of the polyester feedstock is controlled to be 230°C to 270°C.

[0052] In some embodiments, the feed flow rate of the polyester feedstock is controlled to be 5000 Kg / h to 20000 Kg / h.

[0053] In some embodiments, the feed flow rate of the polyester feedstock is controlled to be 8000 Kg / h to 15000 Kg / h.

[0054] In some embodiments, the feed alcohol to acid ratio / alcohol to ester ratio of the polyester feedstock is controlled to be 1.10:1 to 1.25:1.

[0055] In some embodiments, the feed alcohol to acid ratio / alcohol to ester ratio of the polyester feedstock is controlled to be 1.15:1 to 1.20:1.

[0056] In some embodiments, the residence time of the polyester feedstock when mixed is controlled to be 50 min to 500 min.

[0057] In some embodiments, the residence time of the polyester feedstock when mixed is controlled to be 60 min to 200 min.

[0058] In some embodiments, the polyester reaction method employs the polyester reaction device described in any of the above embodiments.

[0059] The polyester reaction device has short residence time of polyester raw materials, uniform heating, and can realize high-efficiency esterification or ester exchange reaction. Specifically, in the present application, the reaction chamber is divided into a feeding area and a reaction area by a sleeve, and the series connection of the full-mixed flow effect of the full-mixed flow reactor and the plug flow effect of the plug flow reactor is realized in one reactor through the sub-chamber structure composed of the feeding area and the reaction area, so as to solve the problems of low material conversion rate and uneven concentration distribution in the production process in the traditional technology, and can be used for esterification and ester exchange production route at the same time. Specifically, when the polyester reaction device in the present application is used, the polyester raw materials are fed into the feeding area through the feeding port, and then the polyester raw materials are transported into the reactor. After the preliminary mixing of the polyester raw materials in the feeding area, the polyester raw materials are mixed in the radial direction under the stirring action in the first direction, and then are mixed in the axial direction under the stirring action in the second direction. Finally, the esterification / ester exchange product is obtained through the discharge port. The flow state of the polyester raw materials under the stirring action in the first direction tends to be plug flow, and the flow state of the polyester raw materials under the stirring action in the second direction tends to be full-mixed flow. The series connection of the plug flow and the full-mixed flow is realized through the sub-chamber structure, so as to effectively improve the production efficiency and significantly shorten the single-pass residence time of the materials. BRIEF DESCRIPTION OF DRAWINGS

[0060] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed in the embodiment description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0061] In order to more completely understand the present application and its beneficial effects, the following will be described with reference to the drawings. In the following description, the same reference numerals represent the same parts.

[0062] Figure 1 The polyester reaction device described in an embodiment of the present application is shown in the schematic diagram.

[0063] BRIEF DESCRIPTION OF DRAWINGS

[0064] 10, polyester reaction device; 100, reactor; 101, reaction chamber; 102, feeding port; 103, discharge port; 104, gas phase outlet; 200, isolation component; 201, sleeve; 202, first partition plate; 203, second partition plate; 204, flow guide plate; 300, stirring component; 301, stirring shaft; 302, paddle stirring paddle; 303, propeller stirring paddle; 304, stirring driving component; 400, temperature control component; 401, heating coil; 402, heat preservation layer; 500, flow guide tower plate. DETAILED DESCRIPTION

[0065] In order to make the above objectives, features and advantages of the present application more clear and comprehensible, the detailed description of the specific embodiments of the present application is made below with reference to the accompanying drawings. In the following description, a lot of specific details are set forth in order to fully understand the present application. However, the present application can be implemented in many other different ways than those described herein, and those skilled in the art can make similar improvements without departing from the spirit of the present application, and therefore the present application is not limited to the specific embodiments disclosed below.

[0066] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only used to facilitate the description of the present application and simplify the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation of the present application.

[0067] In the present application, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connection", "fixing" and the like should be understood broadly, for example, it can be fixed connection, or detachable connection, or integral; it can be mechanical connection, or electrical connection; it can be direct connection, or indirect connection through intermediate medium; it can be the internal communication of two elements or the interaction relationship between two elements, unless otherwise explicitly limited. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0068] In the present application, unless otherwise explicitly specified and limited, the first feature "on" or "under" the second feature can be direct contact between the first and second features, or indirect contact between the first and second features through an intermediate medium. Moreover, the first feature "above", "over" and "on" the second feature can be that the first feature is directly above or obliquely above the second feature, or only indicates that the horizontal height of the first feature is higher than that of the second feature. The first feature "below", "under" and "under" the second feature can be that the first feature is directly below or obliquely below the second feature, or only indicates that the horizontal height of the first feature is less than that of the second feature.

[0069] In the description of the present application, the meaning of several is one or more, the meaning of multiple is two or more, greater than, less than, exceed, etc. are understood as not including the number, above, below, within, etc. are understood as including the number. If it is described as first, second, it is only used for the purpose of distinguishing technical features, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features or the sequence of indicated technical features.

[0070] In this paper, "optionally", "optional", "optional" means optional, that is, selected from "yes" or "no" two parallel schemes. If there are multiple "optional" in a technical solution, unless otherwise specified, and there is no contradiction or mutual restriction, each "optional" is independent of each other. In this application, "optionally contains", "optionally contains" and the like, means "contains or does not contain".

[0071] In this application, if there is no contrary description, the sum of the parts of each component in the composition can be 100 parts by weight. If not specified, the percentage (including weight percentage) in this application is based on the total weight of the composition, and "wt%" in this paper means mass percentage.

[0072] In this paper, unless otherwise specified, each reaction step can be carried out in the order described in this paper, or not in the order described in this paper. For example, each reaction step can contain other steps, and the order of reaction steps can also be appropriately changed. This can be determined by the skilled person according to conventional knowledge and experience. Preferably, the reaction method in this paper is sequential.

[0073] In this application, when referring to a numerical interval (i.e. a numerical range), unless otherwise specified, the distribution of optional values in the numerical interval is considered to be continuous, and includes both numerical endpoints (i.e. minimum and maximum values) of the numerical interval, and each value between the two numerical endpoints. Unless otherwise specified, when a numerical interval refers only to integers within the numerical interval, including both endpoint integers of the numerical range and each integer between the two endpoints, it is equivalent to directly listing each integer. When multiple numerical ranges are provided to describe a characteristic or property, these numerical ranges can be combined. In other words, unless otherwise specified, the numerical range disclosed in this application should be understood to include any and all subranges included therein. The "numerical value" in the numerical interval can be any quantitative value, such as a number, a percentage, a ratio, etc. The "numerical interval" allows the broadest possible inclusion of percentage intervals, ratio intervals, value intervals, etc. quantitative intervals.

[0074] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description herein is for describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items.

[0075] An embodiment of the present application provides a polyester reaction device to solve at least one of the following technical problems in the conventional polyester industrial production: (1) in the conventional full-mixed flow reactor, the unreacted monomers are mixed with the materials that have reacted to a certain extent in real time, and there are multiple disadvantages such as low single-pass conversion rate, low production efficiency, and uneven material concentration distribution. (2) The conversion rate of raw materials is improved by connecting multiple full-mixed flow reactors in series or prolonging the residence time, which reduces the production efficiency of the polyester. The polyester reaction device will be described below with reference to the accompanying drawings.

[0076] An embodiment of the present application provides a polyester reaction device 10, for example, as shown in Figure 1 Figure 1 The polyester reaction device 10 provided by an embodiment of the present application is a structural schematic diagram. The polyester reaction device 10 of the present application can be used for high-efficiency production of polyester.

[0077] In order to more clearly illustrate the structure of the polyester reaction device 10, the polyester reaction device 10 will be introduced below with reference to the accompanying drawings.

[0078] For example, as shown in Figure 1 A polyester reaction device 10 includes a reactor 100, an isolation component 200, a stirring component 300, and a temperature control component 400.

[0079] The reactor 100 has a reaction chamber 101, and a feed inlet 102, a discharge outlet 103, and a gas phase outlet 104 communicating with the reaction chamber 101.

[0080] The isolation component 200 includes a sleeve 201 arranged in the reaction chamber 101. The bottom of the sleeve 201 is sealingly connected to the bottom wall of the reaction chamber 101, the top of the sleeve 201 has a spacing with the top wall of the reaction chamber 101, and the outer side wall of the sleeve 201 has a spacing with the inner side wall of the reaction chamber 101 to form a feed area. The feed area communicates with the feed inlet 102. The inner side wall of the sleeve 201 and the bottom wall of the reaction chamber 101 enclose a reaction area. The reaction area communicates with the discharge outlet 103 and the gas phase outlet 104.

[0081] ​The stirring component 300 is installed in the reactor 100 and extends into the reaction zone to stir the reaction material in the reaction zone along a first direction and a second direction. It should be noted that the first direction and the second direction can be a direction of the reaction chamber 101 intersecting the advancing direction of the polyester raw material and the advancing direction of the polyester raw material.

[0082] The temperature control component 400 is connected to the sleeve 201 to control the temperature of the reaction zone.

[0083] In the present application, the sleeve 201 is used to divide the reaction chamber 101 into a feeding zone and a reaction zone, and the divided chamber structure composed of the feeding zone and the reaction zone realizes the series connection of the mixed flow reactor 100 mixed flow effect + the plug flow reactor 100 plug flow effect in one reactor 100, solves the problems of low material conversion rate and uneven concentration distribution in the production process in the traditional technology, and can be used for esterification and ester exchange production routes at the same time. Specifically, in use of the polyester reaction device 10, the polyester raw material is fed into the feeding zone through the feeding port 102 and is delivered into the reactor 100, the polyester raw material is preliminarily mixed in the feeding zone and then enters the reaction zone, is fully mixed in the radial direction under the action of the first direction stirring, and is fully mixed in the axial direction under the action of the second direction stirring, and finally the esterification / ester exchange product is obtained through the discharge port 103, the flow state of the polyester raw material in the feeding zone and under the action of the first direction stirring tends to be plug flow, and the flow state of the polyester raw material under the action of the second direction stirring tends to be fully mixed flow, the divided chamber structure realizes the series connection of the plug flow and the fully mixed flow, effectively improves the production efficiency, and significantly shortens the single-pass residence time of the material.

[0084] In some embodiments, the feeding zone is provided with annular flow guide trays 500.

[0085] In some embodiments, the number of flow guide trays 500 is multiple, and a part of the flow guide trays 500 are connected to the outer side wall of the sleeve 201, and another part of the flow guide trays 500 are connected to the inner side wall of the reaction chamber 101.

[0086] In some embodiments, the number of flow guide trays 500 is 4-8. For example, the number of flow guide trays 500 is 4, 5, 6, 7 or 8.

[0087] In some embodiments, the flow guide trays 500 connected to the outer side wall of the sleeve 201 and the flow guide trays 500 connected to the inner side wall of the reaction chamber 101 are distributed in a staggered manner to form flow channels capable of allowing the reaction material to flow in a meandering manner, so that the reaction material flows in a meandering manner and improves the reaction efficiency of the reaction material.

[0088] In some embodiments, the flow guide trays 500 connected to the outer side wall of the sleeve 201 are perpendicular to the outer side wall of the sleeve 201.

[0089] In some embodiments, the draft tubes 500 attached to the inner side wall of the reaction chamber 101 are perpendicular to the inner side wall of the reaction chamber 101.

[0090] In some embodiments, the lowest draft tube 500 in the feed zone is located at a height of 20-30% of the feed zone. For example, the lowest draft tube 500 in the feed zone is located at a height of the feed zone, which includes but is not limited to 20%, 22%, 25%, 26%, 28%, 29%, 30%, or a range between any two of the aforementioned values. It should be noted that the height of the feed zone refers to the maximum height from the bottom to the top of the feed zone along the vertical direction.

[0091] In some embodiments, the highest draft tube 500 in the feed zone is located at a height of 60-80% of the feed zone. For example, the highest draft tube 500 in the feed zone is located at a height of the feed zone, which includes but is not limited to 60%, 62%, 65%, 67%, 68%, 70%, 73%, 75%, 77%, 78%, 80%, or a range between any two of the aforementioned values.

[0092] In some embodiments, the reaction chamber 101 has a cylindrical structure, and the sleeve 201 has a cylindrical structure.

[0093] In some embodiments, the distance between the inner side wall of the sleeve 201 and the central axis of the reactor 100 is 40-70% of the radius of the reactor 100. For example, the distance between the inner side wall of the sleeve 201 and the central axis of the reactor 100 is 40-70% of the radius of the reactor 100, which includes but is not limited to 40%, 42%, 45%, 47%, 48%, 50%, 53%, 55%, 57%, 58%, 60%, 62%, 65%, 67%, 68%, 70%, or a range between any two of the aforementioned values. That is, the central axis of the sleeve 201 coincides with the central axis of the reactor 100, and the inner diameter of the sleeve 201 is 40-70% of the inner diameter of the reactor 100.

[0094] In some embodiments, the feed port 102 and the discharge port 103 are located at the bottom of the reactor 100, respectively, and the gas outlet 104 is located at the top of the reactor 100.

[0095] In some embodiments, the isolation component 200 further comprises a first partition plate 202 and a second partition plate 203. The first partition plate 202 and the second partition plate 203 are arranged at different heights in the reaction zone.

[0096] In some embodiments, the first partition plate 202 and the second partition plate 203 are connected to the inner side wall of the sleeve 201.

[0097] In some embodiments, the first partition plate 202 and the second partition plate 203 are each independently annular.

[0098] In some embodiments, the first partition plate 202 and the second partition plate 203 are each independently perpendicular to the inner side wall of the sleeve 201.

[0099] In some embodiments, the first partition plate 202 is located above the second partition plate 203 along the height direction.

[0100] In some embodiments, the first partition plate 202 is located at a position of 50% to 70% of the height of the reaction zone.

[0101] In some embodiments, the second partition plate 203 is located at a position of 20% to 40% of the height of the reaction zone.

[0102] In some embodiments, the width of the first partition plate 202 is equal to the width of the second partition plate 203 along the direction of advancement of the polyester raw material.

[0103] In some embodiments, the isolation component 200 further comprises a flow guide plate 204, which is arranged in the reaction zone and connected to the inner side wall of the sleeve 201.

[0104] In some embodiments, the flow guide plate 204 is located between the first partition plate 202 and the second partition plate 203.

[0105] In some embodiments, the flow guide plate 204 is annular.

[0106] In some embodiments, the width of the flow guide plate 204 is smaller than the width of the first partition plate 202 along the direction of advancement of the polyester raw material.

[0107] In some embodiments, the stirring component 300 comprises a stirring shaft 301, a stirring paddle, and a stirring driving component 304, one end of the stirring shaft 301 extends into the reaction zone, the stirring paddle is connected to the stirring shaft 301, and the stirring driving component 304 is installed on the reactor 100 and connected to the stirring shaft 301, and the stirring driving component 304 is used to drive the stirring shaft 301 to rotate to drive the stirring paddle to rotate.

[0108] In some embodiments, the stirring paddle comprises a spaced apart paddle stirring paddle 302 and a propelling stirring paddle 303.

[0109] In some embodiments, the paddle stirring paddle 302 is located above the propelling stirring paddle 303 along the height direction.

[0110] In some embodiments, the paddle agitator 302 is located at a height of 45% to 55% of the reaction zone along the height direction. For example, the paddle agitator 302 is located at a height of 45%, 47%, 48%, 50%, 53%, 55%, or a range between any two of the aforementioned values, of the reaction zone along the height direction. It is noted that the height of the reaction zone refers to the maximum height from the bottom to the top of the reaction zone along the vertical direction.

[0111] In some embodiments, the propeller agitator 303 is located at a height of 10% to 20% of the reaction zone along the height direction. For example, the propeller agitator 303 is located at a height of 10%, 12%, 15%, 18%, 19%, 20%, or a range between any two of the aforementioned values, of the reaction zone along the height direction.

[0112] In some embodiments, the paddle agitator 302 is located between the first partition plate 202 and the second partition plate 203 along the height direction.

[0113] In some embodiments, the propeller agitator 303 is located below the second partition plate 203 along the height direction.

[0114] In some embodiments, the temperature control component 400 comprises a heating coil 401, which is arranged in the reaction zone.

[0115] In some embodiments, the temperature control component 400 further comprises an insulation layer 402, which is connected to the outer wall of the reactor 100.

[0116] In some embodiments, the polyester reaction device 10 can further comprise a vacuum system according to actual needs, which is used to control and maintain the vacuum degree and to remove light components. The vacuum system is not shown in the drawings.

[0117] In some embodiments, the polyester reaction device 10 can further comprise a circulating water system according to actual needs. The circulating water system is used to cool the agitator motor and the like. The circulating water system is not shown in the drawings.

[0118] An embodiment of the present application provides a polyester reaction method.

[0119] A polyester reaction method comprises the following steps:

[0120] The polyester raw material is mixed by first direction stirring and second direction stirring; the temperature during mixing is controlled to be 150-300°C, and the pressure during mixing is controlled to be 0.03-0.3 MPaA. For example, the temperature during mixing can be controlled to be 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, 210°C, 220°C, 230°C, 240°C, 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, or a range between any two of the foregoing. For example, the pressure during mixing can be controlled to be 0.03 MPaA, 0.05 MPaA, 0.08 MPaA, 0.1 MPaA, 0.12 MPaA, 0.15 MPaA, 0.18 MPaA, 0.2 MPaA, 0.23 MPaA, 0.25 MPaA, 0.27 MPaA, 0.29 MPaA, 0.3 MPaA, or a range between any two of the foregoing.

[0121] It should be noted that the polyester raw material can be mixed by first direction stirring and second direction stirring, or by second direction stirring and first direction stirring, or by first direction stirring and second direction stirring simultaneously.

[0122] In some embodiments, the first direction is the forward direction of the polyester raw material, and the second direction is the direction intersecting the forward direction of the polyester raw material. For example, the first direction is the axial direction, and the second direction is the radial direction perpendicular to the axial direction or the inclined direction with a certain angle.

[0123] In some embodiments, the temperature during mixing is controlled to be 230-270°C.

[0124] In some embodiments, the pressure during mixing is controlled to be 0.1-0.2 MPaA.

[0125] In some embodiments, the stirring speed during first direction stirring is controlled to be 10-100 rpm. For example, the stirring speed during first direction stirring can be controlled to be 10 rpm, 20 rpm, 30 rpm, 40 rpm, 50 rpm, 60 rpm, 70 rpm, 80 rpm, 90 rpm, 100 rpm, or a range between any two of the foregoing.

[0126] In some embodiments, the stirring speed during first direction stirring is controlled to be 30-70 rpm.

[0127] In some embodiments, the stirring speed is controlled to be in a range from 10 rpm to 100 rpm when stirring along the second direction. For example, the stirring speed when stirring along the second direction is controlled to be in a range including, but not limited to: 10 rpm, 20 rpm, 30 rpm, 40 rpm, 50 rpm, 60 rpm, 70 rpm, 80 rpm, 90 rpm, 100 rpm, or a range between any two of the foregoing.

[0128] In some embodiments, the stirring speed is controlled to be in a range from 30 rpm to 70 rpm when stirring along the second direction.

[0129] In some embodiments, the polyester feedstock includes a diacid and / or its corresponding dimethyl ester and a diol, the diacid and / or its corresponding dimethyl ester is selected from C4-C20 diacid and / or its corresponding dimethyl ester, and the diol is selected from C2-C20 aliphatic diol and / or aromatic diol.

[0130] In some embodiments, the diacid and / or its corresponding dimethyl ester includes one or more of succinic acid, adipic acid, terephthalic acid, isophthalic acid, phthalic acid, diphenic acid, naphthalic acid, furandicarboxylic acid, thiophenedicarboxylic acid, and cyclohexanedicarboxylic acid.

[0131] In some embodiments, the diacid and / or its corresponding dimethyl ester includes one or more of succinic acid, adipic acid, and terephthalic acid.

[0132] In some embodiments, the diol includes one or more of 1,4-cyclohexanedimethanol, 2,2,4,4-tetramethyl-1,3-cyclobutanediol, isosorbide, ethylene glycol, neopentyl glycol, 1,3-propanediol, 2-methyl-1,3-propanediol, 1,2-propanediol, 1,4-butanediol, 2,3-butanediol, 1,2-pentanediol, 1,4-pentanediol, 1,5-pentanediol, 3-methyl 1,5-pentanediol, 2,2,4-trimethyl-1,3-pentanediol, diethylene glycol, 1,6-hexanediol, 1,8-octanediol, 1,10-decanediol, spiro glycol, and tricyclodecane dimethanol.

[0133] In some embodiments, the diol includes one or more of neopentyl glycol, 1,4-cyclohexanedimethanol, and 2,2,4,4-tetramethyl-1,3-cyclobutanediol.

[0134] In some embodiments, the polyester feedstock is controlled to have a feed temperature of 150°C to 300°C. For example, the polyester feedstock can have a feed temperature having a value selected from the group consisting of 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, 210°C, 220°C, 230°C, 240°C, 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, and a range between any two of the foregoing.

[0135] In some embodiments, the polyester feedstock is controlled to have a feed temperature of 230°C to 270°C.

[0136] In some embodiments, the polyester feedstock is controlled to have a feed flow rate of 5000 Kg / h to 20000 Kg / h. For example, the polyester feedstock can have a feed flow rate having a value selected from the group consisting of 5000 Kg / h, 6000 Kg / h, 7000 Kg / h, 8000 Kg / h, 9000 Kg / h, 10000 Kg / h, 11000 Kg / h, 12000 Kg / h, 13000 Kg / h, 14000 Kg / h, 15000 Kg / h, 16000 Kg / h, 17000 Kg / h, 18000 Kg / h, 19000 Kg / h, 20000 Kg / h, and a range between any two of the foregoing.

[0137] In some embodiments, the polyester feedstock is controlled to have a feed flow rate of 8000 Kg / h to 15000 Kg / h.

[0138] In some embodiments, the polyester feedstock is controlled to have a feed alcohol acid ratio / alcohol ester ratio of 1.10:1 to 1.25:1. For example, the polyester feedstock can have a feed alcohol acid ratio / alcohol ester ratio having a value selected from the group consisting of 1.10:1, 1.11:1, 1.12:1, 1.13:1, 1.14:1, 1.15:1, 1.16:1, 1.17:1, 1.18:1, 1.19:1, 1.20:1, 1.21:1, 1.22:1, 1.23:1, 1.24:1, 1.25:1, and a range between any two of the foregoing.

[0139] In some embodiments, the polyester feedstock is controlled to have a feed flow rate of 1.15:1 to 1.20:1.

[0140] In some embodiments, the residence time during polyester raw material mixing is controlled to be 50 min to 500 min. For example, the value of the residence time during polyester raw material mixing includes, but is not limited to: 50 min, 60 min, 80 min, 100 min, 120 min, 150 min, 180 min, 200 min, 230 min, 250 min, 280 min, 300 min, 300 min, 350 min, 380 min, 400 min, 420 min, 450 min, 470 min, 500 min, or any range between the foregoing.

[0141] In some embodiments, the residence time during polyester raw material mixing is controlled to be 60 min to 200 min.

[0142] In some embodiments, the polyester reaction method employs the polyester reaction apparatus described in any of the above embodiments.

[0143] Example 1

[0144] This embodiment provides a polyester reaction method.

[0145] The polyester reaction method in this embodiment adopts... Figure 1 The polyester reaction apparatus 10 shown has a sleeve 201 positioned in the reaction chamber 101 at a distance of 60% of the radius of the reaction chamber 101 from its central axis. The top of the sleeve 201 is located at 70% of the height of the reaction chamber 101. The feed zone is equipped with five guide trays 500, with the lowest guide tray 500 located at 30% of the overall height of the feed zone and the highest guide tray 500 located at 60% of the overall height of the feed zone. The inner wall of the sleeve 201 is provided with a first partition plate 202 and a second partition plate 203. The first partition plate 202 and the second partition plate 203 are both perpendicular to the inner wall of the sleeve 201. The first partition plate 202 is located at 60% of the height of the reaction zone, and the second partition plate 203 is located at 30% of the height of the reaction zone. The guide plate 204 is located in the area between the first partition plate 202 and the second partition plate 203. The stirring shaft 301 passes through the first partition plate 202 and the second partition plate 203 and extends to the area below the second partition plate 203. The paddle-type stirring paddle 302 is located at 50% of the height of the reaction zone, and the propeller-type stirring paddle 303 is located at 15% of the height of the reaction zone.

[0146] The polyester reaction method in this embodiment specifically includes the following steps:

[0147] S10. Adjust the pressure inside the reaction chamber 101 to 0.15 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0148] The temperature inside the reaction chamber 101 is adjusted to 250℃ by the heating coil 401 and the inner sleeve 201 of the temperature control component 400.

[0149] The stirring driving component 304 of the stirring component 300 is controlled to drive the stirring shaft 301 to rotate, and the rotating speed of the stirring shaft 301 is adjusted to 30 rpm.

[0150] S20, the polyester raw material composed of the dibasic acid succinic acid and the dibasic alcohol 1,4-cyclohexanedimethanol is transported from the feed inlet 102 at the bottom of the reactor 100 to the feed zone, the feed temperature of the polyester raw material is 250℃, the feed flow rate is 10000 Kg / h, and the alcohol-acid ratio of the feed is 1.15:1. The polyester raw material passes through the multi-stage flow guide tower plate 500 in the feed zone, and advances to the reaction zone in a circuitous manner, and enters the area between the first partition plate 202 and the second partition plate 203 under the action of gravity. In the area between the first partition plate 202 and the second partition plate 203, radial full mixing is realized under the stirring action of the paddle stirring paddle 302. The residence time of the polyester raw material in the reactor 100 (including the feed zone and the reaction zone) is controlled to be 180 min.

[0151] The polyester raw material flows to the area below the second partition plate 203 along the gap between the stirring shaft 301 and the second partition plate 203 under the action of gravity, and in this area, the polyester raw material realizes axial full mixing under the stirring action of the propeller stirring paddle 303, and finally the esterification product is obtained through the discharge port 103.

[0152] After measurement, the esterification rate of the polyester product of the embodiment is shown in Table 1.

[0153] Example 2

[0154] The embodiment provides a polyester reaction method.

[0155] The polyester reaction method of the embodiment adopts the same polyester reaction device 10 as in Example 1, and the polyester reaction method of the embodiment is basically the same as in Example 1.

[0156] The polyester reaction method of the embodiment specifically includes the following steps:

[0157] S10, the pressure inside the reaction chamber 101 is adjusted to 0.15 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0158] The temperature inside the reaction chamber 101 is adjusted to 260℃ by the heating coil 401 and the inner sleeve 201 of the temperature control component 400.

[0159] The stirring driving component 304 of the stirring component 300 is controlled to drive the stirring shaft 301 to rotate, and the rotating speed of the stirring shaft 301 is adjusted to 30 rpm.

[0160] S20, the polyester raw material composed of the dibasic acid hexanedioic acid and the dibasic alcohol 2,2,4,4-tetramethyl-1,3-cyclobutanediol is transported from the feed inlet 102 at the bottom of the reactor 100 to the feed zone, the feed temperature of the polyester raw material is 260℃, the feed flow rate is 10000 Kg / h, and the alcohol-acid ratio of the feed is 1.15:1. The polyester raw material passes through the multi-stage flow guide tray 500 in the feed zone, and advances to the reaction zone in a circuitous manner, and enters the area between the first partition plate 202 and the second partition plate 203 under the action of gravity. In the area between the first partition plate 202 and the second partition plate 203, radial complete mixing is realized under the stirring action of the paddle stirring shaft 302. The residence time of the polyester raw material in the reactor 100 (including the feed zone and the reaction zone) is controlled to be 180 min.

[0161] The polyester raw material flows to the area below the second partition plate 203 under the action of gravity along the gap between the stirring shaft 301 and the second partition plate 203, and in this area, axial complete mixing is realized under the stirring action of the propeller stirring shaft 303, and finally the esterification product is discharged through the discharge port 103.

[0162] It is measured that the esterification rate of the polyester product of the embodiment is shown in Table 1.

[0163] Example 3

[0164] The embodiment provides a polyester reaction method.

[0165] The polyester reaction method of the embodiment adopts the same polyester reaction device 10 as that of Example 1, and the polyester reaction method of the embodiment is basically the same as that of Example 1.

[0166] The polyester reaction method of the embodiment specifically includes the following steps:

[0167] S10, the pressure inside the reaction chamber 101 is adjusted to 0.15 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0168] The temperature inside the reaction chamber 101 is adjusted to 250℃ through the heating coil 401 and the inner sleeve 201 of the temperature control component 400.

[0169] The stirring driving component 304 of the stirring component 300 is controlled to drive the stirring shaft 301 to rotate, and the rotating speed of the stirring shaft 301 is adjusted to 40 rpm.

[0170] S20, polyester raw material composed of binary acid terephthalic acid and binary alcohol ethylene glycol is transported from the feed inlet 102 at the bottom of the reactor 100 to the feed area, the feed temperature of the polyester raw material is 250℃, the feed flow rate is 10000 Kg / h, and the alcohol-acid ratio is 1.15:1. The polyester raw material passes through the multi-stage flow guide tray 500 in the feed area, and advances to the reaction area in a circuitous manner, and enters the area between the first partition plate 202 and the second partition plate 203 under the action of gravity. In the area between the first partition plate 202 and the second partition plate 203, radial full mixing is realized under the stirring action of the paddle stirring paddle 302. The residence time of the polyester raw material in the reactor 100 (including the feed area and the reaction area) is controlled to be 180 min.

[0171] The polyester raw material flows to the area below the second partition plate 203 under the action of gravity along the gap between the stirring shaft 301 and the second partition plate 203, and in this area, the polyester raw material realizes axial full mixing under the stirring action of the propeller stirring paddle 303, and finally the esterification product is discharged through the discharge port 103.

[0172] Through measurement, the esterification rate of the polyester product of the embodiment is shown in Table 1.

[0173] Example 4

[0174] The embodiment provides a polyester reaction method.

[0175] The polyester reaction method of the embodiment adopts the same polyester reaction device 10 as that of Example 1, and the polyester reaction method of the embodiment is basically the same as that of Example 1.

[0176] The polyester reaction method of the embodiment specifically includes the following steps:

[0177] S10, the pressure inside the reaction chamber 101 is adjusted to 0.15 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0178] The temperature inside the reaction chamber 101 is adjusted to 260℃ through the heating coil 401 and the inner sleeve 201 of the temperature control component 400.

[0179] The stirring driving component 304 of the stirring component 300 is controlled to drive the stirring shaft 301 to rotate, and the rotating speed of the stirring shaft 301 is adjusted to 40 rpm.

[0180] S20. A polyester feedstock composed of phthalic acid, biphenyl phthalic acid, and neopentyl glycol in a 1:1 mass ratio of dicarboxylic acid and sodium pentyl glycol is fed into the feed zone from the inlet 102 at the bottom of reactor 100. The feed temperature of the polyester feedstock is 260℃, the feed flow rate is 10000 kg / h, and the feed alcohol-acid ratio is 1.15:1. The polyester feedstock passes through the multi-stage guide tray 500 in the feed zone and advances into the reaction zone in a circuitous manner. Under the action of gravity, it enters the area located between the first partition plate 202 and the second partition plate 203. In the area between the first partition plate 202 and the second partition plate 203, radial mixing is achieved by the stirring action of the paddle agitator 302. The residence time of the polyester feedstock in reactor 100 (including the feed zone and the reaction zone) is controlled to be 180 min.

[0181] Under the action of gravity, the polyester raw material flows along the gap between the stirring shaft 301 and the second partition plate 203 to the area below the second partition plate 203. In this area, the polyester raw material is fully mixed axially under the stirring action of the propulsion stirring paddle 303, and finally the esterified product is discharged through the discharge port 103.

[0182] The esterification rate of the polyester product in this embodiment is shown in Table 1 after measurement.

[0183] Example 5

[0184] This embodiment provides a polyester reaction method.

[0185] The polyester reaction method in this embodiment uses the same polyester reaction apparatus 10 as in Example 1, and the polyester reaction method in this embodiment is basically the same as in Example 1.

[0186] The polyester reaction method in this embodiment specifically includes the following steps:

[0187] S10. Adjust the pressure inside the reaction chamber 101 to 0.1 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0188] The temperature inside the reaction chamber 101 is adjusted to 250°C by the heating coil 401 and inner sleeve 201 of the temperature control component 400.

[0189] The stirring drive component 304 of the stirring component 300 drives the stirring shaft 301 to rotate and adjusts the speed of the stirring shaft 301 to 30 rpm.

[0190] S20, the polyester raw material composed of the binary acid furandicarboxylic acid and the binary alcohol 1,4-pentanediol is transported from the feed inlet 102 at the bottom of the reactor 100 to the feed zone, the feed temperature of the polyester raw material is 250℃, the feed flow rate is 10000 Kg / h, and the alcohol-acid ratio of the feed is 1.15:1. The polyester raw material passes through the multi-stage flow guide tray 500 in the feed zone, and advances to the reaction zone in a circuitous manner, and enters the area between the first partition plate 202 and the second partition plate 203 under the action of gravity. In the area between the first partition plate 202 and the second partition plate 203, radial full mixing is realized under the stirring action of the paddle stirring shaft 302. The residence time of the polyester raw material in the reactor 100 (including the feed zone and the reaction zone) is controlled to be 180 min.

[0191] The polyester raw material flows to the area below the second partition plate 203 along the gap between the stirring shaft 301 and the second partition plate 203 under the action of gravity, and in this area, axial full mixing is realized under the stirring action of the push-type stirring shaft 303, and finally the esterification product is discharged through the discharge port 103.

[0192] Through measurement, the esterification rate of the polyester product of the embodiment is shown in Table 1.

[0193] Example 6

[0194] The embodiment provides a polyester reaction method.

[0195] The polyester reaction method of the embodiment adopts the same polyester reaction device 10 as that of Example 1, and the polyester reaction method of the embodiment is basically the same as that of Example 1.

[0196] The polyester reaction method of the embodiment specifically includes the following steps:

[0197] S10, the pressure inside the reaction chamber 101 is adjusted to 0.1 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0198] The temperature inside the reaction chamber 101 is adjusted to 260℃ through the heating coil 401 and the inner sleeve 201 of the temperature control component 400.

[0199] The stirring driving component 304 of the stirring component 300 is controlled to drive the stirring shaft 301 to rotate, and the rotating speed of the stirring shaft 301 is adjusted to 30 rpm.

[0200] S20, the polyester raw material composed of binary acid thiophene dimethyl acid and binary alcohol 2, 2, 4-trimethyl-1, 3-pentanediol is transported from the feed inlet 102 at the bottom of the reactor 100 to the feed zone, the feed temperature of the polyester raw material is 260℃, the feed flow rate is 10000 Kg / h, and the alcohol-acid ratio of the feed is 1.15:1. The polyester raw material passes through the multi-stage flow guide tray 500 of the feed zone, and advances to the reaction zone in a circuitous manner, and enters the area between the first partition plate 202 and the second partition plate 203 under the action of gravity. In the area between the first partition plate 202 and the second partition plate 203, radial full mixing is realized under the stirring action of the paddle stirring paddle 302. The residence time of the polyester raw material in the reactor 100 (including the feed zone and the reaction zone) is controlled to be 180 min.

[0201] The polyester raw material flows to the area below the second partition plate 203 under the action of gravity along the gap between the stirring shaft 301 and the second partition plate 203, and in this area, the polyester raw material realizes axial full mixing under the stirring action of the propeller stirring paddle 303, and finally the esterification product is discharged through the discharge port 103.

[0202] Through measurement, the esterification rate of the polyester product of the embodiment is shown in Table 1.

[0203] Example 7

[0204] The embodiment provides a polyester reaction method.

[0205] The polyester reaction method of the embodiment adopts the same polyester reaction device 10 as that of Example 1, and the polyester reaction method of the embodiment is basically the same as that of Example 1.

[0206] The polyester reaction method of the embodiment specifically includes the following steps:

[0207] S10, the pressure inside the reaction chamber 101 is adjusted to 0.1 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0208] The temperature inside the reaction chamber 101 is adjusted to 250℃ through the heating coil 401 and the inner sleeve 201 of the temperature control component 400.

[0209] The stirring driving component 304 of the stirring component 300 is controlled to drive the stirring shaft 301 to rotate, and the rotating speed of the stirring shaft 301 is adjusted to 40 rpm.

[0210] S20, the polyester raw material composed of dimethyl naphthalene dicarboxylate, dihydric alcohol diethylene glycol is transported from the feed inlet 102 at the bottom of the reactor 100 to the feed zone, the feed temperature of the polyester raw material is 250℃, the feed flow rate is 10000 Kg / h, and the alcohol-ester ratio of the feed is 1.15:1. The polyester raw material passes through the multi-stage flow guide tray 500 in the feed zone, and advances to the reaction zone in a circuitous manner, and enters the area between the first partition plate 202 and the second partition plate 203 under the action of gravity. In the area between the first partition plate 202 and the second partition plate 203, radial complete mixing is realized under the stirring action of the paddle stirring shaft 302. The residence time of the polyester raw material in the reactor 100 (including the feed zone and the reaction zone) is controlled to be 180 min.

[0211] The polyester raw material flows to the area below the second partition plate 203 along the gap between the stirring shaft 301 and the second partition plate 203 under the action of gravity, and in this area, axial complete mixing is realized under the stirring action of the push-type stirring shaft 303, and finally the transesterification product is obtained through the discharge port 103.

[0212] Through measurement, the transesterification rate of the polyester product of the embodiment is shown in Table 1.

[0213] Example 8

[0214] The embodiment provides a polyester reaction method.

[0215] The polyester reaction method of the embodiment adopts the same polyester reaction device 10 as that of Example 1, and the polyester reaction method of the embodiment is basically the same as that of Example 1.

[0216] The polyester reaction method of the embodiment specifically includes the following steps:

[0217] S10, the pressure inside the reaction chamber 101 is adjusted to 0.1 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0218] The temperature inside the reaction chamber 101 is adjusted to 260℃ through the heating coil 401 and the inner sleeve 201 of the temperature control component 400.

[0219] The stirring driving component 304 of the stirring component 300 is controlled to drive the stirring shaft 301 to rotate, and the rotating speed of the stirring shaft 301 is adjusted to 40 rpm.

[0220] S20, the polyester raw material composed of dimethyl cyclohexane dimethylate, dihydric alcohol 1,6-hexanediol is transported from the feed inlet 102 at the bottom of the reactor 100 to the feed zone, the feed temperature of the polyester raw material is 260℃, the feed flow rate is 10000 Kg / h, and the alcohol-ester ratio of the feed is 1.15:1. The polyester raw material passes through the multi-stage flow guide tray 500 in the feed zone, and advances to the reaction zone in a circuitous manner, and enters the area between the first partition plate 202 and the second partition plate 203 under the action of gravity. In the area between the first partition plate 202 and the second partition plate 203, radial complete mixing is realized under the stirring action of the paddle stirring shaft 302. The residence time of the polyester raw material in the reactor 100 (including the feed zone and the reaction zone) is controlled to be 180 min.

[0221] The polyester raw material flows to the area below the second partition plate 203 along the gap between the stirring shaft 301 and the second partition plate 203 under the action of gravity, and in the area, axial complete mixing is realized under the stirring action of the propeller stirring shaft 303, and finally the ester exchange product is obtained through the discharge outlet 103.

[0222] Through measurement, the ester exchange rate of the polyester product of the embodiment is shown in Table 1.

[0223] Comparative Example 1

[0224] The comparative example provides a polyester reaction method.

[0225] The polyester reaction method of the comparative example adopts a polyester reaction device 10 which is basically the same as that of Example 4, wherein the polyester reaction device 10 in Comparative Example 1 does not contain the sleeve 201 and the first partition plate 202, the second partition plate 203 and the flow guide plate 204 connected on the sleeve 201. The stirring shaft 301 is only provided with the propeller stirring shaft 303, which is located at the position of 15% of the height of the reaction zone.

[0226] The polyester reaction method of the comparative example specifically includes the following steps:

[0227] S10, the pressure inside the reaction chamber 101 is adjusted to 0.15 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0228] The temperature inside the reaction chamber 101 is adjusted to 260℃ through the heating coil 401 of the temperature control component 400 and the inner sleeve 201.

[0229] The stirring driving component 304 of the stirring component 300 is controlled to drive the stirring shaft 301 to rotate, and the rotating speed of the stirring shaft 301 is adjusted to 40 rpm.

[0230] S20, the polyester raw material composed of phthalic acid, diphenyl dicarboxylic acid and dihydric alcohol neopentyl glycol with a mass ratio of 1:1:1 is transported from the feed inlet 102 at the bottom of the reactor 100 to the reaction chamber 101, the polyester raw material feed temperature is 260℃, the feed flow rate is 10000 Kg / h, and the feed alcohol acid ratio is 1.15:1. The polyester raw material is fully mixed in the axial direction under the stirring action of the pusher stirring paddle 303, and finally the esterification product is discharged through the discharge port 103.

[0231] The esterification rate of the polyester product of the embodiment is shown in Table 1.

[0232] Comparative Example 2

[0233] The comparative example provides a polyester reaction method.

[0234] The polyester reaction method of the comparative example uses a polyester reaction device 10 substantially the same as that of Example 4, wherein the polyester reaction device 10 in Comparative Example 2 does not contain the sleeve 201 and the first partition plate 202, the second partition plate 203 and the flow guide plate 204 connected on the sleeve 201. The stirring adopts bubble stirring vertical full-mixing flow stirring.

[0235] The polyester reaction method of the comparative example specifically includes the following steps:

[0236] S10, the pressure inside the reaction chamber 101 is adjusted to 0.15 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0237] The temperature inside the reaction chamber 101 is adjusted to 260℃ through the heating coil 401 of the temperature control component 400 and the inner sleeve 201.

[0238] S20, the polyester raw material composed of phthalic acid, diphenyl dicarboxylic acid and dihydric alcohol neopentyl glycol with a mass ratio of 1:1:1 is transported from the feed inlet 102 at the bottom of the reactor 100 to the reaction chamber 101, the polyester raw material feed temperature is 260℃, the feed flow rate is 10000 Kg / h, and the feed alcohol acid ratio is 1.15:1. The polyester raw material is fully mixed under the stirring action of the bubble stirring vertical full-mixing flow stirring, and finally the esterification product is discharged through the discharge port 103.

[0239] The esterification rate of the polyester product of the embodiment is shown in Table 1.

[0240] Comparative Example 3

[0241] The comparative example provides a polyester reaction method.

[0242] The polyester reaction method of the present comparative example uses the same polyester reaction device 10 as that of Example 8, wherein the polyester reaction device 10 in Comparative Example 3 does not contain the sleeve 201 and the first partition plate 202, the second partition plate 203 and the flow guide plate 204 connected on the sleeve 201. The stirring shaft 301 is provided with only the propeller stirring paddle 303, which is located at a position of 15% of the height of the reaction zone.

[0243] The polyester reaction method of the present comparative example specifically includes the following steps:

[0244] S10, adjust the pressure inside the reaction chamber 101 to 0.1 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0245] Adjust the temperature inside the reaction chamber 101 to 260°C through the heating coil 401 of the temperature control component 400 and the inner sleeve 201.

[0246] Control the stirring driving component 304 of the stirring component 300 to drive the stirring shaft 301 to rotate, and adjust the rotating speed of the stirring shaft 301 to 40 rpm.

[0247] S20, feed the polyester raw material composed of dimethyl cyclohexane dicarboxylate and dihydric alcohol 1,6-hexanediol into the reaction chamber 101 from the feed inlet 102 at the bottom of the reactor 100, the feed temperature of the polyester raw material is 260°C, the feed flow rate is 10000 Kg / h, and the alcohol-ester ratio of the feed is 1.15:1. The polyester raw material is fully mixed axially under the stirring action of the propeller stirring paddle 303, and finally the esterification product is discharged through the discharge outlet 103.

[0248] After measurement, the ester exchange rate of the polyester product of the present example is shown in Table 1.

[0249] Comparative Example 4

[0250] The present comparative example provides a polyester reaction method.

[0251] The polyester reaction method of the present comparative example uses the same polyester reaction device 10 as that of Example 8, wherein the polyester reaction device 10 in Comparative Example 4 does not contain the sleeve 201 and the first partition plate 202, the second partition plate 203 and the flow guide plate 204 connected on the sleeve 201. The stirring uses bubbling stirring vertical full-mixing flow stirring.

[0252] The polyester reaction method of the present comparative example specifically includes the following steps:

[0253] S10, adjust the pressure inside the reaction chamber 101 to 0.1 MPaA through the gas phase outlet 104 at the top of the reactor 100.

[0254] The temperature inside the reaction chamber 101 is adjusted to 260℃ by the heating coil 401 of the temperature control component 400 and the inner sleeve 201.

[0255] S20, the polyester raw material composed of dimethyl cyclohexane dimethyl ester and dihydric alcohol 1,6-hexanediol is transported from the feed port 102 at the bottom of the reactor 100 to the reaction chamber 101, the polyester raw material feed temperature is 260℃, the feed flow rate is 10000 Kg / h, and the alcohol-ester ratio of the feed is 1.15:1. The polyester raw material is mixed under the stirring action of the bubbling stirring vertical full-mixing flow stirring, and finally the esterification product is discharged through the discharge port 103.

[0256] After measurement, the ester exchange rate of the polyester product of the embodiment is shown in Table 1.

[0257] Table 1

[0258]

[0259] As can be seen from Table 1, the esterification rate / ester exchange rate of the polyester esterification / ester exchange reactor 100 device provided by the embodiment of the application is superior to the full-mixing flow reactor 100 without a sub-chamber structure design in Comparative Examples 1-4. The esterification rate / ester exchange rate of the polyester esterification / ester exchange reactor 100 device provided by the embodiment of the application is comparable to the product index obtained by the bubbling stirring vertical reactor 100 without a sub-chamber design and mechanical stirring in Comparative Examples 1-4, but compared to the bubbling reactor 100, it requires the addition of excess diol in the early stage, which causes greater energy consumption for recovery. The cost of the application is reduced by 5%-10%.

[0260] The polyester reaction device 10 described above has a short polyester raw material residence time, uniform heating, and can achieve high-efficiency esterification or ester exchange reaction. In the application, the esterification rate / ester exchange rate of the polyester product obtained after the esterification / ester exchange reaction by the polyester reaction device 10 and the method is greater than 95%, and can even be greater than 97%.

[0261] In the above embodiments, the description of each embodiment focuses on different aspects, and the parts not described in detail in a certain embodiment can be referred to the related description of other embodiments.

[0262] Each technical feature of the above-described embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-described embodiments are described, however, as long as the combinations of the technical features do not exist contradictions, they should be considered as the scope of the present disclosure.

[0263] The above-described embodiments are merely illustrative of several embodiments of the present application, which are described in more detail and in a specific manner, but should not be construed as limiting the scope of the patent of the present application. It should be noted that, for those of ordinary skill in the art, several modifications and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the patent of the present application should be subject to the appended claims.

Claims

1. A polyester reaction apparatus characterized by comprising: The application relates to a reactor for preparing polyester, comprising: a reactor having a reaction chamber and a feed inlet, a discharge outlet and a gas phase outlet communicating with the reaction chamber; an isolation component comprising a sleeve arranged in the reaction chamber, the bottom of the sleeve being sealingly connected to the bottom wall of the reaction chamber, the top of the sleeve being spaced apart from the top wall of the reaction chamber, the outer side wall of the sleeve being spaced apart from the inner side wall of the reaction chamber to form a feed area communicating with the feed inlet, the inner side wall of the sleeve and the bottom wall of the reaction chamber forming a reaction area communicating with the discharge outlet and the gas phase outlet; a stirring component installed on the reactor and extending into the reaction area to stir the reaction material in the reaction area along a first direction and a second direction; and a temperature control component for controlling the temperature of the reaction area.

2. The polyester reaction apparatus according to claim 1, characterized by The feed area is provided with annular flow guiding baffles; Optionally, the number of the flow guiding baffles is multiple, and part of the flow guiding baffles are connected to the outer side wall of the sleeve, and the other part of the flow guiding baffles are connected to the inner side wall of the reaction chamber; Further optionally, the flow guiding baffles connected to the outer side wall of the sleeve and the flow guiding baffles connected to the inner side wall of the reaction chamber are distributed in a staggered manner to form flow channels capable of allowing the reaction material to flow in a meandering manner.

3. The polyester reaction apparatus according to claim 2, characterized by At least one of the following conditions is also met: (1) the lowermost flow guiding baffle in the feed area is located at a position of 20% to 30% of the height of the feed area; (2) the uppermost flow guiding baffle in the feed area is located at a position of 60% to 80% of the height of the feed area.

4. The polyester reaction apparatus according to claim 1, characterized by At least one of the following conditions is also met: (1) the reaction chamber has a cylindrical structure, and the sleeve has a cylindrical structure; Optionally, the central axis of the sleeve coincides with the central axis of the reactor, and the inner diameter of the sleeve is 40% to 70% of the inner diameter of the reactor; (2) the feed inlet and the discharge outlet are respectively located at the bottom of the reactor, and the gas phase outlet is located at the top of the reactor.

5. The polyester reaction apparatus according to any one of claims 1 to 4, characterized by The isolation component further comprises a first partition plate and a second partition plate, and the first partition plate and the second partition plate are arranged at different height positions in the reaction area; Optionally, the first partition plate and the second partition plate respectively independently have an annular structure.

6. The polyester reaction apparatus according to claim 5, characterized by At least one of the following conditions is also met: (1) the first partition plate is located at a position of 50% to 70% of the height of the reaction area; (2) the second partition plate is located at a position of 20% to 40% of the height of the reaction area; (3) along the advancing direction of the polyester raw material, the width of the first partition plate is equal to the width of the second partition plate; (4) the isolation component further comprises a flow guiding plate arranged in the reaction area and connected to the inner side wall of the sleeve; Optionally, the flow guiding plate is located between the first partition plate and the second partition plate; Optionally, the flow guiding plate has an annular structure; Optionally, along the advancing direction of the polyester raw material, the width of the flow guiding plate is smaller than the width of the first partition plate.

7. The polyester reaction apparatus according to any one of claims 1 to 4, 6, characterized by The stirring component comprises a stirring shaft, a stirring paddle and a stirring driving component, one end of the stirring shaft extends into the reaction zone, the stirring paddle is connected to the stirring shaft, the stirring driving component is installed on the reactor and connected to the stirring shaft, and the stirring driving component is used to drive the stirring shaft to rotate to drive the stirring paddle to rotate; Optionally, the stirring paddle comprises spaced paddle stirring paddles and propelling stirring paddles; Further optionally, along the height direction, the paddle stirring paddles are located above the propelling stirring paddles; Further optionally, along the height direction, the paddle stirring paddles are located at a position of 45%~55% of the height of the reaction zone; Further optionally, along the height direction, the propelling stirring paddles are located at a position of 10%~20% of the height of the reaction zone.

8. The polyester reaction apparatus according to any one of claims 1 to 4, 6, wherein At least one of the following conditions is also met: (1) The temperature control component comprises a heating coil, and the heating coil is arranged in the reaction zone; (2) The temperature control component further comprises a heat preservation layer, and the heat preservation layer is connected to the outer wall of the reactor.

9. A process for the reaction of a polyester, characterized in that, The method comprises the following steps: The polyester raw material is mixed by first direction stirring and second direction stirring; the temperature during mixing is controlled to be 150℃~300℃, and the pressure during mixing is controlled to be 0.03MPaA~0.3MPaA.

10. The polyester reaction process according to claim 9, characterized in that, At least one of the following conditions is also met: (1) The first direction is the forward direction of the polyester raw material, and the second direction is the direction intersecting the forward direction of the polyester raw material; (2) The temperature during mixing is controlled to be 230℃~270℃; (3) The pressure during mixing is controlled to be 0.1MPaA~0.2MPaA; (4) The stirring speed along the first direction is controlled to be 10rpm~100rpm; Optionally, the stirring speed along the first direction is controlled to be 30rpm~70rpm; (5) The stirring speed along the second direction is controlled to be 10rpm~100rpm; Optionally, the stirring speed along the second direction is controlled to be 30rpm~70rpm; (6) The polyester raw material comprises diacid and / or its corresponding dimethyl ester and dihydric alcohol, the diacid and / or its corresponding dimethyl ester is selected from C4-C20 diacid and / or its corresponding dimethyl ester, and the dihydric alcohol is selected from C2-C20 aliphatic dihydric alcohol and / or aromatic dihydric alcohol; Optionally, the diacid and / or its corresponding dimethyl ester comprises one or more of succinic acid, adipic acid, terephthalic acid, isophthalic acid, phthalic acid, diphenic acid, naphthalic acid, furan dicarboxylic acid, thiophene dicarboxylic acid and cyclohexane dicarboxylic acid; Further optionally, the diacid and / or its corresponding dimethyl ester comprises one or more of succinic acid, adipic acid and terephthalic acid; Optionally, the diol comprises one or more of 1,4-cyclohexanedimethanol, 2,2,4,4-tetramethyl-1,3-cyclobutanediol, isosorbide, ethylene glycol, neopentyl glycol, 1,3-propanediol, 2-methyl-1,3-propanediol, 1,2-propanediol, 1,4-butanediol, 2,3-butanediol, 1,2-pentanediol, 1,4-pentanediol, 1,5-pentanediol, 3-methyl 1,5-pentanediol, 2,2,4-trimethyl-1,3-pentanediol, diethylene glycol, 1,6-hexanediol, 1,8-octanediol, 1,10-decanediol, spirocyclic glycol, and tricyclodecane dimethylol; Further optionally, the diol comprises one or more of neopentyl glycol, 1,4-cyclohexanedimethanol, and 2,2,4,4-tetramethyl-1,3-cyclobutanediol; (7) the feeding temperature of the polyester raw material is controlled to be 150-300°C; Optionally, the feeding temperature of the polyester raw material is controlled to be 230-270°C; (8) the feeding flow rate of the polyester raw material is controlled to be 5000-20000 Kg / h; Optionally, the feeding flow rate of the polyester raw material is controlled to be 8000-15000 Kg / h; (9) the feeding alcohol-acid ratio / alcohol-ester ratio of the polyester raw material is controlled to be 1.10:1-1.25:1; Optionally, the feeding alcohol-acid ratio / alcohol-ester ratio of the polyester raw material is controlled to be 1.15:1-1.20:1; (10) the residence time when the polyester raw material is mixed is controlled to be 50-500 min; Optionally, the residence time when the polyester raw material is mixed is controlled to be 60-200 min; (11) the polyester reaction method uses the polyester reaction device according to any one of claims 1-8.

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