TW201505707A - Autoclave heating jacket - Google Patents

Autoclave heating jacket Download PDF

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Publication number
TW201505707A
TW201505707A TW103113119A TW103113119A TW201505707A TW 201505707 A TW201505707 A TW 201505707A TW 103113119 A TW103113119 A TW 103113119A TW 103113119 A TW103113119 A TW 103113119A TW 201505707 A TW201505707 A TW 201505707A
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TW
Taiwan
Prior art keywords
heating
autoclave
fluid
heating jacket
jacket
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TW103113119A
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Chinese (zh)
Inventor
Leen Monster
Leonardus J Molendijk
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Invista Tech Sarl
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Publication of TW201505707A publication Critical patent/TW201505707A/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002Chemical plants
    • B01J2219/00018Construction aspects
    • B01J2219/00024Revamping, retrofitting or modernisation of existing plants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/0009Coils
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094Jackets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/02Apparatus characterised by their chemically-resistant properties
    • B01J2219/025Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
    • B01J2219/0277Metal based
    • B01J2219/0286Steel
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D1/00Heat-exchange apparatus having stationary conduit assemblies for one heat-exchange medium only, the media being in contact with different sides of the conduit wall, in which the other heat-exchange medium is a large body of fluid, e.g. domestic or motor car radiators
    • F28D1/06Heat-exchange apparatus having stationary conduit assemblies for one heat-exchange medium only, the media being in contact with different sides of the conduit wall, in which the other heat-exchange medium is a large body of fluid, e.g. domestic or motor car radiators with the heat-exchange conduits forming part of, or being attached to, the tank containing the body of fluid
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/0008Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one medium being in heat conductive contact with the conduits for the other medium
    • F28D7/0016Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one medium being in heat conductive contact with the conduits for the other medium the conduits for one medium or the conduits for both media being bent

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

An autoclave heating jacket can include a heating fluid collar, a fluid inlet, a fluid outlet, and a plurality of fluid flow baffles. The heating fluid collar can have an outer wall which includes an upper contact surface and a lower contact surface forming an enclosed chamber when engaged with an outer surface of an autoclave. The fluid inlet can be oriented through the outer wall and is capable of directing a heating fluid into the enclosed chamber. The fluid outlet can be oriented through the outer wall but is capable of directing the heating fluid out of the enclosed chamber. The plurality of fluid flow baffles can be oriented within the enclosed chamber so as to direct the heating fluid along a predetermined pathway within the enclosed chamber.

Description

高壓釜加熱夾套 Autoclave heating jacket

本發明係關於用於高壓釜容器上之加熱夾套,其在循環加熱下很堅固。 This invention relates to heating jackets for use on autoclave vessels which are very strong under cyclic heating.

相較於過去數十年,聚合物使用顯著增加,其至少部分由於可獲得之材料特性的多樣性及與形成複雜形狀相關聯之相對低成本。連續與分批聚合製程可用於多種聚合物生產設施。各製程視如下多種變數而定具有優點及缺點,諸如資金成本、通過量、聚合物類型、聚合動力學及其他優先考慮因素。分批聚合製程通常使用加熱至適當製程溫度之聚合反應器或高壓釜。 The use of polymers has increased significantly over the past few decades due at least in part to the versatility of the material properties available and the relatively low cost associated with the formation of complex shapes. Continuous and batch polymerization processes are available for a variety of polymer production facilities. Each process has advantages and disadvantages depending on various variables such as capital cost, throughput, polymer type, polymerization kinetics, and other priorities. Batch polymerization processes typically employ a polymerization reactor or autoclave that is heated to a suitable process temperature.

該等聚合反應器之加熱通常涉及使用閉合環路加熱系統,其自加熱流體向反應器中傳遞熱。加熱系統可包括外部加熱旋管、內部加熱環路、夾套系統或其他類似熱傳遞系統。該等系統在熱分佈、加熱速率、可靠性及操作限制方面可具有固有侷限性。因此,仍繼續尋找及研究對聚合反應器上該等加熱系統之改良。 Heating of such polymerization reactors typically involves the use of a closed loop heating system that transfers heat from the heated fluid to the reactor. The heating system can include an external heating coil, an internal heating loop, a jacket system, or other similar heat transfer system. These systems can have inherent limitations in terms of heat distribution, heating rate, reliability, and operational constraints. Therefore, improvements in such heating systems on polymerization reactors continue to be sought and studied.

高壓釜加熱夾套可包括加熱流體環、流體進口、流體出口及複數個流體流動擋板。更特定言之,加熱流體環可具有外壁,其包括上接觸表面及下接觸表面,該等表面在與高壓釜之外表面嚙合時形成封閉室。流體進口可經定向以穿過外壁且能夠將加熱流體引導至封閉室 中。類似地,流體出口可經定向以穿過外壁且能夠將加熱流體引導出封閉室。複數個流體流動擋板可定向在封閉室內從而在封閉室內沿預定路徑引導加熱流體。 The autoclave heating jacket can include a heating fluid ring, a fluid inlet, a fluid outlet, and a plurality of fluid flow baffles. More specifically, the heating fluid ring can have an outer wall that includes an upper contact surface and a lower contact surface that form a closed chamber when engaged with the outer surface of the autoclave. The fluid inlet can be oriented to pass through the outer wall and can direct the heating fluid to the enclosed chamber in. Similarly, the fluid outlet can be oriented to pass through the outer wall and can direct the heated fluid out of the enclosed chamber. A plurality of fluid flow baffles can be oriented within the enclosed chamber to direct the heated fluid along a predetermined path within the enclosed chamber.

亦描述具有複合外部加熱組件之聚合高壓釜。聚合高壓釜可包括高壓釜容器體、加熱夾套及加熱管道。高壓釜容器體可具有內部反應室及包括上部及下部之外表面。加熱夾套可附接於下部而形成封閉室。封閉室具有複數個流體流動擋板,其經組態以在封閉室內且圍繞下部沿繚繞路徑引導加熱流體。加熱管道可纏繞且附接於上部。更特定言之,加熱管道可圍繞上部具有多個纏繞物且與加熱夾套流體連接。因此,加熱流體可循環穿過封閉室及加熱管道以向內部反應室中傳遞熱。此外,加熱夾套及加熱管道一起形成複合外部加熱組件。 A polymeric autoclave having a composite external heating assembly is also described. The polymerization autoclave may include an autoclave vessel body, a heating jacket, and a heating pipe. The autoclave vessel body can have an internal reaction chamber and an outer surface including upper and lower portions. The heating jacket can be attached to the lower portion to form a closed chamber. The enclosed chamber has a plurality of fluid flow baffles configured to direct the heating fluid in the enclosed chamber and around the lower portion along the winding path. The heating pipe can be wound and attached to the upper portion. More specifically, the heating conduit can have a plurality of windings around the upper portion and is in fluid connection with the heating jacket. Thus, the heating fluid can be circulated through the enclosed chamber and the heating conduit to transfer heat to the internal reaction chamber. In addition, the heating jacket and the heating conduit together form a composite external heating assembly.

亦揭示且描述一種修復外部加熱旋管附接於外表面之聚合高壓釜的方法。當加熱旋管在高壓釜外表面之一部分中具有變弱或洩漏區段時,該等缺陷可使用本發明方法有效修復。舉例而言,該方法可包括自高壓釜外表面之受影響部分移除加熱旋管之變弱或洩漏區段以使完好加熱旋管區段保留於外表面之各別部分上。可將上述加熱夾套附接於外表面之受影響部分以形成封閉室。可將封閉室與完好加熱旋管區段流體連接。以此方式可藉由提供複合外部加熱組件修復聚合高壓釜。 A method of repairing a polymeric autoclave to which an external heating coil is attached to an outer surface is also disclosed and described. When the heating coil has a weakened or leaking section in one of the outer surfaces of the autoclave, such defects can be effectively repaired using the method of the present invention. For example, the method can include removing a weakened or leaking section of the heating coil from the affected portion of the outer surface of the autoclave to retain the intact heating coil section on a respective portion of the outer surface. The heating jacket described above can be attached to the affected portion of the outer surface to form a closed chamber. The closed chamber can be fluidly coupled to the intact heating coil section. In this way, the polymerization autoclave can be repaired by providing a composite external heating assembly.

100‧‧‧聚合高壓釜 100‧‧‧Polymerized autoclave

102‧‧‧複合外部加熱組件/外部加熱組件/加熱組件 102‧‧‧Composite external heating unit/external heating unit/heating unit

104‧‧‧加熱夾套/高壓釜加熱夾套 104‧‧‧heating jacket/autoclave heating jacket

106‧‧‧高壓釜容器體/容器體 106‧‧‧ autoclave container body/container body

108‧‧‧加熱管道/加熱旋管 108‧‧‧Heating pipe/heating coil

110‧‧‧上部第一進口 110‧‧‧ upper first import

112‧‧‧第二進口 112‧‧‧second import

114‧‧‧放壓閥 114‧‧‧pressure relief valve

116‧‧‧外表面 116‧‧‧ outer surface

118‧‧‧轉變室 118‧‧‧Transition room

120‧‧‧夾套流體進口/流體進口 120‧‧‧ Jacket fluid inlet/fluid inlet

122‧‧‧夾套流體出口/流體出口 122‧‧‧ Jacket fluid outlet / fluid outlet

124‧‧‧轉變管道 124‧‧‧Transformation pipeline

200‧‧‧加熱流體環 200‧‧‧heating fluid ring

202‧‧‧流體流動擋板/下部流動擋板 202‧‧‧Fluid flow baffle / lower flow baffle

204‧‧‧流體流動擋板/上部流動擋板 204‧‧‧Fluid flow baffle / upper flow baffle

206‧‧‧流體流動擋板/分隔擋板 206‧‧‧Fluid flow baffle / partition baffle

208‧‧‧外壁 208‧‧‧ outer wall

210‧‧‧上接觸表面 210‧‧‧Upper contact surface

212‧‧‧下接觸表面 212‧‧‧ lower contact surface

214‧‧‧封閉室 214‧‧‧Closed room

216‧‧‧蛇形流體流動路徑 216‧‧‧ serpentine fluid flow path

218‧‧‧內部彎曲表面 218‧‧‧Internal curved surface

302‧‧‧圓錐形儲集器 302‧‧‧Conical Reservoir

304‧‧‧進口 304‧‧‧Import

306‧‧‧下部/圓錐形下部 306‧‧‧lower/conical lower part

308‧‧‧凸緣 308‧‧‧Flange

310‧‧‧高壓釜出口 310‧‧‧ autoclave outlet

312‧‧‧內部反應室 312‧‧‧Internal reaction room

313‧‧‧第一容器壁 313‧‧‧First container wall

314‧‧‧加熱管 314‧‧‧heat pipe

316‧‧‧共用出口 316‧‧‧share outlet

402‧‧‧第一壁 402‧‧‧ first wall

404‧‧‧內部塗層 404‧‧‧Internal coating

406‧‧‧流體流動路徑 406‧‧‧ fluid flow path

圖1為本發明之一實施例的聚合高壓釜的透視圖;圖2為本發明之一實施例的高壓釜加熱夾套之透視圖,其中部分幻影圖展示經遮蔽內部特徵;圖3為本發明之一實施例的聚合高壓釜之下部的截面剖視圖;圖4為本發明之一實施例的聚合高壓釜的底部剖視圖;且圖5為修復本發明之一實施例的聚合高壓釜的外部加熱系統的方 法的流程圖。 1 is a perspective view of a polymerization autoclave according to an embodiment of the present invention; and FIG. 2 is a perspective view of an autoclave heating jacket according to an embodiment of the present invention, wherein a part of the phantom diagram shows the shading internal features; 1 is a cross-sectional view of a lower portion of a polymerization autoclave of one embodiment of the invention; FIG. 4 is a bottom cross-sectional view of a polymerization autoclave according to an embodiment of the present invention; and FIG. 5 is an external heating of a polymerization autoclave for repairing an embodiment of the present invention. System side Flow chart of the law.

應注意,該等圖僅為本發明若干實施例之例示且從而不欲限制本發明之範疇。 It should be noted that the figures are merely illustrative of several embodiments of the invention and are not intended to limit the scope of the invention.

儘管出於說明之目的以下實施方式含有諸多特異性,但一般技術之人士應瞭解以下細節之多種變化及改變在本文所揭示實施例之範疇內。 While the following embodiments are intended to be illustrative of the specific embodiments of the present invention, it will be understood that

因此,在不會對所主張之任何發明的一般性造成任何損失且不會對所主張之任何發明造成限制的情況下闡述以下實施例。更詳細描述本發明前,應瞭解本發明並不限於所述特定實施例,因為其可進行變化。亦應瞭解,本文所用之術語僅出於描述特定實施例之目的,且不欲進行限制,因為本發明之範疇僅受隨附申請專利範圍限制。除非另外定義,否則本文所用之所有技術及科學術語具有與本發明所屬領域之一般技術者通常所理解相同之含義。 Therefore, the following embodiments are set forth without any loss to the generality of any invention claimed and without any limitation to any claimed invention. Before the present invention is described in more detail, it is to be understood that the invention is not limited to It is also understood that the terminology used herein is for the purpose of describing the particular embodiments, and is not intended to 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 invention belongs, unless otherwise defined.

除非上下文另外明確規定,否則本說明書及隨附申請專利範圍中所用之單數形式「一(a)」、「一(an)」及「該(the)」包括複數指示物。因此,舉例而言,提及「加熱流體」包括複數種該等流體,且「進口」指一或多個該等特徵。 The singular forms "a", "an", "the" and "the" are used in the <RTI ID=0.0> </ RTI> </ RTI> <RTIgt; Thus, for example, reference to "heating fluid" includes a plurality of such fluids, and "import" refers to one or more of such features.

在本發明中,「包含(comprise)」、「包含(comprising)」、「含有(contain)」及「具有(have)」及其類似術語可具有美國專利法中歸於其之含義且可意謂「包括(include)」、「包括(including)」及其類似含義,且一般解釋為開放性術語。術語「由...組成」為封閉式術語且根據美國專利法僅包括特別列出之裝置、方法、組合物、組件、結構、步驟或其類似物。用於本發明所包涵之裝置、方法、組合物、組件、結構、步驟或其類似物的「基本上由...組成(Consisting essentially of)」或「基本上由...組成(consist essentially)」或其類似術語指如本 文所揭示之元件,但其可含有其他結構群組、組成組件、方法步驟等。然而,相較於本文所揭示之相應裝置、組合物、方法等,該等其他裝置、方法、組合物、組件、結構、步驟或其類似物等不會本質上影響該等裝置、組合物、方法等之基本及新穎特徵。更詳細言之,用於本發明所包涵之裝置、方法、組合物、組件、結構、步驟或其類似物的「基本上由...組成(consisting essentially of)」或「基本上由...組成(consist essentially)」或其類似術語具有美國專利法中歸於其之含義,且該術語為開放式的,從而允許所述以外物之存在,只要所述基本或新穎特徵不因所述以外物之存在而變化,但不包括先前技術實施例。當使用開放式術語(如「包含」或「包括」)時,應瞭解亦應直接支持「基本上由...組成」語言以及「由...組成」語言,如同明確說明一般。 In the present invention, "comprise", "comprising", "contain", "have" and the like may have the meaning attributed to them in the U.S. Patent Law and may mean "include", "including" and the like, and are generally interpreted as open terms. The term "consisting of" is a closed term and includes only the specifically listed devices, methods, compositions, components, structures, steps or the like in accordance with the U.S. Patent. "Consisting essentially of" or "consisting essentially of (consist essentially) or "consist essentially" used in the apparatus, method, composition, component, structure, step or the like of the present invention. ) or similar terms The elements disclosed herein, but which may contain other structural groups, component components, method steps, and the like. However, such other devices, methods, compositions, components, structures, steps, or the like, etc., do not materially affect the devices, compositions, etc., as compared to the corresponding devices, compositions, methods, etc. disclosed herein. Basic and novel features of the method and the like. In more detail, "consisting essentially of" or "substantially by:" used in the apparatus, method, composition, component, structure, step or the like of the present invention. "consist essentially" or the like has the meaning attributed to it in the U.S. Patent Law, and the term is open-ended, thereby allowing the existence of the foreign matter as long as the basic or novel features are not The presence of the object varies, but does not include prior art embodiments. When using open-ended terms (such as "contains" or "includes"), it should be understood that the language "consisting essentially of" and "composed of" should be directly supported, as expressly stated.

在合成方法之上下文中,諸如「適合於提供」、「足以引起」或「足以產生」之片語或其類似片語係指與時間、溫度、溶劑、反應物濃度及其類似因素有關之反應條件,對其進行變化以提供有效量或產率之反應產物係在實驗者的一般技能範疇內。所要反應產物不必為唯一反應產物或起始物質不必完全消耗,只要所要反應產物可經分離或以其他方式進一步使用即可。 In the context of a synthetic method, phrases such as "suitable for providing", "sufficient to cause" or "sufficient to produce" or similar phrases refer to reactions related to time, temperature, solvent, reactant concentration and the like. Conditions, variations in which to provide an effective amount or yield of the reaction product are within the general skill of the experimenter. The desired reaction product need not be the only reaction product or the starting material does not have to be completely consumed, as long as the desired reaction product can be isolated or otherwise used further.

應注意,比率、濃度、量及其他數值資料在本文中可以範圍形式表示。應瞭解該範圍形式係出於方便及簡潔之目的而使用,且因此應以靈活方式解釋為不僅包括經明確陳訴為範圍之極限值的數值,而且包括包涵在該範圍內的所有個別數值或子範圍,如同各數值及子範圍包括「約'x'至約'y'」一般。為進行說明,「約0.1%至約5%」之濃度範圍應解釋為不僅包括經明確陳訴之約0.1wt%至約5wt%之濃度,而且包括該指定範圍內之個別濃度(例如1%、2%、3%及4%)及子範圍(例如0.5%、1.1%、2.2%、3.3%及4.4%)。在一實施例中,術語「約」 可包括根據數值之有效數字進行傳統四捨五入。此外,片語「約『x』至『y』」包括「約『x』至約『y』」。 It should be noted that ratios, concentrations, amounts, and other numerical data may be expressed in a range format herein. It is to be understood that the scope of the invention is to be construed as being in a Range, as if each value and sub-range includes "about 'x' to about 'y'". For purposes of illustration, the range of concentrations from "about 0.1% to about 5%" should be interpreted to include not only concentrations from about 0.1% to about 5% by weight that are specifically reported, but also individual concentrations within the specified range (eg, 1%, 2%, 3%, and 4%) and sub-ranges (eg, 0.5%, 1.1%, 2.2%, 3.3%, and 4.4%). In one embodiment, the term "about" This can include traditional rounding based on the effective number of values. In addition, the phrase "about "x" to "y"" includes "about "x" to about "y"".

當提及數值或範圍時,如本文所用之術語「約」允許在該值或範圍中之變化程度,例如規定值或範圍之規定極限值的10%內,或在一個態樣中,5%內。 When referring to a value or range, the term "about" as used herein is intended to mean a degree of variation in the value or range, such as within 10% of the specified limit value of the specified value or range, or 5% in one aspect. Inside.

另外,若本發明之特徵或態樣關於清單或馬庫西群組(Markush group)描述,則熟習此項技術者應認識到從而本發明亦關於馬庫西群組成員之任何個別成員或子群描述。舉例而言,若X描述為選自由溴、氯及碘組成之群,則完整描述X為溴之技術方案及X為溴及氯之技術方案,如同個別列出一般。舉例而言,若本發明之特徵或態樣關於該等清單描述,則熟習此項技術者應認識到從而本發明亦關於清單或馬庫西群組之成員的個別成員或子群子群的任何組合描述。因此,若X經描述為選自由溴、氯及碘組成之群且Y經描述為選自由甲基、乙基及丙基組成之群,則完整描述且支持X為溴且Y為甲基之技術方案。 In addition, if a feature or aspect of the invention is described in relation to a list or a Markush group, those skilled in the art will recognize that the invention also relates to any individual member or member of the Markusi group member. Group description. For example, if X is described as being selected from the group consisting of bromine, chlorine, and iodine, the technical scheme in which X is bromine and the technical scheme in which X is bromine and chlorine are fully described, as listed separately. For example, if features or aspects of the present invention are described in relation to the list, those skilled in the art will recognize that the present invention also relates to individual members or subgroups of members of the list or members of the Markusi group. Any combination description. Thus, if X is described as being selected from the group consisting of bromine, chlorine, and iodine and Y is described as being selected from the group consisting of methyl, ethyl, and propyl, then fully described and supported that X is bromine and Y is methyl. Technical solutions.

除非另外說明,否則如本文所用之組合物之所有百分比係以重量百分比形式給出。除非另外規定,否則在提及組分之溶液時,百分比係指包括溶劑(例如水)之組合物中的重量百分比。 All percentages of the compositions as used herein are given in weight percent unless otherwise indicated. Unless otherwise specified, when referring to a solution of a component, the percentage is meant to be a percentage by weight of the composition including the solvent (eg, water).

如熟習此項技術者在閱讀本發明後顯而易知,在不背離本發明之範疇或精神的情況下,本文所描述且說明之各個別實施例具有分立組件及特徵,其可容易地與任何其他若干實施例之特徵分離或組合。可以所述事件之次序或以邏輯上可能之任何其他次序執行任何所述方法。 The individual embodiments described and illustrated herein have discrete components and features that can be readily associated with those skilled in the art without departing from the scope or spirit of the invention. The features of any other several embodiments are separated or combined. Any of the methods may be performed in the order of the events or in any other order that is logically possible.

除非另外表明,否則本發明之實施例使用之化學、冶金、焊接技術及其類似技術屬於此項技術之技能範圍內。該等技術在文獻中充分說明。 Unless otherwise indicated, the chemical, metallurgical, welding techniques and the like used in embodiments of the present invention are within the skill of the art. These techniques are fully described in the literature.

分批聚合反應通常包括在各個加工階段期間之反覆溫度循環。通常,向高壓釜中饋入聚合反應物且加熱該等材料以足以引發聚合且驅動製程期間之反應。完成後,將該等材料擠出或以其他方式自高壓釜移出。通常亦可在聚合批次之間使用中間清洗及洗滌階段以提供更一致的產品品質。不幸地是,該等製程在高壓釜內沿高壓釜壁及沿相鄰加熱系統(諸如外部加熱旋管)引入顯著溫度循環變化。此外,跨高壓釜及加熱系統之各部分的溫度差可在焊接接頭及相鄰材料處產生機械應力。 Batch polymerization typically involves repeated temperature cycling during various processing stages. Typically, the polymerization reactant is fed into the autoclave and the materials are heated to initiate polymerization and drive the reaction during the process. Upon completion, the materials are extruded or otherwise removed from the autoclave. Intermediate cleaning and washing stages can also be used between polymerization batches to provide a more consistent product quality. Unfortunately, such processes introduce significant temperature cycling changes in the autoclave along the autoclave wall and along adjacent heating systems, such as external heating coils. In addition, temperature differences across the autoclave and various parts of the heating system can create mechanical stresses at the welded joint and adjacent materials.

作為一說明性實例,二價聚醯胺(諸如尼龍6,6)之形成可包括在約189-250℃之高溫下使尼龍鹽與酸反應數小時。高壓釜壁溫最初低於典型加熱流體溫度。尼龍6,6分批製程循環中之溫度及壓力條件包括初始啟動、饋入尼龍鹽、反應階段、擠出階段及清除階段期間的變化。在此等各個階段中,溫度變化在高壓釜壁與加熱旋管之間產生溫度差。 As an illustrative example, the formation of a divalent polyamine (such as nylon 6,6) can include reacting the nylon salt with an acid for several hours at a temperature of about 189-250 °C. The autoclave wall temperature is initially lower than the typical heating fluid temperature. The temperature and pressure conditions in the nylon 6,6 batch process cycle include initial startup, feed to the nylon salt, reaction stage, extrusion stage, and purge stage. During these various stages, the temperature change creates a temperature differential between the autoclave wall and the heating coil.

表1提供循環聚合操作條件之一個實例。 Table 1 provides an example of cyclic polymerization operating conditions.

值得注意地,加熱旋管與高壓釜壁之間的溫度差可隨時間劇烈變化。外部加熱旋管大多數情況下焊接於高壓釜之外表面。在反應器啟動期間,由相對冷之高壓釜壁抑制加熱旋管之膨脹。此產生壓縮負荷,其超過焊縫之彈性變形極限。在隨後加熱高壓釜壁至正常操作溫度時該永久變形在焊接接頭中產生應力。在溫度條件變化(諸如熬煮、蒸汽清洗、洗滌、關閉及啟動反應器)期間產生類似變形。在各 情況下,溫度變化使得產生跨焊縫之溫度梯度。在尼龍6,6生產之情況下,對於標準產量,分批循環時間通常可在約100-120分鐘範圍內。最終,該等反覆溫度差導致外部加熱旋管與高壓釜壁之間的焊接接頭處發生低循環疲勞損傷。該損傷主要在外部加熱旋管之下部遇到,因為加熱流體在下部進口旋管附近最熱,在此處加熱流體溫度最高。因此,在外部加熱旋管下部,加熱旋管與高壓釜外表面之間的溫度差趨向於較大,且在加熱旋管之前一至四個纏繞物內尤其明顯。不幸的是,在破損位置處之點焊可使經包覆容器壁隨時間變弱且在一些情況下可使內部塗層剝離。 Notably, the temperature difference between the heating coil and the wall of the autoclave can vary drastically over time. The external heating coil is welded to the outer surface of the autoclave in most cases. During the start of the reactor, the expansion of the heating coil is inhibited by the relatively cold autoclave wall. This creates a compressive load that exceeds the elastic deformation limit of the weld. This permanent deformation creates stress in the welded joint when the autoclave wall is subsequently heated to normal operating temperatures. Similar deformations occur during changes in temperature conditions, such as cooking, steam cleaning, washing, shutting down, and starting the reactor. In each In this case, the temperature change causes a temperature gradient across the weld. In the case of nylon 6,6 production, the batch cycle time can typically range from about 100 to 120 minutes for standard yields. Eventually, these repeated temperature differences cause low cycle fatigue damage at the welded joint between the external heating coil and the autoclave wall. This damage is primarily encountered at the lower portion of the external heating coil because the heating fluid is hottest near the lower inlet coil where the heating fluid temperature is highest. Therefore, in the lower portion of the externally heated coil, the temperature difference between the heating coil and the outer surface of the autoclave tends to be large, and is particularly noticeable in one to four windings before heating the coil. Unfortunately, spot welding at the location of the breakage can weaken the wall of the coated container over time and in some cases can strip the inner coating.

可使用高壓釜加熱夾套克服該損傷且減少將來由於低循環疲勞所致之破損。圖1說明具有複合外部加熱組件102之聚合高壓釜100,該複合外部加熱組件102整合該加熱夾套104。聚合高壓釜可包括高壓釜容器體106、加熱夾套及加熱管道108。高壓釜容器體可為可在其中執行聚合反應之任何適合容器。一般而言,適合容器體可包括由高壓釜壁包圍且能夠加壓之內部反應室。儘管操作條件可變化,但高壓釜容器體可經改適以保持至少300psia且在一些情況下至少600psia之壓力。圖1之高壓釜容器體展示上部第一進口110、第二進口112及放壓閥114。可使用進口向內部反應室饋入初始反應物、控制壓力及/或引入分級聚合反應物。應注意,如熟習此項技術者所瞭解,不管此等進口及閥等之描述及所示位置,可以不同於由使用者出於任何設計目的而展示之方式使用此等或其他口。 The autoclave heating jacket can be used to overcome this damage and reduce future damage due to low cycle fatigue. 1 illustrates a polymeric autoclave 100 having a composite external heating assembly 102 that incorporates the heating jacket 104. The polymerization autoclave can include an autoclave vessel body 106, a heating jacket, and a heating conduit 108. The autoclave vessel body can be any suitable vessel in which the polymerization reaction can be carried out. In general, a suitable container body can include an internal reaction chamber surrounded by an autoclave wall and capable of pressurization. While the operating conditions may vary, the autoclave vessel body may be adapted to maintain a pressure of at least 300 psia and in some cases at least 600 psia. The autoclave vessel body of Figure 1 shows an upper first inlet 110, a second inlet 112 and a pressure relief valve 114. The inlet can be used to feed the initial reaction to the internal reaction chamber, control the pressure, and/or introduce a graded polymerization reactant. It should be noted that, as will be appreciated by those skilled in the art, regardless of the description and location of such inlets and valves, such or other locations may be used in a manner different than that exhibited by the user for any design purpose.

視情況,高壓釜容器可為經包覆容器,其中第一容器壁塗有一或多個內層。作為一非限制性實例,碳鋼壁可塗有不鏽鋼內層。碳鋼壁可向容器提供第一機械強度,而不鏽鋼內層向在高溫度及壓力下與聚合反應物及產物接觸之容器內表面提供防腐蝕性。其他材料亦可適合於容器壁,諸如(但不限於)碳鋼合金(例如HII碳鋼)、耐火金屬合 金、鉻合金、其複合物及其組合。在一個實例中,容器壁可由鉻-鉬鋼合金(例如16Mo3)或其類似物形成。類似地,內部塗層可為不鏽鋼(例如SS321)或其類似物。 Optionally, the autoclave container can be a coated container wherein the first container wall is coated with one or more inner layers. As a non-limiting example, the carbon steel wall may be coated with a stainless steel inner layer. The carbon steel wall provides a first mechanical strength to the container, while the stainless steel inner layer provides corrosion protection to the inner surface of the container that is in contact with the polymerization reactant and product at high temperatures and pressures. Other materials may also be suitable for the container wall, such as, but not limited to, carbon steel alloys (eg, HII carbon steel), refractory metal Gold, chromium alloys, composites thereof, and combinations thereof. In one example, the vessel wall may be formed from a chromium-molybdenum steel alloy (eg, 16Mo3) or the like. Similarly, the inner coating can be stainless steel (e.g., SS321) or the like.

容器壁厚可變化但一般為約15mm至約50mm,且在多數情況下為約20mm至40mm。在一個實例中,容器壁厚可為24mm碳鋼以及3mm不鏽鋼內部包覆層。加熱管道之相應壁厚亦可影響溫度轉變期間傳遞至加熱旋管之應力的程度。加熱管道壁厚通常小於容器壁厚且一般小於約25mm。在一個實例中,加熱管道壁厚可為約3mm至約6mm,且在一特定實例中為4mm。一般而言,容器壁厚與管道壁厚之比率可為例如約2:1至約15:1,或為約5:1至約9:1。 The wall thickness of the container can vary, but is generally from about 15 mm to about 50 mm, and in most cases from about 20 mm to 40 mm. In one example, the container wall thickness can be 24 mm carbon steel and a 3 mm stainless steel inner cladding. The corresponding wall thickness of the heating conduit can also affect the extent of stress transmitted to the heating coil during temperature transitions. The wall thickness of the heated conduit is typically less than the wall thickness of the vessel and is generally less than about 25 mm. In one example, the heated conduit wall thickness can be from about 3 mm to about 6 mm, and in one particular example is 4 mm. In general, the ratio of the wall thickness of the vessel to the wall thickness of the conduit can be, for example, from about 2:1 to about 15:1, or from about 5:1 to about 9:1.

再次參考圖1,高壓釜容器體106可具有外表面116,其包括上部及下部。加熱夾套104可附接於下部,而加熱管道108可纏繞且附接於上部。術語「上部」及「下部」為相對術語,且並非意指上半部及下半部,僅相對於下部為上部。加熱管道可圍繞上部具有多個纏繞物。纏繞物之數目可顯著變化,但通常超過十個纏繞物,且在一些情況下高達或超過二十個纏繞物。加熱管道之外部寬度可變化,諸如約50mm至約100mm。此外,各纏繞物通常具有小間隙以使得加熱管道之連續纏繞物中間的外表面暴露。該等間隙一般有限以改良向高壓釜之熱傳遞,但大多數情況下限於不超過周圍加熱管道之寬度的50%(且在多數情況下小於20%)。加熱管道可具有多種截面形狀,諸如(但不限於)半管形、全管形、U型通道、V型通道及其類似形狀。加熱管道可與加熱夾套經由適合電偶(諸如轉變室118)流體連接。因此,加熱流體可經由夾套流體進口120引入外部加熱組件102中且穿過加熱夾套循環至夾套流體出口122。轉變管道124可將加熱流體引導至與加熱管道流體連接之轉變室。以此方式,來自加熱流體之熱可傳遞至聚合高壓釜100之內部反應室中以維持所要溫度。儘管可使用多種加熱流 體,但非限制性實例包括Thermanol 66®、DowthermTM及其混合物。 Referring again to Figure 1, the autoclave vessel body 106 can have an outer surface 116 that includes an upper portion and a lower portion. The heating jacket 104 can be attached to the lower portion, while the heating conduit 108 can be wrapped and attached to the upper portion. The terms "upper" and "lower" are relative terms and do not mean the upper and lower halves, but only the upper portion relative to the lower portion. The heating duct can have a plurality of windings around the upper portion. The number of wraps can vary significantly, but typically exceeds ten wraps, and in some cases up to or over twenty wraps. The outer width of the heating conduit can vary, such as from about 50 mm to about 100 mm. In addition, each wrap generally has a small gap to expose the outer surface intermediate the continuous wrap of the heating pipe. These gaps are generally limited to improve heat transfer to the autoclave, but in most cases are limited to no more than 50% (and in most cases less than 20%) the width of the surrounding heating conduit. The heating conduit can have a variety of cross-sectional shapes such as, but not limited to, a semi-tubular shape, a full tubular shape, a U-shaped channel, a V-shaped channel, and the like. The heating conduit can be fluidly coupled to the heating jacket via a suitable galvanic couple, such as transition chamber 118. Thus, the heating fluid can be introduced into the external heating assembly 102 via the jacketed fluid inlet 120 and circulated through the heating jacket to the jacketed fluid outlet 122. The transition conduit 124 can direct the heating fluid to a transition chamber that is fluidly coupled to the heating conduit. In this manner, heat from the heated fluid can be transferred to the internal reaction chamber of the polymerization autoclave 100 to maintain the desired temperature. Although a variety of heating fluid may be used, but non-limiting examples include Thermanol 66®, Dowtherm TM and mixtures thereof.

視情況,加熱夾套可附接於外表面之上部,而加熱管道附接於下部。在另一替代性情形中,多個加熱夾套可串聯附接於外表面。多個加熱夾套可直接彼此連接,或可連接於中間加熱管道以提供交替之加熱夾套-加熱管道組態。加熱夾套及加熱管道可附接於外表面之不同且不重疊部分。加熱夾套及加熱管道各可視所要熱傳遞效能及其他考慮因素而定覆蓋外表面之不同比例。然而,作為普通準則,加熱夾套可覆蓋外表面之3%至40%,而整個加熱組件可通常覆蓋外表面之30%至80%,且通常40%至70%。在許多實施例中,加熱夾套覆蓋外表面之下部且加熱組件一起覆蓋表面之約5%至約30%。關於表面覆蓋率,加熱管道中繞組之間的間隙包括在由各別加熱裝置覆蓋中。 Optionally, the heating jacket can be attached to the upper portion of the outer surface and the heating conduit attached to the lower portion. In another alternative, multiple heating jackets may be attached to the outer surface in series. Multiple heating jackets may be directly connected to one another or may be connected to an intermediate heating conduit to provide an alternating heating jacket-heating conduit configuration. The heating jacket and the heating conduit can be attached to different and non-overlapping portions of the outer surface. The heating jacket and the heating pipe may each cover different proportions of the outer surface depending on the heat transfer efficiency and other considerations. However, as a general rule, the heating jacket can cover from 3% to 40% of the outer surface, while the entire heating assembly can typically cover from 30% to 80% of the outer surface, and typically from 40% to 70%. In many embodiments, the heating jacket covers the lower portion of the outer surface and the heating assembly together covers about 5% to about 30% of the surface. With regard to surface coverage, the gap between the windings in the heating pipe is included in the coverage by the respective heating means.

轉向圖2,相較於高壓釜容器體更詳細地展示高壓釜加熱夾套104。高壓釜加熱夾套可包括加熱流體環200、流體進口120、流體出口122及複數個流體流動擋板202、204及206。更特定言之,加熱流體環可具有外壁208,其包括上接觸表面210及下接觸表面212,該等表面在與高壓釜之外表面嚙合時形成封閉室214。外壁可具有環形形狀,其與高壓釜之外表面互補,從而為封閉室提供實質上環形體積。或者,外壁可具有其他形狀,只要形成封閉室以使加熱流體可沿高壓釜之外表面穿過即可。 Turning to Figure 2, the autoclave heating jacket 104 is shown in more detail than the autoclave vessel body. The autoclave heating jacket can include a heating fluid ring 200, a fluid inlet 120, a fluid outlet 122, and a plurality of fluid flow baffles 202, 204, and 206. More specifically, the heating fluid ring can have an outer wall 208 that includes an upper contact surface 210 and a lower contact surface 212 that form a closed chamber 214 when engaged with the outer surface of the autoclave. The outer wall can have an annular shape that is complementary to the outer surface of the autoclave to provide a substantially annular volume to the enclosed chamber. Alternatively, the outer wall may have other shapes as long as the closed chamber is formed such that the heating fluid can pass through the outer surface of the autoclave.

封閉室包括複數個流體流動擋板,其經組態以在封閉室內沿預定路徑引導加熱流體。可在封閉室內設計繚繞路徑,其圍繞聚合高壓釜之下部流動。繚繞路徑可經排列以使向內部反應室之熱傳遞的非均一性達最小。在圖2中,流體流動擋板包括分隔擋板206,其在封閉室內形成障壁以迫使加熱流體在封閉室中環向流動。加熱夾套之流體進口120及流體出口122可經定向以彼此貼近以使得加熱流體實質上橫穿整個封閉室。流體進口可經定向以穿過外壁208且能夠將加熱流體引 導至封閉室214中。類似地,流體出口可經定向以穿過外壁但能夠將加熱流體引導出封閉室。 The enclosed chamber includes a plurality of fluid flow baffles configured to direct the heated fluid along a predetermined path within the enclosed chamber. A winding path can be designed in the enclosed chamber that flows around the lower portion of the polymerization autoclave. The winding paths can be arranged to minimize non-uniformity of heat transfer to the internal reaction chamber. In FIG. 2, the fluid flow baffle includes a divider baffle 206 that forms a barrier within the enclosed chamber to force a heating fluid to circulate in the enclosed chamber. The fluid inlet 120 and fluid outlet 122 of the heating jacket can be oriented to abut each other such that the heating fluid substantially traverses the entire enclosed chamber. The fluid inlet can be oriented to pass through the outer wall 208 and can direct the heating fluid Guided into the enclosed chamber 214. Similarly, the fluid outlet can be oriented to pass through the outer wall but can direct the heated fluid out of the enclosed chamber.

如所述,可使用多種擋板以沿繚繞路徑引導加熱流體流。擋板可經定向以界定各種繚繞路徑,諸如(但不限於)蛇形流體流動路徑、環向往復流體流動路徑或其類似路徑。舉例而言,交替之上部流動擋板204及下部流動擋板202可獲得蛇形流體流動路徑216。值得注意地,擋板各包括內部彎曲表面218,其與高壓釜容器體之外表面嚙合以迫使流體圍繞各擋板流動。因此,上部流體流動擋板在該等擋板上方保留開放流動路徑,而下部流動擋板在相應擋板下方保留開放流動路徑。儘管該說明展示垂直變化之蛇形流動路徑,但擋板亦可經置放而誘導水平流動變化。可使用多種擋板配置,但複雜及或多種擋板組態可產生過量壓頭。加熱組件內之該壓力增加可能增加在加熱組件內引起破損之機率,需要高壓加熱流體泵及/或增加操作費用。無論如何,使用內部流動擋板提供有效熱傳遞體積且外表面之帶夾套下部的實質表面經覆蓋。該等開放封閉室可提供不均一加熱流體流動路徑。相比之下,加熱管道通常具有均一橫截面積(半管、全管或其類似形狀)。 As noted, a variety of baffles can be used to direct the flow of heated fluid along the winding path. The baffles can be oriented to define various winding paths such as, but not limited to, serpentine fluid flow paths, circumferential reciprocating fluid flow paths, or the like. For example, alternate upper flow baffles 204 and lower flow baffles 202 may obtain a serpentine fluid flow path 216. Notably, the baffles each include an inner curved surface 218 that engages the outer surface of the autoclave container body to force fluid to flow around the baffles. Thus, the upper fluid flow baffle retains an open flow path above the baffles while the lower flow baffle retains an open flow path below the respective baffles. Although the description shows a vertically varying serpentine flow path, the baffle can also be placed to induce a horizontal flow change. A variety of baffle configurations are available, but complex and or multiple baffle configurations can produce excessive heads. This increase in pressure within the heating assembly may increase the probability of causing breakage within the heating assembly, requiring high pressure heating of the fluid pump and/or increased operating costs. In any event, an internal flow baffle is used to provide an effective heat transfer volume and the substantial surface of the lower portion of the outer jacket is covered. The open enclosed chambers provide a non-uniform heating fluid flow path. In contrast, heating pipes typically have a uniform cross-sectional area (semi-tube, full tube, or the like).

圖3說明附接於聚合高壓釜之外表面116的高壓釜加熱夾套104及加熱旋管108。加熱夾套可視情況在加熱環之底部表面中包括排放口300以使得可關閉及/或清洗加熱組件102。如先前所述,加熱夾套可包括上接觸表面210及下接觸表面212,該等表面與高壓釜之外表面116嚙合以一起形成封閉室214。在此實施例中,上接觸表面可為界定環之頂板的環形脊。類似地,下接觸表面可為界定環之底板的環形凸緣。因此,加熱夾套可包括具有環形垂直外壁連接於底板及頂板的環,底板及頂板一起使加熱流體緊靠外表面之下部。 3 illustrates an autoclave heating jacket 104 and a heating coil 108 attached to the outer surface 116 of the polymerization autoclave. The heating jacket may optionally include a vent 300 in the bottom surface of the heating ring to enable closing and/or cleaning of the heating assembly 102. As previously described, the heating jacket can include an upper contact surface 210 and a lower contact surface 212 that engage the outer surface 116 of the autoclave to form a closed chamber 214. In this embodiment, the upper contact surface can be an annular ridge that defines the top plate of the ring. Similarly, the lower contact surface can be an annular flange that defines the bottom plate of the ring. Thus, the heating jacket can include a ring having an annular vertical outer wall joined to the bottom plate and the top plate, the bottom plate and the top plate together bringing the heating fluid against the lower portion of the outer surface.

加熱夾套可由能夠經得起預期操作溫度、條件及反覆溫度循環 之任何適合材料形成。適合材料之非限制性實例包括碳鋼、不鏽鋼、包含鉻-鉬合金之鋼合金(諸如16Mo3及其類似物)及其組合。在一個實例中,加熱夾套可由鉻-鉬鋼合金形成。通常,加熱夾套可使用高溫焊接合金焊接於外表面。適合焊接合金之非限制性實例可包括包含Mn-Mo、W2 Mo、G 46 AM G4MO、E Mo B32 H5及其組合之合金。亦可使用市售焊接合金(亦即填充金屬),諸如(但不限於)Nertalic 86®、Union® I-Mo及SL® 12G。 The heating jacket can be able to withstand the expected operating temperature, conditions and repeated temperature cycling Any suitable material is formed. Non-limiting examples of suitable materials include carbon steel, stainless steel, steel alloys including chromium-molybdenum alloys such as 16Mo3 and the like, and combinations thereof. In one example, the heating jacket can be formed from a chromium-molybdenum steel alloy. Typically, the heating jacket can be welded to the outer surface using a high temperature solder alloy. Non-limiting examples of suitable solder alloys can include alloys comprising Mn-Mo, W2 Mo, G 46 AM G4MO, E Mo B32 H5, and combinations thereof. Commercially available solder alloys (ie, filler metals) such as, but not limited to, Nertalic 86®, Union® I-Mo, and SL® 12G can also be used.

儘管其他類型高壓釜可與加熱組件102一起使用,亦可使用內部加熱歧管。舉例而言,內部加熱歧管可包括具有進口304之圓錐形儲集器302。圓錐形儲集器可置於高壓釜之下部306內,其在凸緣308處附接於容器體106。下部包括高壓釜出口310,其容許自內部反應室312移出產物以供進一步加工(例如擠出、拉製成纖維、模製等)。在一些情況下,下部之壁厚可大於第一容器壁313之壁厚。舉例而言,下部厚度可比第一容器壁厚大約10%至40%。類似地,夾套厚度可比相應加熱管道大10%至40%。夾套之厚度可為約8mm至約25mm,且在一些情況下為10mm至18mm,但可使用其他厚度。舉例而言,加熱夾套之厚度可為12mm或16mm。在另一實例中,外殼壁之厚度可小於頂板及底板厚度。如同加熱管道一般,下部厚度與加熱夾套厚度之比率可為約2:1至約15:1,且在一些情況下為約5:1至約9:1。 While other types of autoclaves can be used with the heating assembly 102, an internal heating manifold can also be used. For example, the internal heating manifold can include a conical reservoir 302 having an inlet 304. A conical reservoir can be placed within the lower portion 306 of the autoclave that is attached to the container body 106 at the flange 308. The lower portion includes an autoclave outlet 310 that allows the product to be removed from the internal reaction chamber 312 for further processing (e.g., extrusion, drawing into fibers, molding, etc.). In some cases, the wall thickness of the lower portion may be greater than the wall thickness of the first container wall 313. For example, the lower thickness can be about 10% to 40% thicker than the first container wall. Similarly, the jacket thickness can be 10% to 40% greater than the corresponding heating pipe. The thickness of the jacket may range from about 8 mm to about 25 mm, and in some cases from 10 mm to 18 mm, although other thicknesses may be used. For example, the thickness of the heating jacket can be 12 mm or 16 mm. In another example, the thickness of the outer casing wall can be less than the thickness of the top and bottom plates. As with heating the conduit, the ratio of the lower thickness to the thickness of the heating jacket can range from about 2:1 to about 15:1, and in some cases from about 5:1 to about 9:1.

內部加熱歧管可進一步包括一或多個加熱管314,其各與圓錐形儲集器流體連接。加熱管可連接(未示)於用於使已冷卻加熱流體再循環及/或再加熱的共用出口316。在另一替代性情況下,聚合高壓釜可為攪動式高壓釜,其包括內部混合器。內部混合器通常可沿內部反應室之中線垂直定向。內部混合器可提高聚合條件之均一性且縮短聚合反應時間。 The internal heating manifold can further include one or more heating tubes 314 each fluidly coupled to the conical reservoir. The heating tube can be connected (not shown) to a common outlet 316 for recirculating and/or reheating the cooled heating fluid. In another alternative, the polymerization autoclave can be an agitated autoclave that includes an internal mixer. Internal mixers are typically oriented vertically along the line in the internal reaction chamber. The internal mixer can increase the homogeneity of the polymerization conditions and shorten the polymerization time.

現參考圖4,聚合高壓釜100之底視圖展示附接於高壓釜容器體 106之高壓釜加熱夾套104。如上所述,容器體經由凸緣308附接於具有高壓釜出口310之圓錐形下部306。在一些情況下,加熱旋管108以直接焊接於容器體之外表面的半管形式形成。如上所述,容器體可為經包覆容器,其包括第一壁402及內部塗層404。 Referring now to Figure 4, a bottom view of the polymerization autoclave 100 is shown attached to the autoclave vessel body. The autoclave of 106 heats the jacket 104. As described above, the container body is attached via flange 308 to a conical lower portion 306 having an autoclave outlet 310. In some cases, the heating coil 108 is formed as a half tube that is welded directly to the outer surface of the container body. As noted above, the container body can be a coated container that includes a first wall 402 and an inner coating 404.

作為加熱組件的一部分,轉變管道124可將流體出口122流體連接於轉變室118中。轉變室則將加熱流體引導流入半管加熱旋管108中,如流體流動路徑406所示。因此,該加熱組件可為複合加熱系統,其在聚合高壓釜之下部有效使用加熱夾套以及更傳統半管加熱旋管而獲得改良效能。 As part of the heating assembly, the transition conduit 124 can fluidly connect the fluid outlet 122 to the transition chamber 118. The transition chamber directs the heated fluid into the half tube heating coil 108 as shown by fluid flow path 406. Thus, the heating assembly can be a composite heating system that effectively uses a heating jacket under the polymerization autoclave and a more conventional half-tube heating coil for improved performance.

上述加熱夾套可有利地用於聚合高壓釜之原始建構。然而,該等加熱夾套可尤其適用於修復及/或改良現有高壓釜之可靠性。因此,圖5展示一種修復外部加熱旋管附接於外表面之聚合高壓釜的方法500。在該等情況下,標準加熱旋管(例如半管管道)可自高壓釜外表面之底部延伸至外表面之上部。通常,該等加熱旋管沿外表面向上纏繞至少一半路徑。無論如何,加熱旋管之部分可能由於低循環疲勞而開始破損。其大多數情況下與旋管之初始部分相關聯,在該等部分處加熱流體為最大(例如在溫度轉變期間溫度差亦為最大時)。當加熱旋管在高壓釜外表面之下部具有變弱或洩漏區段時,該等缺陷可使用本發明方法有效修復。該方法可包括自高壓釜外表面之下部移除加熱旋管之洩漏區段510。加熱旋管之功能部分以完好加熱旋管區段保留於外表面之上部。洩漏區段可使用不會不利地影響容器體或相鄰焊縫或接頭之任何適合技術移除。在一個替代性情況中,洩漏區段可藉由研磨移除。其他機械技術亦可使用,諸如(但不限於)電漿切割、氣炬切割、金屬切割鋸、雷射切割及其類似技術。暴露之外表面隨後可通常進行清洗。清洗可包括一或多個如下步驟:拋光、洗滌、表面處理及表面塗佈。 The heating jacket described above can be advantageously used in the original construction of a polymerization autoclave. However, such heating jackets are particularly useful for repairing and/or improving the reliability of existing autoclaves. Thus, Figure 5 shows a method 500 of repairing a polymeric autoclave to which an external heating coil is attached to an outer surface. In such cases, a standard heating coil (e.g., a half pipe) may extend from the bottom of the outer surface of the autoclave to the upper portion of the outer surface. Typically, the heating coils are wound up at least halfway along the outer surface. In any case, the portion of the heating coil may begin to break due to low cycle fatigue. In most cases it is associated with the initial portion of the coil where the heating fluid is at a maximum (e.g., when the temperature differential is also maximized during temperature transitions). When the heating coil has a weakened or leaking section below the outer surface of the autoclave, such defects can be effectively repaired using the method of the present invention. The method can include removing a leak section 510 of the heating coil from below the outer surface of the autoclave. The functional portion of the heating coil remains in the upper portion of the outer surface with the intact heating coil section. The leaking section can be removed using any suitable technique that does not adversely affect the container body or adjacent welds or joints. In an alternative case, the leak section can be removed by grinding. Other mechanical techniques may also be used, such as, but not limited to, plasma cutting, torch cutting, metal cutting saws, laser cutting, and the like. The exposed surface can then be typically cleaned. Cleaning can include one or more of the following steps: polishing, washing, surface treatment, and surface coating.

獲得暴露外表面後,可將上述加熱夾套附接於外表面之下部以形成封閉室520。在大多數情況下加熱夾套可藉由焊接附接。焊接技術之非限制性實例包括氣體遮護鎢弧焊(GTAW)、遮蔽金屬弧焊(SMAW)、氣護金屬弧焊(GMAW)及其類似技術。可使用建立焊接接頭時之重疊錯邊焊接沈積物提高焊接接頭力量。此外,焊接接頭可為全滲透焊縫(亦即與點焊或部分滲透焊縫相反)。 After the exposed outer surface is obtained, the heating jacket can be attached to the lower portion of the outer surface to form a closed chamber 520. In most cases the heating jacket can be attached by welding. Non-limiting examples of welding techniques include gas shielded tungsten arc welding (GTAW), shielded metal arc welding (SMAW), gas shielded metal arc welding (GMAW), and the like. The weld joint strength can be increased using overlapping misaligned weld deposits when establishing welded joints. In addition, the welded joint can be a fully permeable weld (ie, as opposed to a spot weld or a partially permeable weld).

再次參考圖5,可將封閉室與完好加熱旋管區段流體連接530。此可涉及連接轉變管道及/或轉變室以將加熱夾套連接於加熱旋管。如同緊固加熱夾套一般,轉變室或其他連接件可使用焊接技術緊固。該等焊接技術可在多種操作條件下提供長期壽命。無論如何,可緊固連接件以阻止加熱流體自外部加熱組件洩漏且經得起典型操作條件。以此方式,可藉由提供複合外部加熱組件修復或改良聚合高壓釜。 Referring again to Figure 5, the enclosed chamber can be fluidly coupled 530 to the intact heating coil section. This may involve connecting a transition duct and/or a transition chamber to connect the heating jacket to the heating coil. As with the heating jacket, the transition chamber or other connections can be tightened using welding techniques. These welding techniques provide long life over a wide range of operating conditions. In any event, the connectors can be tightened to prevent the heating fluid from leaking from the external heating assembly and withstanding typical operating conditions. In this manner, the polymerization autoclave can be repaired or modified by providing a composite external heating assembly.

本文所述之加熱夾套及加熱組件可提供有效熱傳遞,同時亦最小化或去除低循環疲勞之機率。因此,合併該等外部加熱裝置之聚合高壓釜可提供延長之使用壽命、較高可靠性及更均一之熱分佈。 The heating jacket and heating assembly described herein provide for efficient heat transfer while also minimizing or eliminating the chance of low cycle fatigue. Thus, a polymeric autoclave incorporating such external heating devices provides extended life, higher reliability, and a more uniform heat distribution.

儘管標的物已用特異於結構特徵及/或操作之語言描述,但應瞭解隨附申請專利範圍中所定義之標的物不應限於上述特定特徵及操作。相反地,上述特定特徵及操作作為實施申請專利範圍之實例形式而揭示。在不背離所述技術之精神及範疇的情況下,可設想諸多修改形式及其他配置。 Although the subject matter has been described in language specific to structural features and/or operation, it is to be understood that the subject matter defined in the appended claims Rather, the specific features and acts described above are disclosed as examples of the scope of the invention. Many modifications and other configurations are conceivable without departing from the spirit and scope of the technology.

100‧‧‧聚合高壓釜 100‧‧‧Polymerized autoclave

102‧‧‧複合外部加熱組件/外部加熱組件/加熱組件 102‧‧‧Composite external heating unit/external heating unit/heating unit

104‧‧‧加熱夾套/高壓釜加熱夾套 104‧‧‧heating jacket/autoclave heating jacket

106‧‧‧高壓釜容器體/容器體 106‧‧‧ autoclave container body/container body

108‧‧‧加熱管道/加熱旋管 108‧‧‧Heating pipe/heating coil

110‧‧‧上部第一進口 110‧‧‧ upper first import

112‧‧‧第二進口 112‧‧‧second import

114‧‧‧放壓閥 114‧‧‧pressure relief valve

116‧‧‧外表面 116‧‧‧ outer surface

118‧‧‧轉變室 118‧‧‧Transition room

120‧‧‧夾套流體進口/流體進口 120‧‧‧ Jacket fluid inlet/fluid inlet

122‧‧‧夾套流體出口/流體出口 122‧‧‧ Jacket fluid outlet / fluid outlet

124‧‧‧轉變管道 124‧‧‧Transformation pipeline

Claims (20)

一種高壓釜加熱夾套,其包含:具有外壁、上接觸表面及下接觸表面之加熱流體環,其在與高壓釜之外表面嚙合時形成封閉室;經定向以穿過該外壁且能夠將加熱流體引導至該封閉室中之流體進口;經定向以穿過該外壁且能夠將該加熱流體引導出該封閉室之流體出口;及複數個流體流動擋板,其定向在該封閉室內且經組態以在該封閉室內沿預定路徑引導該加熱流體。 An autoclave heating jacket comprising: a heating fluid ring having an outer wall, an upper contact surface, and a lower contact surface, forming a closed chamber when engaged with an outer surface of the autoclave; oriented to pass through the outer wall and capable of heating Fluid is directed to a fluid inlet in the enclosed chamber; a fluid outlet oriented to pass through the outer wall and capable of directing the heating fluid out of the closed chamber; and a plurality of fluid flow baffles oriented within the enclosed chamber and grouped State to direct the heating fluid along the predetermined path within the enclosed chamber. 如請求項1之高壓釜加熱夾套,其進一步包含與該流體出口流體連接且經組態以引導流入附接於該高壓釜之該外表面的半管加熱旋管中的轉變室。 The autoclave heating jacket of claim 1, further comprising a transition chamber fluidly coupled to the fluid outlet and configured to direct flow into a half-tube heating coil attached to the outer surface of the autoclave. 如請求項2之高壓釜加熱夾套,其中該轉變室與該流體出口經由管道流體連接。 The autoclave heating jacket of claim 2, wherein the transition chamber is fluidly connected to the fluid outlet via a conduit. 如請求項1之高壓釜加熱夾套,其中該外壁具有環形形狀。 The autoclave heating jacket of claim 1, wherein the outer wall has an annular shape. 如請求項4之高壓釜加熱夾套,其中該上接觸表面為界定該環之頂板的環形脊。 The autoclave heating jacket of claim 4, wherein the upper contact surface is an annular ridge defining a top plate of the ring. 如請求項4之高壓釜加熱夾套,其中該下接觸表面為界定該環之底板的環形凸緣。 The autoclave heating jacket of claim 4, wherein the lower contact surface is an annular flange defining a bottom plate of the ring. 如請求項1之高壓釜加熱夾套,其中該流體進口及該流體出口彼此貼近,且該複數個流體流動擋板包括分隔擋板,其定向在該流體進口與該流體出口之間以在與該高壓釜之該外表面嚙合時穿過該封閉室環向引導該加熱流體。 The autoclave heating jacket of claim 1, wherein the fluid inlet and the fluid outlet are in close proximity to each other, and the plurality of fluid flow baffles include a dividing baffle oriented between the fluid inlet and the fluid outlet to The outer surface of the autoclave is guided through the closed chamber to guide the heating fluid. 如請求項1之高壓釜加熱夾套,其中該複數個流體流動擋板包括 沿該封閉室分佈的交替之上部擋板及下部擋板,以使得該預定流動路徑為蛇形流體流動路徑。 The autoclave heating jacket of claim 1, wherein the plurality of fluid flow baffles comprises An alternating upper baffle and a lower baffle distributed along the enclosed chamber such that the predetermined flow path is a serpentine fluid flow path. 如請求項8之高壓釜加熱夾套,其中該蛇形流體流動路徑水平且垂直地變化。 The autoclave heating jacket of claim 8 wherein the serpentine fluid flow path varies horizontally and vertically. 一種具有複合外部加熱組件之聚合高壓釜,其包含:具有內部反應室及外表面之高壓釜容器體,該外表面包括上部及下部;附接於該下部而形成封閉室之加熱夾套,該封閉室具有複數個流體流動擋板,其經組態以在該封閉室內且圍繞該下部沿繚繞路徑引導加熱流體;及纏繞且附接於該上部之加熱管道,該加熱管道具有多個圍繞該上部之纏繞物且與該加熱夾套流體連接,以使得該加熱流體可穿過該封閉室及該加熱管道循環來向該內部反應室中傳遞熱,其中該加熱夾套及該加熱管道形成該複合外部加熱組件。 A polymerization autoclave having a composite external heating assembly, comprising: an autoclave container body having an internal reaction chamber and an outer surface, the outer surface including an upper portion and a lower portion; and a heating jacket attached to the lower portion to form a closed chamber, The enclosed chamber has a plurality of fluid flow baffles configured to direct heating fluid within the enclosed chamber and around the lower portion along the winding path; and a heating conduit wound and attached to the upper portion, the heating conduit having a plurality of surrounding An upper wrap and fluidly coupled to the heating jacket such that the heating fluid can circulate through the closed chamber and the heating conduit to transfer heat to the internal reaction chamber, wherein the heating jacket and the heating conduit form the composite External heating assembly. 如請求項10之聚合高壓釜,其中該容器體為經包覆容器。 The polymerization autoclave of claim 10, wherein the container body is a coated container. 如請求項10之聚合高壓釜,其中該加熱夾套覆蓋該外表面之3%至40%。 A polymeric autoclave according to claim 10, wherein the heating jacket covers from 3% to 40% of the outer surface. 如請求項10之聚合高壓釜,其中該加熱夾套為環,其具有連接於底板及頂板之環形垂直外壁,該底板及該頂板一起使該加熱流體緊靠該外表面之該下部。 A polymeric autoclave according to claim 10, wherein the heating jacket is a ring having an annular vertical outer wall joined to the bottom plate and the top plate, the bottom plate and the top plate together bringing the heating fluid against the lower portion of the outer surface. 如請求項10之聚合高壓釜,其中該複數個流體流動擋板經定向以界定蛇形流體流動路徑。 The polymeric autoclave of claim 10, wherein the plurality of fluid flow baffles are oriented to define a serpentine fluid flow path. 如請求項10之聚合高壓釜,其中該加熱管道為半管,其直接焊接於該高壓釜之該外表面。 A polymerization autoclave according to claim 10, wherein the heating pipe is a half pipe which is directly welded to the outer surface of the autoclave. 如請求項10之聚合高壓釜,其進一步包含轉變室,該轉變室使該加熱夾套與該加熱管道流體連接。 The polymerization autoclave of claim 10, further comprising a transition chamber that fluidly couples the heating jacket to the heating conduit. 一種修復具有附接於外表面之外部加熱旋管之聚合高壓釜的方法,該加熱旋管在該高壓釜之該外表面之下部具有變弱或洩漏區段,該方法包含:自該高壓釜之該外表面的該等下部移除該等加熱旋管之該等變弱或洩漏區段,以使完好加熱旋管區段保留於該外表面之上部;將如請求項1之加熱夾套附接於該外表面之該等下部以形成封閉室;及使該封閉室與該完好加熱旋管區段流體連接。 A method of repairing a polymeric autoclave having an external heating coil attached to an outer surface, the heating coil having a weakened or leaking section below the outer surface of the autoclave, the method comprising: from the autoclave The lower portions of the outer surface remove the weakened or leaking sections of the heating coils such that the intact heating coil section remains above the outer surface; the heating jacket of claim 1 is attached Connecting the lower portions of the outer surface to form a closed chamber; and fluidly connecting the closed chamber to the intact heating coil portion. 如請求項17之方法,其中該加熱夾套係藉由焊接附接。 The method of claim 17, wherein the heating jacket is attached by welding. 如請求項17之方法,其中該加熱夾套包含鉻-鉬鋼合金。 The method of claim 17, wherein the heating jacket comprises a chromium-molybdenum steel alloy. 如請求項17之方法,其中該複數個流體流動擋板定向在該封閉室內,為該加熱流體界定蛇形流動路徑。 The method of claim 17, wherein the plurality of fluid flow baffles are oriented within the enclosed chamber to define a serpentine flow path for the heating fluid.
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