200909407 九、發明說明： 【發明所屬^技術領域j 本發明係與一種用於例如經純化的對笨二甲酸 ("ΡΤΑΠ)、經純化的異苯二甲酸以及偏笨三甲酸之聚羧酸的 回收之新方法有關。更明確地說，本申請案係與使用旋轉 加壓過濾器來回收結晶對苯二曱酸、異笨二曱酸以及偏笨 三甲酸的新穎用途，以及一種用來回收所產生之結晶的方 法有關。200909407 IX. INSTRUCTIONS: [Invention] Technical Field j The present invention relates to a polycarboxylic acid for use in, for example, purified p-dicarboxylic acid ("ΡΤΑΠ), purified isophthalic acid, and stupid tricarboxylic acid. The new method of recycling is related. More specifically, the present application relates to the novel use of a rotary pressurizing filter for recovering crystalline terephthalic acid, isobenzoic acid, and stupid tricarboxylic acid, and a method for recovering the resulting crystals. related.
C先前技術:J 10 發明背景 為了簡化說明，該發明背景將著重於對苯二曱酸。對 苯二甲酸係被用於許多不同的聚合物之生產中，其等包括 有聚對苯二甲酸乙二醇酯（PET)。PET的典型製程係直接將 對苯二甲酸與多元醇進行縮合。此一直接酯化作用反應需 15要經純化之對苯二曱酸，以使得該反應產物係為可接受的。 對苯二甲酸係藉著將P-二曱苯直接氡化，並接著自母 澄清液結晶而回收粗萃的對苯二甲酸（CTA)來加以生產。此 一 CTA仍然含有大約為重量的〇.2_〇.4%之4-幾基苯尹酸 (4-CBA)的主要雜質。為了減少内含之4_CBA的含量，該CTA 20係典型地被溶解在水中，然後所產生的溶液係在一氫化作 用反應器中加以處理’而將4-CB A轉換為ρ_甲苯酸。來自該 氣化作用反應器的溶液然後係典型地藉著在一套结晶器中 加以沖洗而冷卻，以將該經純化的對苯二甲酸（ρτΑ)以結晶 加以沈澱。來自該結晶器之淤漿仍然包含有需要自ρτΑ分 5 200909407 離的顯著含量之P-甲基甲酸，以符合常用之不超過i5〇ppm 的常用商業規格。 目刖係運用二階段固相分離來純化該PTA。自母澄清 液刀離PTA的傳統方法’包括有在1〇〇。。至17〇。。的溫度下 、及在1至7bar的壓力下將該游漿加以離心。在這些條件下 大多數的p_甲基甲酸將會留在溶液中而被加以分離。 來自該離心管之P T A結晶僅含有少量的p _甲基甲酸， 但是其確實包含有殘留的母澄清液（典型地為1〇15%)。為 了要去除這些雜質，該結晶通常係與額外添加之水混合（典 10型地在L1至丨.5 m3水/噸PTA的比例内）來沖洗其所仍然包 含之母澄清液。其會產生一具有45(±5)百分比之固體淤 漿。此一淤漿然後被沖洗至常壓下並進給至一第二階段離 心分離作用或是一旋轉真空過濾器（RVF)。該包含殘留 10-15%之水的PTA然後係典型地在一旋轉乾燥器中加以乾 15燥並儲存。§亥PTA結晶仍然包含有較小量的p_甲基甲酸（通 常少於150ppm)而同時4-CBA的含量係典型地低於25ppm。 美國專利第5,175,355號教示一種包含有加壓過遽作 用之純化對本二甲酸的方法。此一參考資料教示將一水性 於漿（其包含有以結晶存在之經純化的對苯二曱酸以及存 20 在於水溶液中以及係為共結晶形式之p-甲基曱酸）導入一 或更多的濾槽中。該淤漿係在一由常壓至16atm的系統壓力 下進行過濾。該具有所得到之濾餅的濾槽，然後係被轉移 至一沖洗區域内’其中一被加熱至38°C至2051的水流係被 導入至該濾槽，以在該濾餅上形成一儲水區。置換洗滌作 200909407 用然後係在-壓力梯度下藉著強迫水分通過該渡餅而同時 維持該儲水區來達成，該梯度係至少為高於系統壓力 〇.5_。該置換洗蘇作關被允許持續—充份的時間來移 除所需之雜質量。該濾槽然後被轉移至一壓力釋放區域， 5其中該系統壓力係被快速地釋放以將殘留在該渡餅中的水 分加以閃蒸（flash evaporate)並回收該產物。壓力釋放區域 然後被增壓回該系統壓力，以準備好接受另外的產物。此 一方法係被報導可以得到含有少於重量的2〇〇ppm之p甲 基甲酸的對苯二甲酸。 10 美國專利第6,639，104號描述一種改良方法，其包含有 將該經沖洗的濾餅轉移至一處於低於該洗滌區域的壓力之 壓力下的降壓區域（或是壓力釋放區域）。此一參考資料描述 一種可以被用來作為降壓系統之特定具體例的圓頂閥。 其他描述用於自包含有結晶的於聚來純化或回收物 15 質之方法的參考資料包括有W0 0155075、US 6,655,531、 US 5,470,473、US 5,093,001、EP 0 406 424、W0 9519335 以及 JP 11179115。 提供一種用於自經純化的對笨二甲酸結晶來回收苯 二甲酸與移除雜質之經改良的方法，將會改善對生產經純 20 化的對苯二甲酸之技藝。 C發明内容3 發明摘要 本發明係為一種用於例如經純化的對苯二甲酸 (，'ΡΤΑΠ)、經純化的異苯二甲酸以及偏苯三曱酸之聚羧酸的 200909407 回收之改良方法，其包含有a)將一包含有水分，結晶對苯 二甲酸以及雜質之液該漿導人—高壓旋轉過遽器；_ 濾該淤漿並至少收集部分的固體部分；c)將該所收集的固 體部分通至-包含有-溫度控制系統的旋轉閥；⑽過該 5 /JBL度控制系統來控制在該旋轉閥中之溫度；並且e)將該固 體部分自該旋轉閥移除。該旋轉閥包含有一閥件殼體與轉 子，而該溫度控制系統可以控制該閥件殼體與轉子之間的 溫度差異。 本發明提供一種用於聚羧酸之回收的改良系統，其運 1〇用一種可以在不影響該過濾器壓力控制系統或物質通量 下，將該固體物質減壓之降壓系統。 【實施方式3 發明詳述 在本發明中，該包含有了含有雜質的例如對苯二甲 15酸、異苯二曱酸、偏笨三曱酸之羧酸的液態淤漿，可以來 自於任何的對苯二曱酸、異苯二甲酸、偏笨三甲酸生產流 知中。其專係為在s亥技藝已知的並在一方面對本發明而古 係為最不重要的。該用於過濾於激之特殊高愿旋轉過漁器 係同樣地對於本發明而言並不重要的。其可以運用任何可 20以在大於常壓之壓力下操作的過濾系統。較佳地，在標準 操作情況下’該過遽器可以處理該設備之整個笨二甲酸通 量，並且係可以在從1.0至10·Obar的壓力下操作。適當的過 濾器係為由Andritz公司所販售並被描述於美國專利第 5,70,473和6,655,53 1號（其等係在此被併入以供參考）中之 200909407C Prior Art: J 10 Background of the Invention In order to simplify the description, the background of the invention will focus on terephthalic acid. Terephthalic acid is used in the production of many different polymers, including polyethylene terephthalate (PET). A typical process for PET is the direct condensation of terephthalic acid with a polyol. This direct esterification reaction requires 15 purified terephthalic acid to make the reaction product acceptable. The terephthalic acid is produced by directly deuterating P-diphenylbenzene and then recovering the crude terephthalic acid (CTA) by crystallizing from the mother liquid. This CTA still contains approximately 0.2% by weight of the major impurities of 4-methylbenzonic acid (4-CBA). In order to reduce the content of the contained 4_CBA, the CTA 20 system is typically dissolved in water, and the resulting solution is treated in a hydrogenation reactor to convert 4-CB A to p-toluic acid. The solution from the gasification reactor is then typically cooled by rinsing in a set of crystallizers to precipitate the purified terephthalic acid (ρτΑ) as crystals. The slurry from the crystallizer still contains a significant amount of P-methylformic acid that needs to be separated from ρτΑ 5 200909407 to meet commonly used commercial specifications not exceeding i5 〇 ppm. The target is to purify the PTA using a two-stage solid phase separation. Self-mother clarification The traditional method of liquid knife away from PTA' includes one. . To 17 baht. . The slurry was centrifuged at a temperature of 1 to 7 bar. Under these conditions most of the p-methylformic acid will remain in solution and be separated. The P T A crystals from the centrifuge tube contained only a small amount of p-methylformic acid, but it did contain residual parent clear liquid (typically 1〇15%). In order to remove these impurities, the crystallization is usually mixed with additional water (in the ratio of L1 to 丨.5 m3 water/ton PTA) to rinse the parent clarified liquid still contained therein. It produces a solid slurry having 45 (± 5) percent. This slurry is then flushed to atmospheric pressure and fed to a second stage of centrifugal separation or a rotary vacuum filter (RVF). The PTA containing 10-15% residual water is then typically dried and stored in a rotary drier. § Hei PTA crystals still contain a smaller amount of p-methylformic acid (usually less than 150 ppm) while the 4-CBA content is typically less than 25 ppm. U.S. Patent No. 5,175,355 teaches a process for the purification of the present dicarboxylic acid containing a pressurized ruthenium. This reference teaches the introduction of an aqueous solution (which contains purified terephthalic acid in the presence of crystals and p-methyl decanoic acid in an aqueous solution and in a co-crystal form). More in the filter tank. The slurry was filtered at a system pressure of from atmospheric to 16 atm. The filter tank having the resulting filter cake is then transferred to a rinse zone where a water stream heated to 38 ° C to 2051 is introduced into the filter tank to form a reservoir on the filter cake. Water area. Displacement wash 200909407 is achieved by then forcing moisture through the cake while maintaining the water reservoir at a pressure gradient that is at least above the system pressure 〇.5_. The replacement wash is allowed to continue - sufficient time to remove the desired amount of impurities. The filter tank is then transferred to a pressure relief zone, 5 wherein the system pressure is rapidly released to flash evaporate the water remaining in the cake and recover the product. The pressure relief zone is then pressurized back to the system pressure to be ready to accept additional product. This method has been reported to give terephthalic acid containing less than 2 ppm by weight of p-methylformic acid. U.S. Patent No. 6,639,104 describes an improved method comprising transferring the rinsed filter cake to a reduced pressure zone (or pressure relief zone) at a pressure below the pressure of the wash zone. This reference describes a dome valve that can be used as a specific example of a buck system. Other references for methods for the purification or recovery of materials from the inclusion of crystals include WO 0155075, US 6,655,531, US 5,470,473, US 5,093,001, EP 0 406 424, WO 9519335, and JP 11179115. Providing an improved process for the recovery of benzoic acid from the purified phthalic acid crystals and removal of impurities will improve the art of producing pure 20 terephthalic acid. C SUMMARY OF THE INVENTION The present invention is an improved process for the recovery of 200909407 for, for example, purified terephthalic acid (''''), purified isophthalic acid, and trimellitic acid polycarboxylic acid. Containing a) a liquid containing moisture, crystalline terephthalic acid and impurities, the slurry is guided by a high pressure rotary converter; _ filtering the slurry and collecting at least part of the solid portion; c) The collected solid portion is passed to a rotary valve containing a temperature control system; (10) the 5/JBL degree control system is passed to control the temperature in the rotary valve; and e) the solid portion is removed from the rotary valve. The rotary valve includes a valve housing and a rotor, and the temperature control system controls the temperature difference between the valve housing and the rotor. SUMMARY OF THE INVENTION The present invention provides an improved system for the recovery of polycarboxylic acids which utilizes a pressure reducing system which depressurizes the solid material without affecting the filter pressure control system or mass flux. [Embodiment 3] DETAILED DESCRIPTION OF THE INVENTION In the present invention, the liquid slurry containing a carboxylic acid having impurities such as terephthalic acid, isophthalic acid or stearic acid may be derived from any The production of terephthalic acid, isophthalic acid, and stupitricarboxylic acid is known. Its specialty is known to be in the art of shai and is the least important to the invention on the one hand. This special high-speed rotating fisherman system for filtering is equally unimportant to the present invention. It can utilize any filtration system that can operate at pressures greater than atmospheric pressure. Preferably, the filter can handle the entire sterol dicarboxylic acid flux of the apparatus under standard operating conditions and can operate at pressures from 1.0 to 10 o. A suitable filter is commercially available from Andritz, Inc. and is described in U.S. Patent Nos. 5,70,473 and 6,655, the entire disclosure of which is incorporated herein by reference.
Bird Young Rotary Filter旋轉過遽器。 該過濾器係典型地由在加工壓力下進行增壓之殼 體，以及一由例如布料或其之等效過濾裝置之過濾裝置所 覆蓋之圓筒來組成，該圓筒係以適當之低於該殼體的壓力 5 來進行增壓。 該圓筒係理想地被區分為三個區域： •移除該母澄清液之第一區域。 •清洗該固體之第二區域。 •該過量之清洗澄清液係被移除而該固體係被移 10 出之第三區域。 該殼體的壓力係較佳地介於1.5至65的範圍内，而最 佳地係為大約4.5bar。該過濾器的殼體係以可以用於將該過 濾器殼體增壓之熱惰性氣體、蒸氣或是該等二者之混合物 來加以增壓。使用熱氣體，蒸氣或是該等二者之混合物來 I5進行增壓’可以允§午在該過;慮裝置内產生一致的溫度，而 避免將會導致雜質的局部性結晶現象然後降低產物品質之 冷點。該過濾作用係最佳地在110至160 〇C下進行，而最佳 地係在147 °C下進行。 該具有110至16〇r之溫度（更佳地為135至150。〇而又 20 更佳地為147°C)的於漿，係以該進給於漿之2〇%至1 〇〇%的 數量會溢流至一液體密封的方式，而自該結晶單元的最後 一個結晶器進給至一位在該過遽器殼體内之進給於漿盆， 該於滎盆包含一具有液面控制系統的壓力導管，該壓力係 通過其本身之管線而與該過濾器殼體平衡。此一具體例允 9 200909407 許對該過濾器維持穩定的進給作用、淹沒該過濾圓筒的作 用’以及穩定該過濾裝置的壓力，並接著回歸至該淤漿進 給導管。 在殼體與圓筒之間的壓力差係介於0.1至2.〇bar的範圍 5内，較佳地係介於0.3至0.7bar的範圍内，最佳地係為〇.5bar。 自該旋轉壓力過濾器所移除之母澄清液可以如在該 技藝中已知的被分別地回收’並在生產製程中被重複使用 或是輸送至廢液處理設備，。 其餘的固體部分然後係以額外數量的水來加以清 10洗。目前已經發現本發明之方法需要較少的洗滌水達到與 傳統類似之純度。因此雖然在本發明的洗滌階段可以使用 任何數量的水，其係較佳地使用少於每噸pTA i立方公尺之 水，以節約用水並減低與將水加熱至加工溫度有關之能 量。該水量係較佳地為介於〇·2至〇7m3/MT的pta之範圍 15内，而最佳地大約為0.5 MT的PTA。該洗滌作用係較佳 地在與該過濾作用相同之溫度下進行，雖然這僅是較為便 利而並非是必要的。清洗該固體物質之該水溫係介於5〇〇c 至16PC’較佳地係介於丨川^至丨％%，最佳地係為147。〔。 該清洗澄清液然後可以被分別地自該母澄清液收集，並如 20同在该技藝十已知的於該生產製程中重複使用或是被回收 至該生產製程中。 如在此技藝中已知的，在經過清洗之後該固體物質可 以由該遽餅移除系統來分離，將熱氣、蒸氣或是該等二者 之混合物，自該旋轉圓筒的内側吹入該過濾'殼體内，而該 10 200909407 吹送液體的溫度係介於110至跡⑽範圍内，更佳地為i35 至獄，且又更佳地為147。〇對該據餅移除系統饋送熱 氣，可以允許將該排出產物之溫度維持在適當的高溫下， 因而使得該最終之接下來的乾燥作業更容易並且更便宜。 5該經分離的固體係較佳地通過一包括有旋轉間之降壓系統 而進入-常壓濾餅漏斗，其係處於一比該過遽器殼體更低 之壓力下。 本發明的降壓系統系為一種在該風扇與該殼體之間 具有適切的間隙之旋轉閥，以使得風扇不會與該旋轉間殼 10體之内部表面密封地接合。可以被用於本發明之旋轉閥的 一具體例係被描述於us 2006/0045729中。基於本發明之目 的，該旋轉閥包含有至少一閥件殼體與一轉子。該旋轉間 也裝設有-溫度控制系統以依據一選定的設定點而維持在 旋轉閥的殼體與轉子之間的溫度差，來控制在該旋轉間的 15風扇和殼體之間的間隙。在此一方法中，該旋轉閥允許存 在於該固體產物中的水分可以在該閥件本身的風扇中以蒸 汽來順暢地釋放，並接著在該間件的排氣端避免閃蒸現象 (sudden flash)。因此，該溫度控制系統係在被用來進行在 »亥轉子與閥件设體之間的間隙之間接控制，而間接地會導 20 致一受到調控之壓力下降模式。 該被用來控制閥件殼體與轉子之間的溫度差之溫度 控制系統，包含有至少一加熱媒介、至少一溫度測量裝置 以及至少一邏輯控制裝置。該所使用之加熱媒介並不重 要，並且可以是例如熱蒸氣、熱氮氣、自該氧化作用反應 200909407 器排出之氣體、任何其他的適當熱惰性氣體、一電加熱儀 器或是一或更多的這些物質之組合。 此一新穎系統的應用允許釋放在該固體產物中之水 氣’卻不防止反而是控制氣體之漏洩量。其需要使用熱氣 5來將該過濾器增壓，以維持一通過該旋轉閥之連續的氣體 漏洩現象；事實上較冷的氣體會在該系統的溫度控制上導 致氣體漏洩量增加或是致使閥件失效的問題。此一新穎的 系統以及所使用之熱增壓液體，可以共同允許限制與控制 經過該閥件之氣體漏洩現像並避免失效現象。 10 該會接受來自該降壓系統的固體產物之濾餅漏斗，可 以選擇性地設有二個出口以釋放氣體物質，並且自一端連 接至一真空系統以避免非所欲之壓力增加，同時自另一端 連接至一常壓緩衝部份，來避免非所欲之完全真空情況。 該固體物質然後可以藉由一例如螺絲之適當的裝置 15而通至一乾燥器，以如在此技藝中已知的來進—步進行處 理。 具體例 下列的方法係被運用於具體例1和2中： 測定水氣含量之方法 有蓋培養皿係在大約105γ下之烤箱中乾燥直到得到 其之恆重。大約10克的樣本係被稱量至最接近〇1毫克而置 於魏燥的有蓋培養皿内。包含有該樣本之有蓋培養皿係 被置入處於大約105〇C之空氣烘箱内2小時，並且在—乾燥 器中於室溫下加以冷卻。該有蓋培養皿㈣被秤重以作為 12 200909407 第重里4數。包含有該樣本之有蓋培養皿係在該烤箱中 多乾燥3G分鐘’並在—乾燥”於室溫下冷卻。該有蓋典 然後被秤重以作為第二重量讀數。該等第一與第二‘ "數係被加以比較。少於G 5毫克之差異係被視為是怪 疋或者，該乾燥作用係、直到該重量i異係為怪定才算完 成0The Bird Young Rotary Filter rotates the filter. The filter is typically comprised of a housing that is pressurized under processing pressure, and a cylinder that is covered by a filtering device such as a cloth or its equivalent filtering device, which is suitably below The pressure of the housing is 5 to boost. The cylinder is ideally divided into three zones: • The first zone of the parent clarified liquid is removed. • Clean the second area of the solid. • The excess cleaning clarified liquid is removed and the solid is removed from the third zone. The pressure system of the housing is preferably in the range of from 1.5 to 65, and most preferably about 4.5 bar. The housing of the filter is pressurized with a hot inert gas, vapor, or a mixture of the two that can be used to pressurize the filter housing. Use hot gas, steam or a mixture of the two to pressurize I5' to allow for a noon; to produce a consistent temperature in the device, avoiding local crystallization that would lead to impurities and then reducing product quality. It’s cold. This filtration is carried out optimally at 110 to 160 ° C, and optimally at 147 ° C. The slurry having a temperature of 110 to 16 Torr (more preferably 135 to 150 Torr and more preferably 20 147 ° C) is fed to the slurry at 2% to 1% by weight. The amount will overflow to a liquid-tight manner, and the last crystallizer from the crystallization unit is fed to a feed tank in the filter housing, the bowl containing a liquid The pressure conduit of the surface control system is balanced with the filter housing by its own line. This specific example allows the filter to maintain a stable feed, submerge the filter cylinder's action and stabilize the pressure of the filter unit, and then return to the slurry feed conduit. The pressure difference between the housing and the cylinder is in the range 5 of 0.1 to 2. 〇 bar, preferably in the range of 0.3 to 0.7 bar, most preferably 〇.5 bar. The mother clarified liquid removed from the rotary pressure filter can be separately recovered as known in the art and reused in the production process or delivered to the waste treatment facility. The remaining solid portion is then washed with an additional amount of water. It has now been found that the process of the present invention requires less wash water to achieve a purity similar to conventional. Thus, although any amount of water can be used in the scrubbing stage of the present invention, it is preferred to use less than pTA im3 of water per ton to conserve water and reduce the energy associated with heating the water to processing temperatures. The amount of water is preferably in the range 15 of pta between 〇·2 and 〇7m3/MT, and is most preferably about 0.5 MT of PTA. This washing action is preferably carried out at the same temperature as the filtration, although this is only convenient and not necessary. The water temperature for cleaning the solid matter is from 5 〇〇 c to 16 PC', preferably from 丨川^ to 丨%%, most preferably 147. [. The cleaning clarified liquid can then be separately collected from the parent clarifying liquid and reused or recycled to the production process as is known in the art. As is known in the art, the solid material may be separated by the cake removal system after washing, and hot gas, steam or a mixture of the two may be blown from the inside of the rotating cylinder. Filtered within the housing, and the temperature of the 10 200909407 blowing liquid is in the range of 110 to 10 (10), more preferably i35 to prison, and even more preferably 147. Feeding the cake removal system with heat may allow the temperature of the effluent product to be maintained at an appropriate elevated temperature, thereby making the final subsequent drying operation easier and less expensive. 5 The separated solids are preferably passed through a pressure reducing system comprising a rotating chamber into an atmospheric filter cake funnel at a lower pressure than the filter housing. The pressure reducing system of the present invention is a rotary valve having a proper gap between the fan and the housing such that the fan does not sealingly engage the inner surface of the rotating housing 10. A specific example of a rotary valve that can be used in the present invention is described in us 2006/0045729. For the purposes of the present invention, the rotary valve includes at least one valve housing and a rotor. The rotating chamber is also provided with a temperature control system for maintaining a temperature difference between the housing and the rotor of the rotary valve in accordance with a selected set point to control the gap between the fan and the housing between the 15 and the rotating chamber. . In this method, the rotary valve allows moisture present in the solid product to be smoothly released by steam in the fan of the valve member itself, and then avoids flashing at the exhaust end of the partition (sudden Flash). Therefore, the temperature control system is used to control the gap between the rotor and the valve member, and indirectly leads to a regulated pressure drop mode. The temperature control system for controlling the temperature difference between the valve housing and the rotor includes at least one heating medium, at least one temperature measuring device, and at least one logic control device. The heating medium used is not critical and may be, for example, hot steam, hot nitrogen, gas vented from the oxidation reaction 200909407, any other suitable hot inert gas, an electric heating instrument, or one or more A combination of these substances. The application of this novel system allows the release of water in the solid product without preventing the leakage of the gas. It is necessary to use hot gas 5 to pressurize the filter to maintain a continuous gas leakage through the rotary valve; in fact, the cooler gas may cause an increase in gas leakage or cause a valve in the temperature control of the system. The problem of failure. This novel system, as well as the hot pressurized liquid used, can collectively allow for limiting and controlling the leakage of gas through the valve member and avoiding failure. 10 that will accept a filter cake funnel from the solids of the pressure reduction system, optionally with two outlets to release gaseous species, and from one end to a vacuum system to avoid undesired pressure increases, while The other end is connected to a constant pressure buffer to avoid undesired full vacuum. The solid material can then be passed to a dryer by a suitable means 15, such as a screw, for further processing as is known in the art. Specific Examples The following methods were applied to Specific Examples 1 and 2: Method for determining moisture content The covered petri dish was dried in an oven at about 105 γ until its constant weight was obtained. Approximately 10 grams of the sample was weighed to the nearest peti dish in the Wei-dry petri dish. The covered petri dish containing the sample was placed in an air oven at approximately 105 ° C for 2 hours and cooled in a desiccator at room temperature. The covered petri dish (4) was weighed as the number of 12 200909407. The covered petri dish containing the sample was dried in the oven for 3 G minutes and cooled at room temperature. The covered code was then weighed to take the second weight reading. The first and second The ' " number system is compared. The difference of less than G 5 mg is considered to be quirks or, the drying effect is not completed until the weight i is strange.
P-曱基曱酸濃度係使用HPLC(日立公司，型號L71〇〇 或等效裝置）來測定。 具體例1和2 具體例1和2證實改變閥件條件與該增壓氣體對於在 6亥產物中的水氣與P-曱基曱酸含量之影響。具體例1和2的 結果係被概述於下列的表1中。The P-mercaptodecanoic acid concentration was measured using HPLC (Hitachi, Model L71® or equivalent). Specific Examples 1 and 2 Specific Examples 1 and 2 confirmed the effect of changing the condition of the valve member and the content of the pressurized gas on the water vapor and P-mercaptodecanoic acid in the product. The results of Specific Examples 1 and 2 are summarized in Table 1 below.
表1Table 1
_^殼體壓力（bar) 3 3 _设體-圓筒壓力差（bar) 一氣流（公斤/hr) ^固體饋料（公斤/hr) _於漿溫度（°C) 洗務水（公斤/hr) 滌水溫度（°C) 閥殼體溫度（°c) 閥轉子溫度（°c) 0.3 0.3 790 530 1200 1200 125.3 128.3 510 510 125 126 56 71 85 124 13 200909407 旋轉閥氣體洩漏（公斤/hr) 430 265 產品品質 . 水分含量（％) 11.8 8.1 在濕濾餅中之p-曱基曱酸（ppm) 183 153 I：圖式簡單說明3 (無） 【主要元件符號說明】 (無) 14_^Shell pressure (bar) 3 3 _Set body-cylinder pressure difference (bar) One air flow (kg/hr) ^Solid feed (kg/hr) _Pulp temperature (°C) Washing water (kg /hr) Washing water temperature (°C) Valve housing temperature (°c) Valve rotor temperature (°c) 0.3 0.3 790 530 1200 1200 125.3 128.3 510 510 125 126 56 71 85 124 13 200909407 Rotary valve gas leak (kg / Hr) 430 265 Product quality. Moisture content (%) 11.8 8.1 p-mercaptodecanoic acid (ppm) in wet cake 183 153 I: simple description of the figure 3 (none) [Key component symbol description] (none) 14