1239948 五、發明說明（ι) 發明之技術範疇 本發明係關於高純度對酞酸（以下簡稱PTA )之製法，係 將對二甲苯之液相氧化所得粗製對酞酸（以下簡稱CTA )， 經加氫處理而得。 習知技術 對二甲苯利用含分子氧之氣體氧化時，在對酞酸（以下 稱T A )之外，令生成含主要雜質爲4 -羧基苯甲醛（以下稱 4-CBA)之CTA。但製造聚酯纖維時，需要pTA爲原料， 上述CTA必須加以精製。 PTA之製已知有CTA在加氫觸媒存在下加氫處理之方法 (例如特開平4 - 6 6 5 5 3號）。此法因加氫，即使低溫亦可 將4 - CBA還原成水溶性對苯乙酸，經晶析、固液分離等， 將對苯乙酸與對酞酸分離，以製成PTA。 上述加氫處理，是在反應器形成固體觸媒之固定層， CTA水溶液在通過此觸媒層中，同時供氫。此時，CTA水 溶液是將CTA粉末分散於水中形成漿液，加熱使CTA溶 於水中調製而成。此時爲使以良好效率進行反應，所形 成漿液濃度需與加熱時的對酞酸之溶解度相當。 習知CTA之漿液化，一般是將水和粉末CTA導入具有 旋轉式攪拌槳葉的水漿液調製槽內，攪拌形成漿液。此 法是一邊將充滿漿液調製槽內之液體攪拌，一邊連續供 應水和粉末CTA ,而使粉末CTA在水中分散。 但因粉末CTA和水之親和性不高，會呈含氣泡的狀態 1239948 五、 發明說明（ 2 ) 分 散 9 氣泡難 以分離。含氣 泡狀態時，粉末CTA會以塊 狀 流 動 ,加熱 也不會溶解， 以塊狀流入加氫反應器時， 會 集 在 加氫觸 媒層，造成堵 塞。 爲 防 止此事 ,向來是減少 分散的粉末CTA量，形成低 濃 度 水 漿液， 減少成爲含氣 泡塊狀之CTA量，因此即可加 熱 溶 解 。然而 供給低濃度漿 液時，加氫反應的效率會降 低 爲 其問題 所在。 發 明 要 匕 本 發 明之目 的，在於提供 一種高純度對酞酸之製法， 可 促 進 氣泡分 解，使粉末CAT均勻分散，形成高濃度水 漿 液 ， 以良好 效率進行加氫 反應，因此以良好效率製造 PTA ‘ ) 本 發 明爲下 述高純度對酞 酸之製法。 1 . 一 種尚純 度對酞酸之方 法，係將對二甲苯因液相氧 化所 得 粗製對 酞酸，與水混 合形成漿液，對此漿液加熱 以 形 成 粗製對 酞酸溶液，於加氫觸媒存在下加氫處理，以 製 尚 純度對 酞酸，其特徵 爲，粉末粗製對酞酸與一部 份水在 捏合裝 置預混合，形 成5 5〜7 5重量％濃度之預混 合 物 ， 此預混 合物再與剩餘 水混合形成漿液，進行加氫 處 理 者 Ο 2 . 如 剩餘第 (1 )項之方法， 係以連續式捏合裝置進行預 混 合 者 〇 3 . 如 上述第 (1 )項之方法， 係利用按水平方向配置之旋 -4- 1239948 五、發明說明（3) 轉圓板，將粉末CTA呈徑向送出，並與水混合，使混合 物按狹窄的曲折狀阻礙路徑移動，並予以均質化之一種 旋轉圓板形捏合裝置進行預混合者。 圖式簡蜇說明 第1圖爲高純度對酞酸製法實施例之流程圖； 第2圖爲捏合裝置之剖面圖。 靈明之詳細說明 本發明加氫處理對象之粗製對酞酸（CAT )，係由對二甲 苯利用液相氧化所得粗製對酞酸。此等對酞酸一般含主 要雜質4-CBA0 . 1〜0.4重量％左右。 上述對二甲苯的液相氧化，係使用溶劑和觸媒進行。 對二甲苯在液相氧化中所用溶劑，有例如乙酸、丙酸、 正丁酸、異丁酸、正戊酸、三甲基乙酸、己酸等脂肪酸， 或與水之混合物。其中以乙酸或後述含水之酸爲佳。 對二甲苯之液相氧化觸媒，一般爲重金屬化合物和/或 含溴化合物，前者有鎳、鈷、鐵、鉻、錳等，二者共同 爲元素形態或化合物，以溶解於反應系的形態使用爲 佳。以鈷化合物，錳化合物、溴化合物爲佳，鈷化合物 用量通常爲鈷佔溶劑之10至10,000ppm，以100至3000ppm 爲佳，錳化合物則錳對鈷之原子比爲0 . 00 1至2，同理，溴 化合物係對鈷的原子比爲0 . 1至5。 對二甲苯之液相氧化，係使用含分子氧的氣體進行。 此等含氧氣體通常使用以惰性氣體稀釋之氧，例如空氣 1239948 五、發明說明（4) 或富氧空氣。氧化反應之溫度通常爲150至270 °C ,以 1 7 0 °C至2 2 0 °C爲佳，壓力至少要在反應溫度時使混合物 保持液相之壓力以上，通常爲〇 . 5至4MPa (錶計壓力）。 再者，反應時間視裝置大小等而定，惟通常滯留時間要 2〇至180分鐘左右。反應系內的水份濃度通常爲3至 30重量％，以5至15重量％爲佳。 將上述液相氧化反應所得CTA導入反應器內，於加氫 觸媒存在下進行加氫處理，以製造PTA，此時，從液相 氧化反應中的母液分離之CTA加以水漿液化，將所得水 漿液加熱、加壓，與對酞酸水水溶液導入反應器，進行 加氫處理。一般漿液的CTA濃度爲10〜40重量％，以20〜 3〇重量％爲佳，惟以相當於加熱、加壓時的溶解度之濃 度爲佳。 本發明爲形成漿液，將粉末CTA —部份與水利用捏合 裝置預混合，形成5 5 - 7 5重量％濃度之預混合物，以60 〜7 0重量％爲佳，此預混合物再與剩餘水混合，使粉末 CTA均勻分散，形成氣泡或塊狀物少之漿液。 粉末CTA和部份水的預混合，利用捏合裝置進行。捏 合裝置是將混末CTA在水存在下加以捏合之裝置，可用 一般性的捏合裝置。此等捏合裝置，若容器轉動型可爲 球磨機形；容器固定型，則有水平軸旋轉式刮刀形、滾 輪形、螺桿形、圓板形，以及垂直軸旋轉式刮刀形，平 輪形，高速流動形、旋轉圓板形、搖動旋轉形；容器振 1239948 五、發明說明（5 ) 動型有振動磨機，以連續式爲佳。 最好的捏合裝置有旋轉因板形混合裝置，是利用水平 乃向配置之旋轉圓板將粉末CTA按徑向送出，並與水混 合，令混合物在狹窄的曲折狀阻礙路徑移動，使之均質 化。 於此捏合裝置，將粉末CTA和部份水進行混合，使 CTA濃度爲55-75重量％，以60-70重量％爲佳，將附著 於粉末C T A的氣泡分離，使粉末c T A與水呈均勻混合， 而形成均質化預混合物。 如此所得預混合物除去氣泡，係水與CTA呈均勻混合 之狀態，再與剩餘水導入漿液調製槽，加以攪拌棍合， 粉末CTA呈均勻分散，形成均質化漿液。此時的混合機 構可用具有旋轉式攪拌槳葉之混合槽等，向來調製漿液 所用者。 此時漿液的CTT濃度如前所述，惟在此情形下，因預 混合物中除去氣泡而塊狀物少，故漿液濃度高，容易溶 解，且漿液濃度可接近溶解度。 如此所得漿液因加熱使CTA溶解，成爲對苯二甲酸溶 液，導入反應器內進行加氫處理。加氫處理所用反應器， 只要能在內部充塡觸觸，與CTA水溶液接觸之狀態供氫 即可，其形狀、構造等不加限制。 較佳反應器係充塡固體觸媒，形成固定層，具有進路 和出路，使CTA水溶液可以通過，並宜具有供氫路，以 1239948 五、發明說明（6) 供應氫。CTA溶液可向上流動，惟以進路連接於反應器 上方，出路連接於下方，故向下流動爲佳，另供氫路連 接於反應器上方，使氫從上方供應爲佳。 加氫處理在正常狀態，是將CTA和水漿液加熱加壓到 溫度230°C以上，以240〜30(TC爲佳，壓力Ι-llMPa，以 3〜9 MPa爲佳，將對酞酸溶解，所得CTA水溶液供應至 反應器，於通過觸媒層時，並以CTA水溶液中的4 - CBA之 1.5倍莫耳以上，更好是2倍莫耳以上之流量供應氫氣， 進行加氫。加氫之反應溫度在230°C以上，以255〜30(TC 爲佳，壓力1〜llMPa以3〜9MPa (錶計壓力）爲佳，氫分壓爲 〇.〇5MPa以上，以〇.〇5〜2MPa左右爲佳。 利用加氫處理，使CTA中的4 - CBA還原爲水溶性對苯乙 酸，在300°C以下，更好是在1〇〇〜280t晶析，進行固液 分離，從對酞酸漿液分離對苯乙酸，而得精製對酞酸。此 精製對酞酸再經水漿液化，令附著結晶之異物向水側移動， 然後進行固液分離和乾燥，製成高純度對酞酸（PTA)。 發明效果 . 按照本發明，粉末CTA和一部份水捏合形成預混合物， 此預混合物與剩餘水混合，形成漿液，可促進氣泡分離， 將粉末CTA均勻分散，形成高溫度水漿液，以良好效率進 行加氫反應，因此即可以良好效率製造PTA。 發明之實施形態 茲就附圖說明本發明之實施形態。 1239948 五、發明說明（7) 第1圖爲PTA製法之實施例流程圖。 在第1圖中，PTA之製造是先將粉末CTA1與一部份水2a， 供至捏合裝置3進行預混合，形成55〜75重量％濃度之預 混合物4 ,再與其他水2b —同供至漿液調製槽5，必要時再 供應其他水（補給水）2 c ,攪拌形成漿液。此漿液經加熱加壓， 把CTA溶解，將此CTA水溶液6和氫7供應至加氫反應器 8，進行加氫處理。加氫處理後之反應液9經減壓，冷卻， 導入晶析槽1 0內進行晶析。 生成之漿液1 1導入固液分離裝置1 2，進行固液分離。固 液分離通常以複數段進行，前段之分離液13a做爲廢水排 出，後段的固液分離是供水（洗淨水）2d再漿液化，經固液 分離，此後段分離液1 3b即做爲水2a，2b循環。 分離之結晶1 4在乾燥器1 5內乾燥，製成PTA 1 6。 第2圖爲捏合裝置3斷面圖，使用垂直軸旋轉式之旋轉 圓板形捏合裝置。捏合裝置3利用垂直旋轉軸2 1旋轉，在 水平方向配置的旋轉圓板22中心部開啓CTA供應路23，在 其前端周圍經環狀間隙24設有圓圈盤狀隔板25,與旋轉圓 板22大約平行，周邊部加厚，從上、下側被覆此等周緣部 的導板26, 27之周邊部間，形成曲折狀阻礙路28。29爲包 圍CTA供應路23所設水供應路，30爲外殻。 捏合裝置3利用旋轉軸2 1轉動旋轉圓板22，由CTA供 應路23供應粉末CTA，由水供應路29供水2a,CTA供應路 23出來的粉末CTA1碰到旋轉圓板22，按徑向流動，與間隙 1239948 五、發明說明（8) 2 4流出的水混合，在周邊方向呈渦形流動，與隔板2 5上側 流出的水混合，呈曲折狀流過阻礙路28,藉此將粉末CTA 和水預混合，氣泡分離，使粉末CTA和水均勻混合，形成 均質的預混合物4。 如此均質化之預混合物4在漿液調製槽5中，與水2b, 2 c攪拌、混合，使粉末CTA不會結塊，而均勻分散水中，形 成均質化漿液。因此，即使提高漿液的CTA濃度，在加熱 加壓時，可幾乎完全溶解，而得均勻TA水溶液，可於加氫 反應器8中提高加氫處理之反應效率。 以上舉例係使用旋轉圓板形捏合裝置，惟亦可使用其他 形式。在固液分離裝置1 2中，經固液分離之結晶1 4即可 加以乾燥，但亦可對分離的結晶1 4加水，再度水漿液化， 將此再度水漿液化之漿液，經固液分離而精製。 實施例 茲說明本發明實施例如下。 參考例 在·具有旋轉漿葉式攪拌機之第]•圖所示漿液調製槽5, 導入CTA200公斤和水800公斤，攪拌混合形成20重量％漿 液，靜置30分鐘，觀察相分離狀態。 實施例1和2 .參考例2 於第2圖所示旋轉圓板形捏合裝置3 ,導入粉末CTA和部 份水加以捏合，預混合物再與其餘水，按參考例1導入第 1圖所示漿液調製槽5內，攪拌混合，調製20重量％漿液， -10- 1239948 五、發明說明（9) 同樣靜置30分鐘後，觀察分離狀態。 上述結果如表1所示。 表1 靜置30分鐘後容積 比例（容量％) 氣泡 浮遊CTA 水 漿液 參考例1 直接調製20wt%漿液 4 27 43 26 參考例2 8〇wt%捏合— 2〇wt%漿液 80重量％預混合物爲粉末狀、漿液 化困難。 實施例1 70wt%捏合 2〇wt%漿液 1 0 4 95 實施例2 60wt%捏合 2〇wt%獎液 1 0 2 97 參考例3 5〇wt%捏合 2〇wt%漿液 7 9 35 49 由表1結果可知，粉末CTA和部份水捏合，形成55-75 重量％，尤其是60〜70重量％濃度之預混合物，再與剩餘水 混合，形成漿液，可以減少氣泡加浮遊CTA，而得均質化漿 液。 -11- 1239948 五、發明說明（1〇) 符號之說明 1 ......CTA(粗製對酞酸） 2 ......水 3 ......捏合裝置 4 ......預混合物 5 ......獎液調製槽 6 ......CTA水溶液 7 ......氫 8 ......加氫反應器 9 ......反應液 10 .....晶析槽 11 .....漿液 12 .....固液分離裝置 1 3.....分離液 14 .....結晶 15 .....乾燥器 16 .....PTA(高純度對酞酸） 21 .....垂直旋轉軸 22 .....旋轉圓盤 23 .....CTA供應路 24 .....環狀間隙 25 .....隔板 26,27..導板 28 .....阻礙路 29 .....水供應路 30 .....外殼 -12-1239948 V. Description of the invention (ι) Technical scope of the invention The present invention relates to a method for preparing high-purity terephthalic acid (hereinafter referred to as PTA), which is a crude terephthalic acid (hereinafter referred to as CTA) obtained by liquid-phase oxidation of para-xylene. Obtained from hydroprocessing. Conventional technology When para-xylene is oxidized with a molecular oxygen-containing gas, in addition to terephthalic acid (hereinafter referred to as TA), a CTA containing 4-carboxybenzaldehyde (hereinafter referred to as 4-CBA) as a major impurity is formed. However, when manufacturing polyester fibers, pTA is required as a raw material, and the above-mentioned CTA must be refined. For the production of PTA, a method for hydrotreating CTA in the presence of a hydrogenation catalyst is known (for example, Japanese Patent Application Laid-Open No. 4-6 6 5 5 3). Due to hydrogenation, 4-CBA can be reduced to water-soluble p-phenylacetic acid even at low temperatures. After crystallization, solid-liquid separation, etc., p-phenylacetic acid is separated from terephthalic acid to make PTA. The above-mentioned hydrogenation treatment forms a fixed layer of a solid catalyst in the reactor, and a CTA aqueous solution passes through the catalyst layer to supply hydrogen at the same time. At this time, the CTA aqueous solution is prepared by dispersing CTA powder in water to form a slurry, and heating to dissolve CTA in water. In order to perform the reaction with good efficiency at this time, the concentration of the formed slurry should be equivalent to the solubility of terephthalic acid when heated. Conventionally, the slurrying of CTA is generally carried out by introducing water and powdered CTA into a water slurry preparation tank having a rotating stirring blade, and stirring to form a slurry. This method is to continuously supply water and powdered CTA while agitating the liquid in the slurry preparation tank to disperse the powdered CTA in water. However, because the affinity of powder CTA and water is not high, it will be in a state containing bubbles. 1239948 V. Description of the invention (2) Dispersion 9 Bubbles are difficult to separate. In the bubble-containing state, the powdered CTA will flow in a block shape and will not dissolve when heated. When it flows into the hydrogenation reactor in a block shape, it will collect in the hydrogenation catalyst layer, causing blockage. To prevent this, the amount of powdered CTA dispersed has been reduced to form a low-concentration aqueous slurry, which reduces the amount of CTA that becomes a bubble-like mass, so that it can be dissolved by heating. However, when supplying a low-concentration slurry, the efficiency of the hydrogenation reaction decreases, which is a problem. The object of the present invention is to provide a method for producing high-purity terephthalic acid, which can promote the decomposition of air bubbles, uniformly disperse the powder CAT, form a high-concentration aqueous slurry, and perform the hydrogenation reaction with good efficiency. Therefore, PTA can be produced with good efficiency. ') The present invention is a method for producing high-purity terephthalic acid described below. 1. A method for purifying terephthalic acid, which is a process of mixing the crude terephthalic acid obtained by liquid-phase oxidation of p-xylene with water to form a slurry. The slurry is heated to form a crude terephthalic acid solution, which is present in a hydrogenation catalyst. Hydrogenation treatment to produce pure terephthalic acid, which is characterized in that the powdered crude terephthalic acid and a part of water are pre-mixed in a kneading device to form a premix having a concentration of 55 to 75 wt%. Mixed with the remaining water to form a slurry, and subjected to hydrotreating. 0 2. As for the remaining method of item (1), it is premixed by a continuous kneading device. 03. As for the method of item (1) above, it is used. The rotation arranged in the horizontal direction -4- 1239948 V. Description of the invention (3) Turn the circular plate to send the powder CTA in a radial direction and mix it with water to make the mixture obstruct the path movement in a narrow zigzag shape and homogenize it. A rotating disc-shaped kneading device performs premixing. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flowchart of an example of a method for producing a high-purity terephthalic acid; and FIG. 2 is a cross-sectional view of a kneading device. Lingming detailed description The crude terephthalic acid (CAT) of the hydrotreating object of the present invention is a crude terephthalic acid obtained by the liquid-phase oxidation of p-xylene. These terephthalic acids generally contain the main impurity 4-CBA0.1 to about 0.4% by weight. The above-mentioned liquid-phase oxidation of p-xylene is performed using a solvent and a catalyst. The solvents used in the liquid-phase oxidation of p-xylene include fatty acids such as acetic acid, propionic acid, n-butyric acid, isobutyric acid, n-valeric acid, trimethylacetic acid, and hexanoic acid, or mixtures with water. Among them, acetic acid or an aqueous acid described later is preferred. The liquid-phase oxidation catalysts of para-xylene are generally heavy metal compounds and / or bromine-containing compounds, the former being nickel, cobalt, iron, chromium, manganese, etc., both of which are elemental forms or compounds to dissolve in the form of the reaction system Better to use. Cobalt compounds, manganese compounds, and bromine compounds are preferred. The amount of cobalt compounds is usually 10 to 10,000 ppm of cobalt in the solvent, preferably 100 to 3000 ppm. For manganese compounds, the atomic ratio of manganese to cobalt is 0.001 to 2. Similarly, the atomic ratio of the bromine compound to cobalt is 0.1 to 5. Liquid-phase oxidation of para-xylene is performed using a molecular oxygen-containing gas. These oxygen-containing gases are usually oxygen diluted with an inert gas, such as air 1239948 5. Invention Description (4) or oxygen-enriched air. The temperature of the oxidation reaction is usually from 150 to 270 ° C, preferably from 170 ° C to 220 ° C. The pressure must be at least the pressure at which the mixture remains in the liquid phase at the reaction temperature, usually 0.5 to 4 MPa. (Gauge pressure). Moreover, the response time depends on the size of the device, etc., but usually the residence time is about 20 to 180 minutes. The water concentration in the reaction system is usually 3 to 30% by weight, and preferably 5 to 15% by weight. The CTA obtained from the above-mentioned liquid-phase oxidation reaction is introduced into a reactor, and is subjected to a hydrogenation treatment in the presence of a hydrogenation catalyst to produce PTA. At this time, the CTA separated from the mother liquor in the liquid-phase oxidation reaction is liquefied with water, and the obtained The aqueous slurry is heated and pressurized, and is introduced into the reactor with an aqueous terephthalic acid solution, and is subjected to a hydrogenation treatment. Generally, the CTA concentration of the slurry is 10 to 40% by weight, preferably 20 to 30% by weight, but the concentration corresponding to the solubility during heating and pressurizing is preferred. In the present invention, to form a slurry, a part of powder CTA is pre-mixed with water using a kneading device to form a pre-mixture with a concentration of 55-75 wt%, preferably 60 to 70 wt%. This pre-mix is then mixed with the remaining water. Mix to make the powder CTA uniformly dispersed to form a slurry with few bubbles or lumps. The pre-mixing of the powder CTA and part of the water is performed by a kneading device. The kneading device is a device for kneading the mixed CTA in the presence of water, and a general kneading device can be used. For these kneading devices, if the container rotating type can be a ball mill shape, the container fixed type can be a horizontal axis rotary blade shape, a roller shape, a screw shape, a disc shape, and a vertical axis rotary blade shape, a flat wheel shape, and high-speed flow. Shape, rotating disc shape, shaking and rotating shape; container vibration 1239948 V. Description of the invention (5) The moving type has a vibration mill, preferably a continuous type. The best kneading device is a rotating plate mixing device, which uses a rotating circular plate arranged horizontally to send the powder CTA in a radial direction and mixes it with water to make the mixture move in a narrow zigzag shape and obstruct the path, making it homogeneous. Into. In this kneading device, the powder CTA and a part of water are mixed so that the CTA concentration is 55-75% by weight, preferably 60-70% by weight. The air bubbles adhering to the powder CTA are separated to make the powder cTA and water present. Mix uniformly to form a homogenized premix. The premix thus obtained removes air bubbles, and the water and CTA are in a state of being uniformly mixed, and then introduced into the slurry preparation tank with the remaining water, followed by stirring and sticking, and the powder CTA is uniformly dispersed to form a homogenized slurry. In this case, the mixing mechanism can be prepared by using a mixing tank or the like having a rotary stirring blade. At this time, the CTT concentration of the slurry is as described above, but in this case, there are fewer lumps due to the removal of bubbles in the premix, so the slurry concentration is high, it is easy to dissolve, and the slurry concentration can approach the solubility. The slurry thus obtained was heated to dissolve the CTA to become a terephthalic acid solution, which was introduced into the reactor and subjected to a hydrogenation treatment. The reactor used for the hydrotreating treatment is only required to be capable of supplying hydrogen in a state in which it is in contact with the CTA aqueous solution, and its shape and structure are not limited. The preferred reactor is filled with solid catalyst to form a fixed layer, which has an inlet and outlet to allow the CTA aqueous solution to pass through. It should also have a hydrogen supply path to supply hydrogen according to 1239948 V. Description of the invention (6). The CTA solution can flow upward, but the inlet is connected to the upper part of the reactor and the outlet is connected to the lower part, so it is better to flow downward, and the hydrogen supply path is connected to the top of the reactor so that the hydrogen is supplied from above. The hydrotreating is in a normal state. The CTA and water slurry are heated and pressurized to a temperature above 230 ° C, preferably 240 ~ 30 (TC is preferred, the pressure is 1-11 MPa, and preferably 3 ~ 9 MPa, which dissolves the terephthalic acid. The obtained CTA aqueous solution is supplied to the reactor, and when passing through the catalyst layer, hydrogen is supplied at a flow rate of 1.5 times more than 4 CBA in the CTA aqueous solution, more preferably 2 times more than Molar, for hydrogenation. The reaction temperature of hydrogen is above 230 ° C, preferably 255 to 30 (TC is preferred, pressure is 1 to 11 MPa is preferably 3 to 9 MPa (gauge pressure), and the hydrogen partial pressure is above 0.05 MPa to 0.05 About 2 MPa is preferred. Hydrogenation treatment is used to reduce 4-CBA in CTA to water-soluble p-phenylacetic acid, which is crystallized at 300 ° C or lower, more preferably at 100 to 280 t, and subjected to solid-liquid separation. The terephthalic acid slurry is separated from p-phenylacetic acid to obtain purified terephthalic acid. This purified terephthalic acid is then liquefied in an aqueous slurry to move the foreign matter attached to the crystal to the water side, and then solid-liquid separation and drying are performed to make a high-purity pair. Phthalic acid (PTA). Effect of the invention. According to the present invention, the powder CTA and a part of water are kneaded to form a premix, and this premix Mixed with the remaining water to form a slurry, which can promote the separation of bubbles, uniformly disperse the powder CTA, form a high temperature water slurry, and perform the hydrogenation reaction with good efficiency, so the PTA can be manufactured with good efficiency. Embodiments of the invention are shown in the drawings Explain the embodiment of the present invention. 1239948 V. Description of the invention (7) The first diagram is a flowchart of an embodiment of the PTA method. In the first diagram, the PTA is manufactured by first supplying powder CTA1 and a portion of water 2a to The kneading device 3 is premixed to form a premix 4 having a concentration of 55 to 75% by weight, and then supplied to the slurry preparation tank 5 with other water 2b, and if necessary, other water (supply water) 2c is supplied and stirred to form a slurry. This slurry is heated and pressurized to dissolve CTA, and this CTA aqueous solution 6 and hydrogen 7 are supplied to a hydrogenation reactor 8 for hydrogenation treatment. The reaction solution 9 after the hydrogenation treatment is depressurized, cooled, and introduced into a crystallization tank. Crystallize within 10. The resulting slurry 11 is introduced into the solid-liquid separation device 12 to perform solid-liquid separation. The solid-liquid separation is usually performed in multiple stages. The separation liquid 13a in the previous stage is discharged as waste water, and the solid-liquid separation in the later stage is Water supply (Washing water) 2d and then slurried, and after solid-liquid separation, the subsequent separation liquid 1 3b is circulated as water 2a, 2b. The separated crystals 14 are dried in a desiccator 15 to make PTA 16. 6. Section 2 The figure is a cross-sectional view of the kneading device 3, which uses a rotating disk-shaped kneading device of a vertical axis rotation type. The kneading device 3 is rotated by a vertical rotating shaft 21, and the center of the rotating disk 22 arranged in the horizontal direction opens the CTA supply path 23, A circular disk-shaped partition plate 25 is provided around the front end via an annular gap 24, which is approximately parallel to the rotating circular plate 22, and the peripheral portion is thickened, and the peripheral portions of the guide plates 26, 27 covering these peripheral portions from the upper and lower sides are covered. At the same time, a meandering obstacle path 28 is formed. 29 is a water supply path provided around the CTA supply path 23, and 30 is a casing. The kneading device 3 uses the rotating shaft 21 to rotate the rotating circular plate 22, and the powder CTA is supplied by the CTA supply channel 23. The water is supplied 2a by the water supply channel 29. The powder CTA1 from the CTA supply channel 23 hits the rotating circular plate 22 and flows in a radial direction. It is mixed with the gap 1239948 V. Description of the invention (8) 2 4 The water flowing out flows in a vortex in the peripheral direction, mixes with the water flowing out of the upper side of the partition plate 25 and flows in a zigzag way through the obstructing path 28, thereby powdering CTA and water are pre-mixed, and the air bubbles are separated, so that the powder CTA and water are evenly mixed to form a homogeneous pre-mix 4. The homogenized premix 4 is stirred and mixed with the water 2b, 2c in the slurry preparation tank 5 so that the powdered CTA does not agglomerate, and the water is evenly dispersed to form a homogenized slurry. Therefore, even if the CTA concentration of the slurry is increased, it can be almost completely dissolved when heated and pressurized to obtain a homogeneous TA aqueous solution, which can improve the reaction efficiency of the hydrogenation treatment in the hydrogenation reactor 8. The above examples use a rotating disk-shaped kneading device, but other forms can also be used. In the solid-liquid separation device 12, the crystals 14 separated by the solid-liquid separation can be dried, but the separated crystals 14 can also be added with water to liquefy the water again. Separated and refined. Examples Examples of the present invention will be described below. Reference example: [No. 1 with a rotary paddle type mixer] • The slurry preparation tank 5 shown in the figure is introduced with 200 kg of CTA and 800 kg of water, stirred and mixed to form a 20% by weight slurry, and allowed to stand for 30 minutes to observe the phase separation state. Examples 1 and 2. Reference Example 2 Rotate the circular plate-shaped kneading device 3 shown in FIG. 2 and introduce the powder CTA and part of the water to knead the pre-mixture with the remaining water. In the slurry preparation tank 5, stir and mix to prepare 20% by weight slurry. -10- 1239948 V. Description of the invention (9) After standing still for 30 minutes, observe the separation state. The above results are shown in Table 1. Table 1 Volume ratio (volume%) after standing for 30 minutes Bubble floating CTA water slurry Reference Example 1 Direct preparation of 20wt% slurry 4 27 43 26 Reference Example 2 80wt% kneading—20wt% slurry 80wt% premix is It is difficult to form powder and slurry. Example 1 70wt% kneading 20wt% slurry 1 0 4 95 Example 2 60wt% kneading 20wt% prize liquid 1 0 2 97 Reference example 3 50wt% kneading 20wt% slurry 7 9 35 49 From the table 1 The results show that the powder CTA and some water are kneaded to form a premix with a concentration of 55-75% by weight, especially 60 ~ 70% by weight, and then mixed with the remaining water to form a slurry, which can reduce air bubbles and float the CTA to obtain a homogeneous Chemical slurry. -11- 1239948 V. Description of the invention (10) Explanation of symbols 1 ... CTA (crude terephthalic acid) 2 ... Water 3 ... Kneading device 4 ... ... pre-mixture 5 ... preparation solution preparation tank 6 ... CTA aqueous solution 7 ... hydrogen 8 ... hydrogenation reactor 9 ... .Reaction liquid 10 ..... Crystallization tank 11 ..... Slurry 12 ..... Solid-liquid separation device 1 3 ... Separation liquid 14 ..... Crystallization 15 .... .Drier 16 ..... PTA (High-purity terephthalic acid) 21 .... Vertical rotation axis 22 ..... Rotating disc 23 ..... CTA supply path 24 ..... Ring gap 25 ..... partition 26, 27 .. guide plate 28 .... obstruction path 29 ..... water supply path 30 ..... shell -12-