200944476 九、發明說明： 【發明所屬之技術領域】 本發明是有關於一種連續式碳化裝置及碳化方法，且 特別是有關於一種於負壓環境下進行碳化的連續式碳化 裝置及碳化方法。 【先前技術】 碳化裝置的應用範疇廣泛，諸如應用於碳纖維織物的 製造上。現有的連續式碳化裝置及方法，係於碳化裝置的 一碳化腔體中施以高溫並通入大量惰性氣體，如氮氣 (N2)。藉此，當原材料（如一織物）被送入碳化腔體中進行 碳化時，惰性氣體可排除原材料與空氣中的氧產生接觸， 以於高溫製程下使原材料所含的非碳元素，自原材料本體 脫除而留下碳元素（即如碳纖維織物）。 由於是通入大量惰性氣體於碳化腔體中，因此碳化腔 體中會處於正壓氣氛（相較於碳化腔體外的大氣氣氛），亦 即碳化腔體中的氣體壓力會大於碳化腔體外的大氣壓力。 然而，在正壓的環境下，非碳元素較不易脫除且脫除 氣體會充滿腔内，故造成灰份的增加、焦油的產生及碳化 程度的降低（因原材料内非碳元素於正壓氣氛下不易自原 材料本體脫除而影響碳層的重新排列）。 因此’需要有一種改良的連續式碳化裝置及碳化方 法，來解決前述問題。 200944476 【發明内容】 因此本發明的目的就是在提供一種連續式碳化裳置 及碳化方法，係於負壓的碳化腔體對原材料進行碳化，碳 化腔體的壓力係小於一大氣壓，而為一負壓狀態。 依照本發明之一種連續式負壓碳化裝置，包含供料裝 置、腔體裝置以及收料裝置。供料裝置提供一原材料。腔 體裝置接收並碳化原材料。 腔體裝置包含碳化裝置以及兩緩衝裝置。碳化裝置具 有碳化腔體，碳化腔體具有進料口以及出料口。緩衝裝置 刀別連接於進料口以及出料口。收料裝置收集經碳化的原 材料。當原材料於碳化腔體中進行碳化時，碳化腔體的壓 力係為一小於一大氣壓的負壓狀態。 依照本發明之一種連續式負壓碳化方法，包含提供一 連續式的原材料。接著使用碳化腔體碳化原材料，當原材 料於碳化腔體中進行碳化時，碳化腔體的壓力係為一小於 一大氣壓的負壓狀態。 取據本發明所能達成的功效在於： 當原材料於碳化腔體中進行碳化時，碳化腔體中所產 生的非碳氣體脫除容易。經碳化的原材料（即產品）碳層排 列較整齊’且碳化程度較高。 同時’碳化腔體中產生的灰份較少（避免脫除氣體與經 碳化的原材料，如碳布反應）。經碳化的原材料，如碳布均 勻度南。 最後’由於不需一直供應大量氮氣，加上緩衝裝置的 6 200944476 設計已能隔絕了連續製程中外來空氣中氧的影響，使得能 源消耗惰性氣體(如氮氣)需求量少，同時熱損耗少(大量: 性氣體如氮氣進入碳化腔體内會帶走熱量）。 【實施方式】 依照本發明之連續式碳化裝置及碳化方法，係於碳化 裝置的碳化腔體中，提供一種負壓環境，當原材料進入碳 化腔體中時，係於負壓環境進行碳化。本發明之應用包含 但不限於碳纖維織物’以可應用於其他可連續供料以及收 料的原材料之碳化製程。為方便說明，以下實施例係以纖 維織物的碳化為例說明。 請參照第1圖，其緣示依照本發明一第一實施例的一 種碳化裝£ 1〇〇,包含供料裝i 11〇、腔體裝置12〇、收料 裝置130、供氣裝置140、熱交換器15〇以及抽氣裝置 供料裝置11G係可包含複數輥輪⑴，藉由輥#⑴供應 原材料200以及控制原材料2〇〇的張力。在本實施例中， 原材料200為一纖維織布。 原材料200經過腔體裝置12〇後，會被碳化為碳纖維 織布’並由收料裝置13〇收集。 腔體裝i 120包含一碳化裝£ 121以及複數緩衝裝置 122。緩衝裝置122係分別設於碳化裝置121的進料口以 及出料π位置。在本實施例中，碳化裝置121包含一碳化 腔體123，各緩衝裝置122包含一緩衝腔體124。各緩衝 裝置122的緩衝腔體124也可以依照實際需求配置為複數 200944476 個。碳化裝置121另設有一氣滌口 125，連通於碳化腔體 123以對碳化腔髏123進行氣滌。 供氣裝置140係分別連通於緩衝腔體124以及碳化腔 體123，以提供緩衝腔體124以及碳化腔體123惰性氣體， 如氮氣。供氣裝置140包含控制閥（如圖中之vi以及V2)， 以配合壓力計量計（如圖中之P1以及P2)分別控制進入緩 衝腔體124的氣體流量，使緩衝腔體124保持於正壓狀態 (相對於碳化腔體123);供氣裝置140另包含控制閥（如圖 中之V4)，以配合氧計量計126控制進入碳化腔體123的 惰性氣體氣滌量。 抽氣裝置160係連通於碳化腔體123，以抽出其中碳 化原材料所產生的氣體’抽氣裝置160包含控制閥（如圖中 之V3) ’以配合壓力計量計（如圖中之P3)控制抽出碳化腔 體123的氣體流量，使碳化腔體123保持於負壓狀態（相對 於緩衝腔體124)。 熱交換器150係設於腔體裝置120與供氣裝置14〇以 及抽氣裝置160之間，使抽氣裝置160所抽出之高溫的碳 化氣體與供氣裝置140之惰性氣體進行熱交換以加熱惰性 氣體® 在本實施例中，緩衝腔體124的壓力維持大於76〇托 耳（Τ〇ΓΓ)，亦即大於一大氣壓（P2、Pl> latm> P3)。碳化 腔體123的壓力維持於托耳之間，亦即小於一大氣 壓。在原材料200進入碳化腔體123之前，藉由氣滌口 ι25 通入惰性氣體，如氮氣進入碳化腔體123，以降低腔内空 8 200944476 氣氧含量。 魯BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a continuous carbonization apparatus and a carbonization method, and more particularly to a continuous carbonization apparatus and a carbonization method for carbonization in a negative pressure environment. [Prior Art] The carbonization apparatus has a wide range of applications, such as application to the manufacture of carbon fiber fabrics. The existing continuous carbonization apparatus and method is applied to a carbonization chamber of a carbonization apparatus at a high temperature and is supplied with a large amount of an inert gas such as nitrogen (N2). Thereby, when a raw material (such as a fabric) is fed into the carbonization chamber for carbonization, the inert gas can exclude the raw material from coming into contact with oxygen in the air to make the non-carbon element contained in the raw material from the raw material body in a high-temperature process. Remove to leave carbon (ie, such as carbon fiber fabric). Since a large amount of inert gas is introduced into the carbonization chamber, the carbonization chamber is in a positive pressure atmosphere (compared to the atmosphere outside the carbonization chamber), that is, the gas pressure in the carbonization chamber is greater than that outside the carbonization chamber. Atmospheric pressure. However, in a positive pressure environment, non-carbon elements are less likely to be removed and gas removal will fill the cavity, resulting in an increase in ash content, tar production and a reduction in carbonation (because the non-carbon elements in the raw material are at positive pressure) It is not easy to remove from the raw material body under the atmosphere and affect the rearrangement of the carbon layer). Therefore, there is a need for an improved continuous carbonization apparatus and carbonization method to solve the aforementioned problems. SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a continuous carbonization skirting and carbonization method for carbonizing a raw material in a negative pressure carbonization chamber, the pressure of the carbonization chamber being less than one atmosphere, and being a negative Pressure state. A continuous negative pressure carbonization apparatus according to the present invention comprises a supply device, a cavity device, and a receiving device. The feeding device provides a raw material. The cavity device receives and carbonizes the raw materials. The cavity device comprises a carbonization device and two buffer devices. The carbonization unit has a carbonization chamber having a feed port and a discharge port. Buffer device The knife is connected to the feed port and the discharge port. The receiving device collects the carbonized raw material. When the raw material is carbonized in the carbonization chamber, the pressure of the carbonization chamber is a negative pressure state of less than one atmosphere. A continuous negative pressure carbonization process in accordance with the present invention comprises providing a continuous raw material. Next, the carbonization chamber is used to carbonize the raw material. When the raw material is carbonized in the carbonization chamber, the pressure of the carbonization chamber is a negative pressure state of less than one atmosphere. The effect that can be achieved according to the present invention is that the removal of non-carbon gas generated in the carbonization chamber is easy when the raw material is carbonized in the carbonization chamber. The carbonized raw material (i.e., product) has a relatively uniform carbon layer and a high degree of carbonization. At the same time, the amount of ash produced in the carbonization chamber is less (to avoid the removal of gases and reaction with carbonized raw materials such as carbon cloth). The carbonized raw materials, such as carbon cloth, are evenly distributed. Finally, 'there is no need to supply a large amount of nitrogen all the time, plus the buffer device's 6 200944476 design can isolate the influence of oxygen in the external air in the continuous process, so that the energy consumption of inert gas (such as nitrogen) is less, and the heat loss is small ( Large amount: Sex gases such as nitrogen entering the carbonization chamber will carry away heat). [Embodiment] The continuous carbonization apparatus and the carbonization method according to the present invention are provided in a carbonization chamber of a carbonization apparatus to provide a negative pressure environment for carbonization in a negative pressure environment when the raw material enters the carbonization chamber. Applications of the present invention include, but are not limited to, carbon fiber fabrics as a carbonization process that can be applied to other raw materials that can be continuously fed and received. For convenience of explanation, the following examples illustrate the carbonization of the fiber fabric as an example. Please refer to FIG. 1 , which illustrates a carbonization device according to a first embodiment of the present invention, comprising a feeding device i 11 , a cavity device 12 , a receiving device 130 , a gas supply device 140 , The heat exchanger 15A and the suction device supply device 11G may include a plurality of rollers (1), which supply the raw material 200 by the roller #(1) and control the tension of the raw material 2〇〇. In the present embodiment, the raw material 200 is a fiber woven fabric. After the raw material 200 passes through the cavity device 12, it is carbonized into a carbon fiber woven fabric' and collected by the receiving device 13〇. The cavity mount i 120 includes a carbonized package 121 and a plurality of buffers 122. The buffering device 122 is provided at the feed port of the carbonization device 121 and the discharge π position, respectively. In the present embodiment, the carbonization device 121 includes a carbonization chamber 123, and each of the buffer devices 122 includes a buffer chamber 124. The buffer cavity 124 of each buffer device 122 can also be configured as a plurality of 200944476 according to actual needs. The carbonization device 121 is further provided with a gas scrubbing port 125 connected to the carbonization chamber 123 to gas-carbonize the carbonization chamber crucible 123. The gas supply unit 140 is connected to the buffer chamber 124 and the carbonization chamber 123, respectively, to provide a buffer chamber 124 and a carbonization chamber 123 inert gas such as nitrogen. The gas supply device 140 includes control valves (vi and V2 in the figure) to control the flow rate of the gas entering the buffer chamber 124 in conjunction with the pressure meter (P1 and P2 in the figure) to keep the buffer chamber 124 in positive The pressure state (relative to the carbonization chamber 123); the gas supply device 140 further includes a control valve (V4 in the figure) to control the inert gas gas amount entering the carbonization chamber 123 in conjunction with the oxygen meter 126. The air extracting device 160 is connected to the carbonization chamber 123 to extract the gas generated by the carbonized raw material. The air extracting device 160 includes a control valve (V3 in the figure) to be controlled by a pressure meter (P3 in the figure). The gas flow rate of the carbonization chamber 123 is extracted to maintain the carbonization chamber 123 in a negative pressure state (relative to the buffer chamber 124). The heat exchanger 150 is disposed between the cavity device 120 and the air supply device 14A and the air suction device 160, and heat-exchanges the high-temperature carbonized gas extracted by the air suction device 160 with the inert gas of the air supply device 140 to heat Inert Gas® In this embodiment, the pressure of the buffer chamber 124 is maintained to be greater than 76 Torr, i.e., greater than one atmosphere (P2, Pl > latm > P3). The pressure of the carbonization chamber 123 is maintained between the ears, i.e., less than one atmospheric pressure. Before the raw material 200 enters the carbonization chamber 123, an inert gas such as nitrogen is introduced into the carbonization chamber 123 through the gas-washing port to reduce the oxygen content in the cavity. Lu
^製程中’碳化腔體⑵維持負壓。此外，碳化腔體 本*可設有一氧計量計126，設定碳化腔體123内氧濃度， 當碳化腔體m内氧濃度超過設定值時，可再度藉由氣： 125通入惰性氣體，如氮氣進入碳化腔體，以降低 内二氣氧含量，使氧濃度維持於丨1 範圍之間。 、另外，原材料200於碳化腔體123中的加熱時間為i 分鐘到25分鐘。原材料2〇〇㈣力可為緊張化或無張力， 以控制原材料2〇〇的縮率及避免毀損。碳化腔體⑵中的 處理溫度為500。〇1200。(：之間。 请參照第2圖，其繪示依照本發明一第二實施例的一 種奴化裝置，第二實施例與第一實施例的特徵大致相同， 兩者的差異僅在於： 供氣裝置140係連通於碳化腔體123，以提供碳化腔 體123惰性氣體，如氮氣。供氣裝置14〇包含控制閥（如圖 中之V4)，以配合氧計量計126控制進入碳化腔體氣滌口 125惰性氣體通入之氣滌量。 抽氣裝置160係分別連通於緩衝腔體124及碳化腔體 123 ’以抽出其中的空氣。抽氣裝置16〇包含控制閥（如圖 中之VI、V2以及V3) ’以配合壓力計量計（如圖中之pi、 P2以及P3)分別控制抽出緩衝腔體124以及碳化腔體ία 的氣體流量’使緩衝腔體124以及碳化腔體123保持於負 壓狀態（相對於大氣壓力）。 在本實施例中，碳化腔體123的壓力大於緩衝腔體124 200944476 的壓力’即latm>P3>P1、P2。所以碳化腔體123中碳化 產生的氣體，會流入緩衝腔體124中，並由抽氣裝置16〇 ' 抽出排放。碳化腔體123的壓力維持於i — 760托耳之間， ，亦即小於一大氣壓。 於製程中，碳化腔體123維持負壓。此外，碳化腔體 123可設有一氧計量計126，設定碳化腔體123内氧濃度， 當碳化腔體123内氧濃度超過設定值時，可再度藉由氣滌 Ο 口 125通入惰性氣體，如氮氣進入碳化腔體123，以降低 腔内空氣氧含量，使氧濃度維持於lppm_1〇%範圍之間。 若取相同之PAN(PolyAcryloNitrile)聚丙烯腈氧化 纖維布作為碳化之原料，分別以上述第一實施例之製程條 件（實驗組）以及現有業界使用之製程條件（對照組）進行加 工碳化，來製得碳纖維布。製程條件如下： 對照組之製程條件：（以生產50公尺之碳布為例） 溫度：1000°c ; 鲁熱處理時間：10分鐘； 張力：3.0-4.0公斤； 碳化腔體123之内壓力：大於（>)760 t〇r(N2通入碳化 腔體123内作為保護氣體）； 消耗功率：11 (Μ 15 KW/hr ; N2(總）用量：188公斤。 實驗組之製程條件：（以生產5〇公尺之碳布為例） 溫度：iooo°c ; 熱處理時間：10分鐘； 200944476 張力：3.0-4.0公斤； 碳化腔體123之内壓力：小於（< )76〇 tor (約450-500 tor)； 消耗功率：95-100 KW/hr ; N2(總）用量：1〇5公斤。 兩組所得之碳布，經測試可得下表之結果： 項 巨 碳層堆 疊厚度 Lc 碳層堆 疊長度 度La 密度 元素分析 表面電 阻 灰 份 nm nm g/cm3 C% N% H% 0% Ω/cm2 % 對 照 組 145.1 0.8028 1.8011 89.975 7.635 0.71 1.68 0.9132 0.86 實 驗 組 155.8 1.3302 1.7784 92.03 6.205 0.95 0.815 0.6523 0.12 經由上表可得知，依據本發明之負壓碳化方法，在製 程電力消耗降低13.4%，N2用量消耗降低44·1%。若進一 步分析連續式負壓碳化所生產碳纖維布微結構： 碳層堆疊厚度（Lc)增加7.4%，碳層堆疊長度（La)增加 65.7%’碳含量％增加2.28%;故可知依據本發明之製程相 對於同樣處理溫度下之現有製程，可增進材料碳化之程 度0 11 200944476 由微結構分析結果可進一步印證碳纖維布之表面電 阻值降低28.6%(意指導電度提高），碳化程度越高，導電 度越高。 因連續式負壓碳化製程會將材料排除之非碳元素抽 走，除碳化程度提高外亦使碳纖維布灰份降低，此實施例 灰份百分比（％)則降低86%。 雖然本發明已以數較佳實施例揭露如上，然其並非用 以限定本發明，任何熟習此技藝者，在不脫離本發明之精 神和範圍内’當可作各種之更動與潤飾，因此本發明之保 護範圍當視後附之申請專利範圍所界定者為準。 【圖式簡單說明】 為讓本發明之上述和其他目的、特徵、優點與實施例 能更明顯易懂，所附圖式之詳細說明如下： 第1圖係繪示依照本發明一第一實施例的一種連續式 負壓碳化裝置的示意圖。 第2圖係繪示依照本發明一第二實施例的一種連續式 負壓碳化裝置的示意圖。 125 :氣滌口 126 :氧計量計 130 :收料裝置 140 :供氣裝置 【主要元件符號說明】 100 :碳化裝置 11〇 :供料裝置 ill :輥輪 120 ·•腔體裝置 12 200944476 121 :碳化裝置 150 ： 122 :緩衝裝置 160 ： 123 :碳化腔體 200 ： 124 :緩衝腔體 熱交換器 抽氣裝置 原材料^ The carbonization chamber (2) in the process maintains a negative pressure. In addition, the carbonization chamber can be provided with an oxygen meter 126 to set the oxygen concentration in the carbonization chamber 123. When the oxygen concentration in the carbonization chamber m exceeds the set value, the inert gas can be again introduced by the gas: 125, such as Nitrogen enters the carbonization chamber to reduce the internal oxygen content and maintain the oxygen concentration between 丨1. In addition, the heating time of the raw material 200 in the carbonization chamber 123 is from 1 minute to 25 minutes. The raw material 2〇〇(4) force can be tensioned or tension-free to control the shrinkage of raw materials and avoid damage. The treatment temperature in the carbonization chamber (2) was 500. 〇1200. (: Between. Please refer to FIG. 2, which illustrates a enslaving device according to a second embodiment of the present invention. The second embodiment is substantially the same as the first embodiment, and the difference between the two is only: The device 140 is connected to the carbonization chamber 123 to provide an inert gas of the carbonization chamber 123, such as nitrogen. The gas supply device 14A includes a control valve (V4 in the figure) to control the entry into the carbonization chamber gas with the oxygen meter 126. The air pumping device 160 is connected to the buffer chamber 124 and the carbonization chamber 123' to extract air therein. The air extracting device 16〇 includes a control valve (VI in the figure). , V2 and V3) 'Control the gas flow rate of the extraction buffer chamber 124 and the carbonization chamber ία with the pressure meter (pi, P2 and P3 in the figure) to keep the buffer chamber 124 and the carbonization chamber 123 in In the present embodiment, the pressure of the carbonization chamber 123 is greater than the pressure of the buffer chamber 124 200944476, i.e., lamat > P3 > P1, P2. Therefore, the gas generated by carbonization in the carbonization chamber 123 Will flow into the buffer The chamber 124 is evacuated by the air extracting device 16'. The pressure of the carbonizing chamber 123 is maintained between i and 760 Torr, that is, less than one atmosphere. During the process, the carbonizing chamber 123 maintains a negative pressure. In addition, the carbonization chamber 123 may be provided with an oxygen meter 126 for setting the oxygen concentration in the carbonization chamber 123. When the oxygen concentration in the carbonization chamber 123 exceeds a set value, the inert gas may be again introduced through the gas cleaning port 125. For example, nitrogen enters the carbonization chamber 123 to reduce the oxygen content in the cavity, so that the oxygen concentration is maintained between 1 ppm and 1%. If the same PAN (PolyAcryloNitrile) polyacrylonitrile oxidized fiber cloth is used as the carbonization material, The process conditions (experimental group) of the first embodiment and the process conditions (control group) used in the prior art were processed and carbonized to obtain a carbon fiber cloth. The process conditions were as follows: Process conditions of the control group: (to produce 50 meters) Carbon cloth as an example) Temperature: 1000 ° C; Lu heat treatment time: 10 minutes; Tension: 3.0-4.0 kg; Pressure inside the carbonization chamber 123: greater than (>) 760 t〇r (N2 is introduced into the carbonization chamber 123 Internal work To protect the gas); Power consumption: 11 (Μ 15 KW / hr; N2 (total) dosage: 188 kg. Process conditions of the experimental group: (for the production of carbon cloth of 5 ft.) Temperature: iooo °c; Heat treatment time: 10 minutes; 200944476 Tension: 3.0-4.0 kg; Pressure inside the carbonization chamber 123: less than (<) 76〇tor (about 450-500 tor); Power consumption: 95-100 KW/hr; N2 ( Total) dosage: 1〇5 kg. The carbon cloth obtained from the two groups can be tested to obtain the following results: Item Thick Carbon Layer Stacking Thickness Lc Carbon Layer Stacking Length La Density Element Analysis Surface Resistance Ash Part nm nm g/cm3 C% N% H% 0% Ω /cm2 % Control group 145.1 0.8028 1.8011 89.975 7.635 0.71 1.68 0.9132 0.86 Experimental group 155.8 1.3302 1.7784 92.03 6.205 0.95 0.815 0.6523 0.12 As can be seen from the above table, the negative pressure carbonization method according to the present invention reduces the power consumption in the process by 13.4%, N2 The consumption was reduced by 44.1%. If the carbon fiber cloth microstructure produced by continuous negative pressure carbonization is further analyzed: the carbon layer stack thickness (Lc) is increased by 7.4%, the carbon layer stack length (La) is increased by 65.7%, and the carbon content % is increased by 2.28%; The process can increase the degree of carbonization of the material relative to the existing process at the same processing temperature. 0 11 200944476 The results of the microstructure analysis can further confirm that the surface resistance of the carbon fiber cloth is reduced by 28.6% (intended to improve the electrical conductivity), and the degree of carbonization is higher. The higher the conductivity. Because the continuous negative pressure carbonization process will remove the non-carbon elements from the material, the carbon fiber ash content is reduced in addition to the increased carbonization. The percentage of ash (%) in this example is reduced by 86%. While the present invention has been described above in terms of a preferred embodiment, it is not intended to limit the invention, and the invention may be modified and modified without departing from the spirit and scope of the invention. The scope of the invention is defined by the scope of the appended claims. BRIEF DESCRIPTION OF THE DRAWINGS The above and other objects, features, advantages and embodiments of the present invention will become more <RTIgt; An example of a continuous negative pressure carbonization unit. Figure 2 is a schematic view showing a continuous negative pressure carbonization apparatus in accordance with a second embodiment of the present invention. 125: gas scrubbing port 126: oxygen meter 130: receiving device 140: gas supply device [main component symbol description] 100: carbonizing device 11: feeding device ill: roller 120 · cavity device 12 200944476 121 : Carbonization device 150: 122: buffer device 160: 123: carbonization chamber 200: 124: buffer chamber heat exchanger suction device raw material
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