WO2007073658A1 - Procede de separation de l'acide terephtalique brut - Google Patents

Procede de separation de l'acide terephtalique brut Download PDF

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Publication number
WO2007073658A1
WO2007073658A1 PCT/CN2006/003045 CN2006003045W WO2007073658A1 WO 2007073658 A1 WO2007073658 A1 WO 2007073658A1 CN 2006003045 W CN2006003045 W CN 2006003045W WO 2007073658 A1 WO2007073658 A1 WO 2007073658A1
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Prior art keywords
pressure
zone
filter
filtration
filter cake
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PCT/CN2006/003045
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English (en)
French (fr)
Inventor
Taiping Huang
Weiye Tan
Hongbo Fan
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Action Perfect Engineering (Xiamen) Co., Ltd
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Publication of WO2007073658A1 publication Critical patent/WO2007073658A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption

Definitions

  • the present invention relates to a process for recovering crude terephthalic acid from a slurry containing acetic acid. Background technique
  • a centrifuge or a rotary vacuum filter is used in the solid-liquid separation process, that is, the material of the third crystallization tank is pumped into the centrifuge, and the coarse pair contained in the slurry is separated by centrifugal force.
  • Phthalic acid and mother liquor or pre-vacuum fully depressurized, cooled (temperature: 90 ⁇ , pressure -0.5 kg / cm 2 (gauge)) sent to the feed tank of the rotary vacuum filter, and then pumped to the rotation
  • the bottom hopper of the vacuum filter causes the suspension of the crystal in the acetic acid solvent by overflowing the partial slurry, so that the crystal is adsorbed on the rotating drum by the pressure difference between the inside and outside of the drum to achieve the purpose of filtration.
  • the rotary vacuum filter has a pressure drop due to filtration, which causes crystallization of the product on the filter cloth, the frequency of the alkali washing is high, which not only causes waste of the product and caustic soda, but also affects the normal operation of the production.
  • the filter cloth is damaged and needs to be replaced, it takes a long time, the repair cost is high, and the yield and product quality are affected.
  • the invention relates to a method for separating crude terephthalic acid (CTA), which adopts a rotary pressure filter, and the filter is divided into four functional zones: hydraulic filtration, acetic acid washing, air pressure filtration and blanking, and the filtration of the filter is always controlled.
  • CTA crude terephthalic acid
  • the temperature and pressure of the filter cloth are not crystallized; the filter cake with a moisture content of 12wt% is formed for drying; the impurity ash content of the product is less than 60ppm, and the ash content is effectively removed, and the catalyst of the hydrogenation reactor of the subsequent refining section can be increased.
  • a method for separating crude terephthalic acid (CTA) according to the present invention further comprising: a slurry containing acetic acid containing crude terephthalic acid crystals is sent to a hydraulic filtration zone of a rotary pressure filter to form a filter The cake, wherein the temperature and pressure on both sides of the filter cloth in the hydraulic filtration zone are maintained at a temperature and pressure in which the acid-containing slurry and the filtrate do not reach a state of being saturated to crystallize; the filter cake formed by the filtration is rotated into the next zone to be pickled.
  • CTA crude terephthalic acid
  • the filter cake is then rotated into the air pressure filter zone and squeezed and filtered by an inert gas.
  • the temperature and pressure on both sides of the filter cloth in the air pressure filter zone are maintained at a temperature and pressure at which the filter cake and the filtrate do not reach a state of being saturated to crystallize;
  • the filter cake passing through the pressure filtration zone is rotated into the next zone, the discharge zone, and the moisture content of the filter cake entering the blanking zone is controlled within 12%, and the filter cake is dropped into the dryer for drying;
  • FIG. 1 is a schematic illustration of the production process of one embodiment of a process for separating crude terephthalic acid (CTA) of the present invention.
  • An embodiment of a method for separating crude terephthalic acid (CTA) according to the present invention comprises a rotary pressure filter manufactured by BHS, which divides four functional zones, a hydraulic filtration zone, an acetic acid washing zone, and an air pressure. Filtration zone and blanking zone.
  • Rotary pressure filter for solid-liquid separation of acetic acid-containing mother liquor slurry containing crude terephthalic acid (CTA) crystals, while removing most of the ash impurities dissolved in acetic acid to increase the subsequent purification stage hydrogenation reaction The period of use of the catalyst.
  • the content of terephthalic acid in the slurry containing 111 of acetic acid containing crude terephthalic acid (CTA) crystal is about 32-36%, the temperature is 106 °C, and the concentration of main impurity ash (heavy metal and oxidation reaction by-product) 5 to 600 ppm, the acetic acid-containing slurry 111 is sent to the hydraulic filtration zone 11 of the filter 1 under pressure of about 2 to 4 kg/cm 2 (gauge pressure), and after filtering, it stays in the filter 11 to filter. A wet cake is produced in the tank, and the filtrate 112 is led to a filtrate collection system for recycling.
  • CTA crude terephthalic acid
  • the saturation pressure of the slurry 111 is 0 kg/cm 2 (gauge pressure)
  • the saturation temperature is 106 Torr
  • the pressure drop of the hydraulic filtration zone 11 is about 1 kg/cm 2 (gauge pressure)
  • the first filter cake and The pressure and temperature of the filtrate 112 entering the filtrate collection system after filtration are both greater than the saturation pressure of the slurry 111 by 0 kg/cni 2 (gauge pressure) and the saturation temperature of 106 ° C, thereby avoiding the occurrence of pressure drop during the filtration process. Crystallization on the filter cloth causes a problem of clogging of the filter cloth.
  • This hydraulic filtration zone 11 removes about 80% of the acetic acid mother liquor.
  • the filtered filter cake will be rotated into the next zone with the filter tank, that is, the acetic acid washing zone 12 is washed with pressurized acetic acid 121, and the washed washing liquid 122 is separately collected and treated, and the acetic acid pressure for washing is 2 - 3 .
  • Kg/cm 2 gauge pressure
  • the washed filter cake will rotate with the filter tank into the next zone, that is, the air pressure filtration zone 13.
  • the liquid in the filter cake is removed by extrusion filtration with a pressurized inert gas, and the inert gas containing the filtrate 132 It is taken out to the gas-liquid separator for the corresponding gas-liquid separation and recovery treatment.
  • the pressure of the inert gas 131 is about 2-3 kg/cm 2 (gauge pressure), the temperature is 100 ° C, and the pressure drop of filtration is about 1 kg/cm 2 (gauge pressure) in the gas pressure filtration zone 13
  • the pressure of the filter cake and the inert gas containing the filtrate 132 entering the gas-liquid separator is greater than the saturation pressure of the slurry 111 by 0 kg/cm 2 (gauge pressure), and also avoids clogging of the filter cloth due to crystallization. problem.
  • the gas pressure filtration zone 13 removes about 8% of the water, and after filtration, a filter cake having a moisture content of 12 wt% is obtained, and most of the impurity ash dissolved in the slurry 111 is removed.
  • the ash content can be controlled at 50-60 ppm.
  • the filter cake passing through the gas filtration zone 13 will be rotated with the filter tank into the next zone, the lowering zone 14, where the filter tank is reversely blown by the inert gas 141 to blank the filter cake.
  • the filter cloth is washed with acetic acid 142, and the washed acetic acid 144 can be used for recycling for other purposes.
  • the filter cake enters the feeding screw of the rotary steam dryer through the corresponding unloading channel, and after heating, removes the remaining acetic acid to obtain a crude phthalic acid product (CTA) having a lower ash content.
  • CTA crude phthalic acid product
  • Hydraulic zone feed pressure 2.0 ⁇ 4.0 kg/cm2 (gauge pressure) 2.0-3.0 kg cm2 (table
  • Acetic acid washing zone pressure 2.0 ⁇ 3.0 kg cm2 (gauge pressure)
  • Pressure zone feed pressure 2.0 ⁇ 3.0 kg/cm2 (gauge pressure)
  • the moisture content of the filter cake in the blanking area is 12% 12%
  • a method for separating crude terephthalic acid according to the present invention uses a rotary pressure filter, and the filtration of the filter always controls the temperature and pressure of the filter cloth not to be crystallized, thereby effectively preventing filtration during filtration. Crystallization on the cloth causes a problem of clogging of the product on the filter cloth.
  • the present invention is suitable for industrial use and has good industrial applicability.

Description

技术领域
本发明涉及一种从含醋酸母液浆料中回收粗对苯二甲酸的方法。 背景技术
传统的粗对苯二甲酸（简称为 CTA)制造过程中固液分离多采用离 心机或旋转真空过滤器， 即将第三结晶罐之 料泵入离心机， 借由离心 力分离浆液中所含粗对苯二甲酸及母液或预抽真空， 充分降压、 降温后 (温度为 90Ό，压力为 -0.5 kg/cm2 (表压））送至旋转真空过滤器之饲料罐, 再由泵送至旋转真空过滤器之底部料斗，通过溢流部分浆料的方式造成 晶体在醋酸溶剂中的悬浮，从而由转鼓内外之压差将晶体吸附在转鼓上， 达到过滤之目的 。
但由于旋转真空过滤器存在由于过滤时产生压降， 从而造成产品在 滤布上结晶堵塞的问题，碱洗之频率很高，不但造成产品及烧碱的浪费， 还影响生产的正常运行。此外， 当滤布破损须更换时， 需要花费较长时 间， 修护成本高且影响产量及产品品质。 发明内容
本发明的目的是提供一种分离粗对二苯二甲酸的方法， 特别是解决 在对苯二甲酸的过滤过程控制在滤布上不至于结晶，造成产品在滤布上 结晶堵塞的问题。 本发明一种用来分离粗对苯二甲酸 (CTA) 的方法， 采用旋转式压 力过滤器， 过滤器分成液压过滤、醋酸洗涤、气压过滤、 下料四个功能 区， 过滤器之过滤始终控制在滤布上不至于结晶的温度和压力； 形成含 湿率 12wt%以内的滤饼进行干燥处理； 产品中杂质灰份在 60ppm以内， 有效去处灰份，可以增加后续精制段氢化反应器之触媒使用周期
本发明的一种用来分离粗对苯二甲酸（CTA)的方法；更进一步为： 含粗对苯二甲酸晶体的含醋酸母液浆料送至旋转式压力过滤器之液 压过滤区中形成滤饼，其中液压过滤区滤布两侧的温度和压力维持在含 酸浆料和滤液均不达到呈过饱状态以至结晶析出的温度和压力；过滤形 成的滤饼旋转进入下一区即酸洗区， 由新鲜或回收的醋酸对滤饼进行洗 涤， 以洗去滤饼中的杂质，用来酸洗醋酸的温度不大于 95Ό, 流量为进 料浆料的 8-30%,；洗涤后的滤饼随后旋转进入气压过滤区由惰性气体迸 行挤压过滤，其中气压过滤区滤布两侧的温度和压力维持在滤饼和滤液 均不达到呈过饱状态以至结晶析出的温度和压力； 经过气压过滤区的滤 饼旋转进入下一区即下料区，进入下料区之滤饼含湿率控制在 12 ％以 内， 滤饼下料落入至干燥机进行干燥； 附图说明
图 1是本发明一种用来分离粗对苯二甲酸（CTA)的方法的一个实 施例的生产流程示意图。 具体实施方式 本发明一种用来分离粗对苯二甲酸（CTA) 的方法的一个实施例， 采用徳国 BHS公司生产的旋转式压力过滤机，划分四个功能区一液压过 滤区、 醋酸洗涤区、 气压过滤区和下料区。通过加大液压过滤区及气压 过滤区以增加过滤处理能力，并在下料区增设滤布清洗以延长过滤机进 料时间， 有效提高过滤机处理量。釆用旋转式压力过滤器来进行含粗对 苯二甲酸（CTA) 晶体的含醋酸母液浆料固液分离， 同时去除溶解在醋 酸中的大部份灰份杂质，以增加后续精制段氢化反应器触媒之使用周 期。
实施例 1
本实施例具体的生产流程， 请参见图 1。含粗对苯二甲酸（CTA)晶 体的含醋酸母液浆料 111 中对苯二甲酸含量约为 32— 36%左右， 温度 106°C，主要杂质灰份 (重金属及氧化反应副产物）的浓度为 500-600ppm， 该含醋酸浆料 111经加压在约 2— 4kg/cm2 (表压)的压力下送至过滤器 1 之液压过滤区 11中经过滤后停留在该过滤器 11滤槽中产生湿的滤饼， 滤液 112被引出到滤液收集系统， 做回收处理。 由于此浆料 111之饱和 压力为 0 kg/cm2 (表压)， 饱和温度为 106Ό, 此液压过滤区 11之压降约 为 1 kg/cm2 (表压)，因此第一滤饼及过滤后进入滤液收集系统的滤液 112 的压力及温度均大于所述浆料 111的饱和压力 0 kg/cni2(表压)及饱和温 度 106°C， 避免了在过滤过程中由于压降而产生在滤布上结晶致使滤布 堵塞的问题。 此液压过滤区 11可去除约 80%的醋酸母液。 过滤后的滤 饼会随滤槽旋转进入下一区即醋酸洗涤区 12用带压力之醋酸 121进行 洗涤,洗涤后的洗液 122被单独收集处理，用来洗涤之醋酸压力为 2 - 3 kg/cm2 (表压)，洗涤后的滤饼会随滤槽旋转进入下一区即气压过滤区 13 用带压力惰性气体 进行挤压过滤去除滤饼中的液体，含滤液的惰性 气体 132被引出到气液分离器， 做相应气液分离回收处理。此惰性气体 131之压力约为 2—3 kg/cm2 (表压)， 温度为 100° C, 而过滤之压降约 为 1 kg/cm2 (表压)， 在气压过滤区 13中的滤饼及进入气液分离器的含 滤液 132的惰性气体的压 1力大于所述漿料 111的饱和压力 0 kg/cm2 (表 压)， 同样达到了避免由于结晶而使滤布堵塞的问题。 此气压过滤区 13 可去除约 8%的水份， 过滤后得到含湿率在 12wt%以内之滤饼， 去除了 绝大部分溶解在浆料 111 中的杂质灰份。 灰份的含量可控制在 50-60ppm。 经过此气压过滤区 13的滤饼将随滤槽旋转进入下一区即下 料区 14， 在下料区 14由惰性气体 141反向喷吹滤槽使滤饼落料。 下料 区 14的滤饼落料后， 由醋酸 142对滤布进行清洗， 清洗后的醋酸 144 可用于回收用于其它用途。滤饼经对应下料槽道进入旋转式蒸汽干燥机 之进料螺旋器， 经加热后去除剩余醋酸， 得到灰份较低的粗对苯二甲酸 产品（CTA)。 实施例 2
序号 1 2 进料之饱和压力 0 kg/cm2(表压） 0 kg cm2(表压） 进料之饱和温度 106 ° C
进料之浓度 20〜30.1% 32〜40%
2.0〜4.0 kg cm2(表
液压区进料压力 2.0〜4.0 kg/cm2(表压） 压） 2.0—3.0 kg cm2(表
醋酸洗涤区压力 2.0〜3.0 kg cm2(表压） 压）
2.0〜3.0 kg/cm2(表
气压区进料压力 2.0〜3.0 kg/cm2(表压） 压）
进料中灰份浓度 500〜600ppm 500〜600ppm 下料区之滤饼中灰份浓
50〜60ppm 50~60ppm 度
下料区之滤饼中含湿率 12% 12%
工业实用性 本发明一种用来分离粗对苯二甲酸的方法采用旋转式压力过滤 器， 过滤器之过滤始终控制在滤布上不至于结晶的温度和压力， 有效的 防止过滤过程中在滤布上结晶、造成产品在滤布上结晶堵塞的问题。 本 发明适用于工业上使用， 具有良好的工业实用性。

Claims

权 利 要 求
1、 一种用来分离粗对苯二甲酸的方法， 采用旋转式压 力过滤器， 过滤器分成液压过滤、 醋酸洗涤、 气压过滤、 下 料四个功能区； 过滤器之过滤始终控制在滤布上不至于结晶 的温度和压力；形成含湿率 12wt%以内的滤饼进行干燥处理。
2、根据权利要求 1所述的一种用来分离粗对苯二甲酸的 方法； 其特征是： 含粗对苯二甲酸晶体的含醋酸母液浆料送 至旋转式压力过滤器之液压过滤区中形成滤饼， 其中液压过 滤区滤布两侧的温度和压力维持在含酸桨料和滤液均不达到 呈过饱状态以至结晶析出的温度和压力； 过滤形成的滤饼旋 转进入下一区即酸洗区， 由新鲜或回收的醋酸对滤饼进行洗 涤， 以洗去滤饼中的杂质； 洗涤后的滤饼随后旋转进入气压 过滤区由惰性气体进行挤压过滤， 其中气压过滤区滤布两侧 的温度和压力维持在滤饼和滤液均不达到呈过饱状态以至结 晶析出的温度和压力； 经过气压过滤区的滤饼旋转进入下一 区即下料区， 进入下料区之滤饼含湿率控制在 12wt%以内， 滤饼下料落入至干燥机进行干燥。
3、 根据权利要求 1或 2所述的一种用来分离粗对苯二甲 酸 （CTA ) 的方法， 其特征是： 所述的含醋酸母液浆料对苯 二甲酸晶体含量为 30-40 wt , 此浆料的饱和压力为 0-1 kg/cm2 (表压） ， 饱和温度在 105—126 ° C ； 该含醋酸母液浆 料经加压送入旋转式压力过滤器之液压过滤区， 经过滤后停 留在该过滤器滤槽中湿的滤饼及进入滤液收集系统的滤液的 压力及温度均不小于所述浆料的饱和压力及饱和温度； 经液 压过滤区收集在该滤槽中湿的滤饼随即旋转进入醋酸洗涤 区， 由带压力的新鲜或回收醋酸对滤饼进行洗涤， 以去处滤 饼中含有的杂质， 用来酸洗醋酸的温度不大于 95 °C， 流量为 进料浆料的 8-30%， 洗涤后的洗液单独收集处理； 随后滤饼旋 转进入下一区， 即气压过滤区， 在气压过滤区内使用带压力 惰性气体去除滤饼中的液体， 含滤液的惰性气体进入气液分 离器， 过滤后得到含湿率在 12wt%以内之滤饼， 在气压过滤 区中的滤饼及进入气液分离器含滤液的惰性气体的压力不小 于所述浆料的饱和压力； 经过气压过滤区的滤饼旋转进入下 料区， 在下料区使用惰性气体吹落或使用刮刀刮落滤饼， 使 滤饼经下料槽道落入干燥机之螺旋输送器。
4. 根据权利要求 1或 2所述的一种用来分离粗对苯二甲 酸 （CTA) 的方法， 其特征是： 所述的含醋酸母液浆料对苯 二甲酸晶体含量为 32-36 %，此浆料的饱和压力为 Q_ kg/cm2 (表 压） ， 饱和温度在 106 ° C； 旋转式压力过滤器之液压过滤区 中压力在 1— 4kg/cm2 (表压），此过滤区之压降为 1〜3 kg/cm2, 醋酸洗涤区中之压力在 1一 3 kg/cm2 (表压）， 此洗涤区之压降 为 1〜3 kg/cm2，气压过滤区惰性气体之压力为 1一 3kg/cm2 (表 压）而过滤之压降约为 1〜3 kg/cm2 (表压）。
PCT/CN2006/003045 2005-12-27 2006-11-13 Procede de separation de l'acide terephtalique brut WO2007073658A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CNB2005101046751A CN100522915C (zh) 2005-12-27 2005-12-27 一种用来分离粗对苯二甲酸(cta)的方法
CN200510104675.1 2005-12-27

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WO2007073658A1 true WO2007073658A1 (fr) 2007-07-05

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CN114057568A (zh) * 2020-07-29 2022-02-18 三达膜科技（厦门）有限公司 将精对苯二甲酸生产中主装置外排稀醋酸水回收的方法

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CN101624342B (zh) * 2009-08-13 2012-10-31 中国纺织工业设计院 精对苯二甲酸制备中cta分离过滤的方法及系统
CN104016847A (zh) * 2013-03-01 2014-09-03 中石化上海工程有限公司 从对苯二甲酸滤饼中脱除醋酸的方法
CN115445290A (zh) * 2022-09-13 2022-12-09 天华化工机械及自动化研究设计院有限公司 一种降低压力过滤机滤饼湿含量的方法

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* Cited by examiner, † Cited by third party
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WO2008071332A1 (de) * 2006-12-09 2008-06-19 Lurgi Gmbh Verfahren und anlage zur herstellung von roh-terephthalsäure
CN114057568A (zh) * 2020-07-29 2022-02-18 三达膜科技（厦门）有限公司 将精对苯二甲酸生产中主装置外排稀醋酸水回收的方法
CN114057568B (zh) * 2020-07-29 2024-04-19 三达膜科技（厦门）有限公司 将精对苯二甲酸生产中主装置外排稀醋酸水回收的方法

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