WO2021073301A1 - Continuous washing process for polyphenylene sulfide slurry - Google Patents

Continuous washing process for polyphenylene sulfide slurry Download PDF

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WO2021073301A1
WO2021073301A1 PCT/CN2020/113369 CN2020113369W WO2021073301A1 WO 2021073301 A1 WO2021073301 A1 WO 2021073301A1 CN 2020113369 W CN2020113369 W CN 2020113369W WO 2021073301 A1 WO2021073301 A1 WO 2021073301A1
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polyphenylene sulfide
slurry
washing
tower
temperature
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PCT/CN2020/113369
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French (fr)
Chinese (zh)
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高碧波
魏光辉
张雄伟
王良初
周贵阳
覃广德
胡灯
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浙江新和成特种材料有限公司
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
    • C08G75/02—Polythioethers
    • C08G75/0204—Polyarylenethioethers
    • C08G75/0277—Post-polymerisation treatment
    • C08G75/0281—Recovery or purification
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
    • C08G75/02—Polythioethers
    • C08G75/0204—Polyarylenethioethers
    • C08G75/025—Preparatory processes
    • C08G75/0254—Preparatory processes using metal sulfides

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  • the invention belongs to the field of polymer materials, and relates to a continuous washing process of slurry, in particular to a continuous washing process of polyphenylene sulfide slurry.
  • Polyphenylene sulfide (PPS) resin is a new type of high-performance thermoplastic material. Because of its good high temperature resistance and chemical stability, it is widely used in flue gas dust removal, automobiles, electronics, electrical appliances and other fields.
  • the production of PPS resin usually adopts the method of solution polymerization.
  • the commonly used raw materials for industrial equipment are p-dichlorobenzene and sodium sulfide.
  • the by-product sodium chloride crystallizes out in the reaction solvent.
  • 1.2 tons of by-products per ton of PPS resin produced Sodium chloride, how to separate the PPS resin from the reaction solvent and sodium chloride is the key to organizing the production process and also determines the economics of the production process.
  • the patent CN 208121002 U discloses a device for removing salt in the synthesis of polyphenylene sulfide, that is, under a high temperature and high pressure reaction environment, PPS resin is dissolved in a solvent, and sodium chloride crystallizes out of the solvent. In the separation, the sodium chloride is separated first, and then the liquid part is reduced in temperature and pressure, so that the PPS resin crystallizes out, and the separation from the solvent is realized.
  • the method has a long process route, long salt washing time, high energy consumption, large waste water treatment capacity and unstable control of the salt content of the product (the salt content fluctuates between 0.2-1.0%).
  • the present invention provides a continuous washing process for polyphenylene sulfide slurry. Based on the PPS resin and sodium chloride solid-solid separation process, the process solves the problem of high consumption of pure water, high energy consumption, and low salt washing effect. Problems such as good, unstable control and so on.
  • a continuous washing process for polyphenylene sulfide slurry including:
  • the polyphenylene sulfide slurry is pressurized and heated, and then passed into the top of the scrubbing tower, while the high-temperature washing liquid is passed into the bottom of the scrubbing tower, where the high-temperature scrubbing liquid is used for the polyphenylene sulfide slurry Perform countercurrent washing to obtain washed polyphenylene sulfide resin at the bottom of the tower;
  • the polyphenylene sulfide slurry contains PPS resin, sodium chloride and water.
  • the polyphenylene sulfide slurry is obtained by sieving and separating the reaction product obtained by the polymerization reaction, and then adding water to beating the slurry, and the solid content of the slurry is 5%-45% (including PPS resin and salt).
  • the method of the present invention has a relatively good effect when used in a slurry with a salt content of 10-15% and a PPS content of 20-30%.
  • polyphenylene sulfide is formed into high-temperature and high-pressure slurry, and then it is in countercurrent contact with the high-temperature washing liquid.
  • the washing liquid can fully extract the inorganic salt in the system, and the washing efficiency is greatly improved.
  • the salt content can be reduced to less than 0.2%.
  • the process can be operated continuously. Compared with the intermittent washing process, it can save 60% of fixed asset investment and save water by more than 50%.
  • the high-temperature washing liquid in the countercurrent washing process enters from the bottom of the tower, and the slurry enters from the top of the tower main body.
  • the pressure and temperature during countercurrent washing will have a greater impact on the washing effect.
  • the boosting is performed by a slurry pump, and the pressure after boosting is 0.1-2.5 MPaG; more preferably 0.8-2.5 MPaG. 1.2MPaG.
  • the temperature increase is carried out in a two-stage heat exchange manner, the first-stage heat exchange makes the slurry outlet temperature 80-120°C, and the second-stage heat exchange makes the slurry outlet temperature 120-250°C, more preferably 160°C. ⁇ 180°C.
  • the primary heat exchange is the heat exchange and energy coupling between the slurry feed and the polyphenylene sulfide resin output at the bottom of the scrubber.
  • water vapor or heat transfer oil is used for heating during the secondary heat exchange.
  • the temperature of the slurry entering the scrubber is controlled by adjusting the flow of heating steam or heat transfer oil.
  • the temperature of the high-temperature washing liquid is 120 to 250°C, more preferably 160 to 180°C.
  • the volume ratio of the high-temperature washing liquid to the polyphenylene sulfide slurry is 1 to 4:1, more preferably 3 to 4:1.
  • the component of the high-temperature washing liquid is the condensed water of the pressurized steam, and the pressurized steam can be wholly or partly derived from the water vapor used in the secondary heat exchange, thereby realizing the reuse of resources.
  • the washed polyphenylene sulfide resin is discharged from the bottom of the washing tower, and the heat is recovered and then sent to the downstream processing system.
  • the salty wastewater after washing is obtained at the top of the tower, and the driving force provided by the liquid level and the pressure in the washing tower is transported to the downstream brine treatment system, and the difference between the brine flow rate and the washing liquid flow rate is controlled to be 0-0.1mL /min, a full lift safety valve is installed on the top of the tower.
  • the beneficial effects of the present invention are embodied in that the continuous washing process can greatly shorten the process route compared with the original intermittent washing process, save 60% of fixed asset investment, save 70% of installation space, and save more than 50% of water.
  • the time slurry treatment efficiency is greatly improved, and the salt content of the product is stabilized below 0.2%.
  • Fig. 1 is a schematic diagram of the continuous washing process of the present invention.
  • solid content or content involved are all mass percentages.
  • Alkali metal sulfides and dihalogenated aromatic compounds undergo high temperature and high pressure reaction in a polar organic solvent (N-methylpyrrolidone) to obtain polyphenylene sulfide particles (PPS), side reaction products sodium chloride and polar organic
  • the polymerization slurry of solvent (N-methylpyrrolidone) is sieved by a vibrating screen to obtain PPS particles containing part of sodium chloride and N-methylpyrrolidone slurry containing most of sodium chloride. Pure water is added to the sieved PPS particles to make a PPS slurry with a solid content of 5%-45% and main components of PPS resin, water, and sodium chloride.
  • FIG 1 is a schematic diagram of the washing device of the present invention. It can be seen from Figure 1 that the PPS slurry to be washed is first pressurized by the slurry pump 1, and then input into the primary heat exchanger 2 for the first heat exchange and heating (the heat source is washing The latter PPS slurry), and then input into the secondary heat exchanger 3 for the second heat exchange temperature increase (the heat source comes from the heated steam or heat-conducting oil), and then enter the top of the scrubber 4, flow from the top to the bottom; at the same time; The high-temperature washing liquid is input from the bottom of the side wall of the washing tower, and the high-temperature washing liquid flows from the bottom to the top.
  • the PPS slurry to be washed is first pressurized by the slurry pump 1, and then input into the primary heat exchanger 2 for the first heat exchange and heating (the heat source is washing The latter PPS slurry), and then input into the secondary heat exchanger 3 for the second heat exchange temperature increase (the heat source comes from the heated steam
  • the PPS slurry and the high-temperature washing liquid are in countercurrent contact in the tower. After the washing process is completed, the washed PPS slurry is from the bottom Output, heat exchange and cooling in the first-stage heat exchanger 2 to realize heat recovery and utilization.
  • the PPS resin forms a slurry after beating and washing.
  • the PPS resin content is 20% and the salt content is 10%.
  • the slurry is pressurized to 0.8MPaG by a transfer pump, and after passing through the primary heat exchanger and secondary heat exchanger, The temperature is raised to 160°C, and then it enters the top of the scrubber.
  • the secondary heater uses 1MPaG medium-pressure steam to heat, the medium-pressure steam condensate and 0.5MPaG low-pressure steam condensate are mixed and the temperature is 160°C, and the pump is used to transport to the lower end of the washing tower to perform countercurrent washing of the slurry.
  • the feed rate of PPS slurry is controlled to 35L/h, the feed rate of steam condensate at the bottom of the scrubber is 105L/h, and the volume ratio of scrubbing liquid to PPS slurry is maintained at 3:1.
  • the output volume of the PPS slurry after washing is 35L/h, the PPS resin content is maintained at 20%, and the output volume of waste brine is 105L/h.
  • the PPS resin After the PPS resin is beaten and washed, the PPS resin content is 30%, the salt content is 15%, and the slurry is increased to 1.2MPaG through the transfer pump. After passing through the primary heater and secondary heater, it is heated to 180°C, and then enters the scrubber tower. top.
  • the secondary heater is heated by 1.4MPaG medium pressure steam. After the medium pressure steam condensate and 0.8MPaG steam condensate are mixed, the temperature after mixing is 180°C, and the pump is transported to the lower end of the washing tower to perform countercurrent washing of the slurry.
  • the volume ratio with PPS slurry is 4:1.
  • the feed rate of PPS slurry is controlled to 35L/h, and the feed rate of steam condensate at the bottom of the scrubber is 140L/h.
  • the output volume of the washed PPS slurry is 40L/h, the PPS resin content is maintained at 26.26%, and the output volume of waste brine is 135L/h. Sampling and measuring the salt content of the waste water produced at the top of the scrubber was 3.86%, and the salt content of the slurry at the bottom was 0.1%.

Abstract

Disclosed is a continuous washing process for a polyphenylene sulfide (PPS) slurry, which mainly comprises the following steps: pressurizing and heating a PPS slurry, and then feeding same to the top of a washing tower, while feeding a high-temperature washing liquid to the bottom of the washing tower; using the high-temperature washing liquid in the tower to perform countercurrent washing on the PPS slurry to obtain a washed PPS resin at the bottom of the tower. The process significantly improves the washing efficiency, and the salt content of the product can be reduced to less than 0.2%.

Description

一种聚苯硫醚浆料连续洗涤工艺Continuous washing process of polyphenylene sulfide slurry 技术领域Technical field
本发明属于高分子材料领域，涉及一种浆料连续洗涤工艺，具体涉及一种聚苯硫醚浆料连续洗涤工艺。The invention belongs to the field of polymer materials, and relates to a continuous washing process of slurry, in particular to a continuous washing process of polyphenylene sulfide slurry.
背景技术Background technique
聚苯硫醚(PPS)树脂是一种新型高性能热塑性材料，因其具有良好的耐高温性能和化学稳定性，广泛应用于烟气除尘、汽车、电子、电器等领域。PPS树脂的生产通常采用溶液聚合的方法，产业化装置常用原料为对二氯苯和硫化钠，副产物氯化钠在反应溶剂中结晶析出，理论上每生产1吨PPS树脂会副产1.2吨氯化钠，如何实现PPS树脂与反应溶剂、氯化钠的分离，是组织生产流程的关键，也决定了生产工艺的经济性。Polyphenylene sulfide (PPS) resin is a new type of high-performance thermoplastic material. Because of its good high temperature resistance and chemical stability, it is widely used in flue gas dust removal, automobiles, electronics, electrical appliances and other fields. The production of PPS resin usually adopts the method of solution polymerization. The commonly used raw materials for industrial equipment are p-dichlorobenzene and sodium sulfide. The by-product sodium chloride crystallizes out in the reaction solvent. In theory, 1.2 tons of by-products per ton of PPS resin produced Sodium chloride, how to separate the PPS resin from the reaction solvent and sodium chloride is the key to organizing the production process and also determines the economics of the production process.
比如，专利CN 208121002 U公开了一种聚苯硫醚合成中除盐的装置，即在高温、高压的反应环境下，PPS树脂溶解于溶剂，氯化钠从溶剂中结晶析出，可通过固液分离，先将氯化钠分离出来，然后液体部分减温、减压，使PPS树脂结晶析出，实现与溶剂的分离。该方法工艺路线较长，盐洗涤时间长，能耗高，废水处理量大且产品盐含量控制不稳定(盐含量在0.2-1.0％之间波动)。For example, the patent CN 208121002 U discloses a device for removing salt in the synthesis of polyphenylene sulfide, that is, under a high temperature and high pressure reaction environment, PPS resin is dissolved in a solvent, and sodium chloride crystallizes out of the solvent. In the separation, the sodium chloride is separated first, and then the liquid part is reduced in temperature and pressure, so that the PPS resin crystallizes out, and the separation from the solvent is realized. The method has a long process route, long salt washing time, high energy consumption, large waste water treatment capacity and unstable control of the salt content of the product (the salt content fluctuates between 0.2-1.0%).
发明内容Summary of the invention
本发明提供了一种聚苯硫醚浆料连续洗涤工艺，该工艺在PPS树脂、氯化钠固-固分离工艺的基础上，解决了纯水消耗量大、能耗大、盐洗涤效果不佳、控制不稳定等问题。The present invention provides a continuous washing process for polyphenylene sulfide slurry. Based on the PPS resin and sodium chloride solid-solid separation process, the process solves the problem of high consumption of pure water, high energy consumption, and low salt washing effect. Problems such as good, unstable control and so on.
本发明通过以下技术方案实现的：The present invention is achieved through the following technical solutions:
一种聚苯硫醚浆料连续洗涤工艺，包括：A continuous washing process for polyphenylene sulfide slurry, including:
将聚苯硫醚浆料进行增压和升温，然后通入洗涤塔的塔顶，同时将高温洗涤液通入洗涤塔的塔底，在塔内所述高温洗涤液对聚苯硫醚浆料进行逆流洗涤，在塔底得到洗涤后的聚苯硫醚树脂；The polyphenylene sulfide slurry is pressurized and heated, and then passed into the top of the scrubbing tower, while the high-temperature washing liquid is passed into the bottom of the scrubbing tower, where the high-temperature scrubbing liquid is used for the polyphenylene sulfide slurry Perform countercurrent washing to obtain washed polyphenylene sulfide resin at the bottom of the tower;
所述的聚苯硫醚浆料包含PPS树脂、氯化钠和水。该聚苯硫醚浆料是将聚合反应得到的反应产物经过筛分分离，然后加水打浆后得到，其固含率为5％～45％(包括PPS树脂和盐)。作为优选，本发明的方法用于盐含量为10～15％，PPS含量为20～30％的浆料时，具有比较好的效果。The polyphenylene sulfide slurry contains PPS resin, sodium chloride and water. The polyphenylene sulfide slurry is obtained by sieving and separating the reaction product obtained by the polymerization reaction, and then adding water to beating the slurry, and the solid content of the slurry is 5%-45% (including PPS resin and salt). Preferably, the method of the present invention has a relatively good effect when used in a slurry with a salt content of 10-15% and a PPS content of 20-30%.
本发明将聚苯硫醚形成高温高压的浆料，然后与高温洗涤液进行逆流接触，在该逆流接触过程中，洗涤液能将体系中的无机盐充分提取出来，洗涤效率大幅度提升，产品含盐量可降低至0.2％以下。同时，该工艺可以连续操作，同间歇洗涤工艺相比，可节省固定资产投资60％，节水50％以上。In the present invention, polyphenylene sulfide is formed into high-temperature and high-pressure slurry, and then it is in countercurrent contact with the high-temperature washing liquid. In the countercurrent contact process, the washing liquid can fully extract the inorganic salt in the system, and the washing efficiency is greatly improved. The salt content can be reduced to less than 0.2%. At the same time, the process can be operated continuously. Compared with the intermittent washing process, it can save 60% of fixed asset investment and save water by more than 50%.
本发明中，在逆流洗涤过程中的高温洗涤液从塔底进，浆料从塔主体顶部进。In the present invention, the high-temperature washing liquid in the countercurrent washing process enters from the bottom of the tower, and the slurry enters from the top of the tower main body.
本发明中，逆流洗涤时压力和温度会对洗涤效果产生较大的影响，作为优选，所述的增压采用浆料泵进行，增压后的压力为0.1～2.5MPaG；进一步优选为0.8～1.2MPaG。In the present invention, the pressure and temperature during countercurrent washing will have a greater impact on the washing effect. Preferably, the boosting is performed by a slurry pump, and the pressure after boosting is 0.1-2.5 MPaG; more preferably 0.8-2.5 MPaG. 1.2MPaG.
作为优选，所述的升温采用两级换热的方式进行，一级换热使浆料出口温度为80～120℃，二级换热使浆料出口温度为120～250℃，进一步优选为160～180℃。Preferably, the temperature increase is carried out in a two-stage heat exchange manner, the first-stage heat exchange makes the slurry outlet temperature 80-120°C, and the second-stage heat exchange makes the slurry outlet temperature 120-250°C, more preferably 160°C. ～180℃.
作为进一步的优选，所述的一级换热为浆料进料与洗涤塔塔底聚苯硫醚树脂出料之间的换热、能量耦合。As a further preference, the primary heat exchange is the heat exchange and energy coupling between the slurry feed and the polyphenylene sulfide resin output at the bottom of the scrubber.
作为进一步的优选，二级换热时，采用水蒸气或者导热油进行加热。此时，通过调节加热蒸汽或导热油流量，控制进入洗涤塔的浆料温度。As a further preference, water vapor or heat transfer oil is used for heating during the secondary heat exchange. At this time, the temperature of the slurry entering the scrubber is controlled by adjusting the flow of heating steam or heat transfer oil.
作为优选，高温洗涤液的温度为120～250℃，进一步优选为160～180℃。Preferably, the temperature of the high-temperature washing liquid is 120 to 250°C, more preferably 160 to 180°C.
作为优选，所述的高温洗涤液与所述的聚苯硫醚浆料体积比为1～4：1，进一步优选为3～4：1。Preferably, the volume ratio of the high-temperature washing liquid to the polyphenylene sulfide slurry is 1 to 4:1, more preferably 3 to 4:1.
本发明中，高温洗涤液的成分为加压蒸气的冷凝水，该加压蒸气可全部或者部分地来自于二级换热时所用的水蒸气，从而实现资源的重复利用。In the present invention, the component of the high-temperature washing liquid is the condensed water of the pressurized steam, and the pressurized steam can be wholly or partly derived from the water vapor used in the secondary heat exchange, thereby realizing the reuse of resources.
作为优选，洗涤后的聚苯硫醚树脂从洗涤塔底部排出，回收热量后送下游处理系统。Preferably, the washed polyphenylene sulfide resin is discharged from the bottom of the washing tower, and the heat is recovered and then sent to the downstream processing system.
作为优选，在塔顶得到洗涤后的含盐废水，通过液位及洗涤塔内压力 提供的推动力，输送到下游的盐水处理系统，并控制盐水流量与洗涤液流量差值在0-0.1mL/min，塔顶安装全启式安全阀。Preferably, the salty wastewater after washing is obtained at the top of the tower, and the driving force provided by the liquid level and the pressure in the washing tower is transported to the downstream brine treatment system, and the difference between the brine flow rate and the washing liquid flow rate is controlled to be 0-0.1mL /min, a full lift safety valve is installed on the top of the tower.
同现有技术相比，本发明的有益效果体现在：该连续洗涤工艺较原间歇洗涤工艺可大大缩短工艺路线，节省固定资产投资60％，节省安装空间70％，节水50％以上，单位时间浆料处理效率大幅提升，且产品盐含量稳定在0.2％以下。Compared with the prior art, the beneficial effects of the present invention are embodied in that the continuous washing process can greatly shorten the process route compared with the original intermittent washing process, save 60% of fixed asset investment, save 70% of installation space, and save more than 50% of water. The time slurry treatment efficiency is greatly improved, and the salt content of the product is stabilized below 0.2%.
附图说明Description of the drawings
图1为本发明的连续洗涤工艺的装置示意图。Fig. 1 is a schematic diagram of the continuous washing process of the present invention.
具体实施方式Detailed ways
本发明中，如无特别说明，涉及到固含率或含量都为质量百分数。In the present invention, unless otherwise specified, the solid content or content involved are all mass percentages.
PPS浆料配置：PPS slurry configuration:
碱金属硫化物和二卤代芳香族化合物在极性有机溶剂(N-甲基吡咯烷酮)经过高温高压反应后得到含有聚苯硫醚颗粒(PPS)、副反应生成物氯化钠和极性有机溶剂(N-甲基吡咯烷酮)的聚合浆料，经过振动筛筛分后得到含有部分氯化钠的PPS颗粒和含有大部分氯化钠的N-甲基吡咯烷酮浆液。在筛分出的PPS颗粒中加入纯水打浆，配成固含率为5％-45％、主要成分为PPS树脂、水、氯化钠的PPS浆料。Alkali metal sulfides and dihalogenated aromatic compounds undergo high temperature and high pressure reaction in a polar organic solvent (N-methylpyrrolidone) to obtain polyphenylene sulfide particles (PPS), side reaction products sodium chloride and polar organic The polymerization slurry of solvent (N-methylpyrrolidone) is sieved by a vibrating screen to obtain PPS particles containing part of sodium chloride and N-methylpyrrolidone slurry containing most of sodium chloride. Pure water is added to the sieved PPS particles to make a PPS slurry with a solid content of 5%-45% and main components of PPS resin, water, and sodium chloride.
下面结合附图和具体实施例对本发明做进一步的描述。The present invention will be further described below in conjunction with the drawings and specific embodiments.
图1为本发明的洗涤装置示意图，由图1可知，待洗涤的PPS浆料首先通过浆料泵1进行加压，然后输入一级换热器2进行第一次换热升温(热源为洗涤后的PPS浆料)，再输入二级换热器3进行第二次换热升温(热源来自于加热的水蒸气或者导热油)，然后进入洗涤塔4的顶部，从顶部向底部流动；同时，高温洗涤液从洗涤塔的侧壁底部输入，高温洗涤液从底部向顶部流动，PPS浆料和高温洗涤液在塔内进行逆流接触，完成洗涤过程后，洗涤完成后的PPS浆料从底部输出，在一级换热器2中进行换热降温，实现热量的回收利用。Figure 1 is a schematic diagram of the washing device of the present invention. It can be seen from Figure 1 that the PPS slurry to be washed is first pressurized by the slurry pump 1, and then input into the primary heat exchanger 2 for the first heat exchange and heating (the heat source is washing The latter PPS slurry), and then input into the secondary heat exchanger 3 for the second heat exchange temperature increase (the heat source comes from the heated steam or heat-conducting oil), and then enter the top of the scrubber 4, flow from the top to the bottom; at the same time; The high-temperature washing liquid is input from the bottom of the side wall of the washing tower, and the high-temperature washing liquid flows from the bottom to the top. The PPS slurry and the high-temperature washing liquid are in countercurrent contact in the tower. After the washing process is completed, the washed PPS slurry is from the bottom Output, heat exchange and cooling in the first-stage heat exchanger 2 to realize heat recovery and utilization.
在洗涤塔的塔顶安装全启式安全阀5，图中6～10的标记都为阀门。Install a full-lift safety valve 5 on the top of the scrubbing tower. The marks from 6 to 10 in the figure are all valves.
实施例1Example 1
PPS树脂经过打浆洗涤之后形成浆料，其中，PPS树脂含量为20％，盐含量为10％，浆料通过输送泵增压到0.8MPaG，经过一级换热器、二级换热器后，升温到160℃，然后进入洗涤塔的塔顶。The PPS resin forms a slurry after beating and washing. The PPS resin content is 20% and the salt content is 10%. The slurry is pressurized to 0.8MPaG by a transfer pump, and after passing through the primary heat exchanger and secondary heat exchanger, The temperature is raised to 160°C, and then it enters the top of the scrubber.
二级加热器使用1MPaG中压蒸汽加热，中压蒸汽冷凝液和0.5MPaG低压蒸汽冷凝液混合后温度160℃，使用泵输送到洗涤塔下端，对浆料进行逆流洗涤。The secondary heater uses 1MPaG medium-pressure steam to heat, the medium-pressure steam condensate and 0.5MPaG low-pressure steam condensate are mixed and the temperature is 160°C, and the pump is used to transport to the lower end of the washing tower to perform countercurrent washing of the slurry.
控制PPS浆料进料量为35L/h，洗涤塔底部蒸汽冷凝液进料量为105L/h，保持洗涤液与PPS浆料体积比3:1。洗涤后的PPS浆料出料量为35L/h，保持PPS树脂含量为20％，废盐水的出料量为105L/h。取样测得洗涤塔顶部采出废水含盐量3.27％，底部浆料含盐量0.18％。The feed rate of PPS slurry is controlled to 35L/h, the feed rate of steam condensate at the bottom of the scrubber is 105L/h, and the volume ratio of scrubbing liquid to PPS slurry is maintained at 3:1. The output volume of the PPS slurry after washing is 35L/h, the PPS resin content is maintained at 20%, and the output volume of waste brine is 105L/h. Sampling measured the salt content of the waste water produced at the top of the scrubber tower was 3.27%, and the salt content of the slurry at the bottom was 0.18%.
实施例2Example 2
PPS树脂经过打浆洗涤之后，PPS树脂含量30％，盐含量15％浆料通过输送泵增加到1.2MPaG，经过一级加热器、二级加热器后，升温到180℃，然后进入洗涤塔的塔顶。After the PPS resin is beaten and washed, the PPS resin content is 30%, the salt content is 15%, and the slurry is increased to 1.2MPaG through the transfer pump. After passing through the primary heater and secondary heater, it is heated to 180°C, and then enters the scrubber tower. top.
二级加热器使用1.4MPaG中压蒸汽加热，中压蒸汽冷凝液和0.8MPaG蒸汽冷凝液混合后，混合后温度为180℃，使用泵输送到洗涤塔下端，对浆料进行逆流洗涤，洗涤液与PPS浆料体积比4:1。The secondary heater is heated by 1.4MPaG medium pressure steam. After the medium pressure steam condensate and 0.8MPaG steam condensate are mixed, the temperature after mixing is 180℃, and the pump is transported to the lower end of the washing tower to perform countercurrent washing of the slurry. The volume ratio with PPS slurry is 4:1.
控制PPS浆料进料量为35L/h，洗涤塔底部蒸汽冷凝液进料量为140L/h。洗涤后的PPS浆料出料量为40L/h，保持PPS树脂含量为26.26％，废盐水的出料量为135L/h。取样测得洗涤塔顶部采出废水含盐量3.86％，底部浆料含盐量0.1％。The feed rate of PPS slurry is controlled to 35L/h, and the feed rate of steam condensate at the bottom of the scrubber is 140L/h. The output volume of the washed PPS slurry is 40L/h, the PPS resin content is maintained at 26.26%, and the output volume of waste brine is 135L/h. Sampling and measuring the salt content of the waste water produced at the top of the scrubber was 3.86%, and the salt content of the slurry at the bottom was 0.1%.

Claims (9)

  1. 一种聚苯硫醚浆料连续洗涤工艺，其特征在于，包括：A continuous washing process for polyphenylene sulfide slurry, which is characterized in that it comprises:
    将聚苯硫醚浆料进行增压和升温，然后通入洗涤塔的塔顶，同时将高温洗涤液通入洗涤塔的塔底，在塔内所述高温洗涤液对聚苯硫醚浆料进行逆流洗涤，在塔底得到洗涤后的聚苯硫醚树脂；The polyphenylene sulfide slurry is pressurized and heated, and then passed into the top of the scrubbing tower, while the high-temperature washing liquid is passed into the bottom of the scrubbing tower, where the high-temperature scrubbing liquid is used for the polyphenylene sulfide slurry Perform countercurrent washing to obtain washed polyphenylene sulfide resin at the bottom of the tower;
    所述的聚苯硫醚浆料包含PPS树脂、氯化钠和水。The polyphenylene sulfide slurry contains PPS resin, sodium chloride and water.
  2. 根据权利要求1所述的聚苯硫醚浆料连续洗涤工艺，其特征在于，所述的增压采用浆料泵进行，增压后的压力为0.1～2.5MPaG。The continuous washing process of polyphenylene sulfide slurry according to claim 1, wherein the pressurization is performed by a slurry pump, and the pressure after pressurization is 0.1-2.5 MPaG.
  3. 根据权利要求1所述的聚苯硫醚浆料连续洗涤工艺，其特征在于，所述的升温采用两级换热的方式进行，一级换热使浆料出口温度为80～120℃，二级换热使浆料出口温度为120～250℃。The continuous washing process for polyphenylene sulfide slurry according to claim 1, wherein the temperature increase is carried out in a two-stage heat exchange manner, the first-stage heat exchange makes the slurry outlet temperature 80-120°C, and the second Stage heat exchange makes the slurry outlet temperature 120-250°C.
  4. 根据权利要求3所述的聚苯硫醚浆料连续洗涤工艺，其特征在于，所述的一级换热为所述聚苯硫醚浆料进料与洗涤塔塔底聚苯硫醚树脂出料之间的换热和能量耦合。The continuous washing process of polyphenylene sulfide slurry according to claim 3, characterized in that, the primary heat exchange is that the polyphenylene sulfide slurry feed and the polyphenylene sulfide resin output from the bottom of the washing tower Heat exchange and energy coupling between materials.
  5. 根据权利要求3所述的聚苯硫醚浆料连续洗涤工艺，其特征在于，二级换热时，采用水蒸气或者导热油进行加热。The continuous washing process of polyphenylene sulfide slurry according to claim 3, characterized in that, during the secondary heat exchange, water vapor or heat transfer oil is used for heating.
  6. 根据权利要求1或5所述的聚苯硫醚浆料连续洗涤工艺，其特征在于，所述的高温洗涤液为加压水蒸气的冷凝液，温度为120～250℃。The continuous washing process of polyphenylene sulfide slurry according to claim 1 or 5, wherein the high-temperature washing liquid is a condensate of pressurized water vapor, and the temperature is 120-250°C.
  7. 根据权利要求6所述的聚苯硫醚浆料连续洗涤工艺，其特征在于，二级换热时所用的水蒸气换热冷凝后，用作所述的高温洗涤液。The continuous washing process of polyphenylene sulfide slurry according to claim 6, wherein the water vapor used in the secondary heat exchange is used as the high-temperature washing liquid after heat exchange and condensation.
  8. 根据权利要求1所述的聚苯硫醚浆料连续洗涤工艺，其特征在于，洗涤后的聚苯硫醚树脂从洗涤塔底部排出，回收热量后送下游处理系统。The continuous washing process of polyphenylene sulfide slurry according to claim 1, wherein the washed polyphenylene sulfide resin is discharged from the bottom of the washing tower, and the heat is recovered and then sent to a downstream processing system.
  9. 根据权利要求1所述的聚苯硫醚浆料连续洗涤工艺，其特征在于，在塔顶得到洗涤后的含盐废水，通过液位及洗涤塔内压力提供的推动力，输送到下游的盐水处理系统，并控制盐水流量与洗涤液流量差值在0-0.1mL/min。The continuous washing process of polyphenylene sulfide slurry according to claim 1, wherein the salt-containing wastewater obtained after washing at the top of the tower is transported to the downstream brine through the driving force provided by the liquid level and the pressure in the washing tower Treat the system and control the difference between the flow rate of the brine and the flow rate of the washing liquid to be 0-0.1mL/min.
PCT/CN2020/113369 2019-10-15 2020-09-04 Continuous washing process for polyphenylene sulfide slurry WO2021073301A1 (en)

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