WO2021047266A1 - 一种提高反应结晶器内固含率的装置和方法 - Google Patents

一种提高反应结晶器内固含率的装置和方法 Download PDF

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WO2021047266A1
WO2021047266A1 PCT/CN2020/100523 CN2020100523W WO2021047266A1 WO 2021047266 A1 WO2021047266 A1 WO 2021047266A1 CN 2020100523 W CN2020100523 W CN 2020100523W WO 2021047266 A1 WO2021047266 A1 WO 2021047266A1
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liquid
pipe
crystallizer
clear liquid
supernatant
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PCT/CN2020/100523
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French (fr)
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朱全红
黄青山
肖航
杨超
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中国科学院青岛生物能源与过程研究所
中国科学院过程工程研究所
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Priority to US17/051,735 priority Critical patent/US11896946B2/en
Publication of WO2021047266A1 publication Critical patent/WO2021047266A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/06—Solidifying liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0063—Control or regulation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D2009/0086—Processes or apparatus therefor

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  • the invention relates to the field of reaction crystallizers, in particular to a technical scheme for increasing the solid content rate in the reaction crystallizer and regulating the crystal morphology and particle size distribution.
  • Increasing the solid content in the reaction crystallizer can not only increase the equipment volume utilization efficiency, but also effectively improve the crystal surface morphology, microstructure and particle size distribution.
  • the increase in solid content is usually achieved by increasing the concentration of the feed solution.
  • this method has the following shortcomings.
  • the concentration of the feed solution is limited by the solubility of the solute, on the other hand, it is restricted by the local supersaturation in the reaction crystallizer not being too high and cannot be increased indefinitely, which ultimately limits the reaction crystallizer.
  • the increase of the internal solid content will affect the morphology and size distribution of crystal particles.
  • the solid content rate in the reaction crystallizer can also be increased.
  • the invention patent with the authorized announcement number CN 100586550C proposes a liquid-solid continuous separation method and equipment for a slurry-bed reactor.
  • the raw materials and catalyst particles are contacted and reacted in the slurry-bed reactor, and the reacted suspension slurry is introduced
  • the separation unit including the inclined plate settler is quickly separated into the supernatant liquid and the concentrated slurry in the inclined plate settler.
  • the concentrated slurry returns to the reactor to continue to participate in the reaction, and the clear liquid flows upward along the gap between the plates to the upper part of the inclined plate settler discharge.
  • the invention can realize continuous separation and recycling of solid catalyst particles and liquid products.
  • this method has the disadvantages of high equipment investment, complicated operation, high operating cost, incomplete separation, and difficulty in achieving continuous operation.
  • the purpose of the present invention is to solve the above technical problems and provide a method for effectively increasing the solid content in the reaction crystallizer and regulating the crystal morphology and particle size distribution.
  • the method has the advantages of small equipment investment, low operating cost, safety and reliability, and easy realization of continuous operation and automatic control.
  • a device for increasing the solid content rate in the reaction crystallizer of the technical solution includes a discharge pipe, a clear liquid pipe, a gas collecting pipe and a clear liquid barrel; the crystallizer and the clear liquid barrel are mutually connected through the discharge pipe and the clear liquid pipe. Unicom, the liquid level remains flat.
  • an inverted cone-shaped enlarged section is arranged on the upper part of the discharge pipe to reduce the liquid velocity and improve the liquid-solid separation efficiency.
  • the cone angle of the inverted cone section needs to be greater than the accumulation angle of the crystal particles to prevent material clogging.
  • the air collecting pipe is provided with an exhaust pump.
  • a method for increasing the solid content in the reaction crystallizer Based on the above-mentioned device for increasing the solid content in the reaction crystallizer, the slurry in the crystallizer realizes liquid-solid separation through the sedimentation principle in the discharge pipe, and the solid particles fall into Crystallizer, and the clear liquid enters the clear liquid bucket through the clear liquid pipe and overflows and discharges; the gas collecting pipe collects the gas that enters the discharge pipe and the clear liquid pipe.
  • the liquid level in the gas collecting pipe needs to be always higher than the junction of the discharge pipe and the clear liquid pipe, so as to ensure that the crystallizer and the clear liquid barrel are always connected and the liquid level is flat.
  • the gas collecting pipe is provided with an exhaust pump to discharge the gas from time to time to ensure that the liquid level therein is always higher than the connection point of the discharge pipe and the clear liquid pipe.
  • the gas collecting pipe reduces the speed at which the liquid level drops by increasing the cross-sectional area, thereby eliminating the need for exhaust during the entire reaction process.
  • the beneficial effects of the present invention are: the discharge pipe, the gas collecting pipe and the clear liquid pipe are connected by a three-way connection, the solid-liquid mixture slowly rises in the discharge pipe, the solid particles return to the reaction crystallizer through sedimentation, and the clear liquid passes through the clear liquid pipe It can continuously flow out of the reaction crystallizer, thereby continuously increasing the solid content in the reaction crystallizer and improving the crystal morphology and particle size distribution.
  • the gas from the gas collecting pipe can be extracted manually or automatically to ensure that the liquid level in the gas collecting pipe is always higher than the junction of the discharge pipe and the clear liquid pipe, so as to ensure that the reaction crystallizer and the clear liquid barrel are always connected. Bits are flat. The device has vibrant design, simple structure, low cost and good continuity of operation.
  • Figure 1 is a schematic diagram of an automatic exhaust device.
  • Figure 2 is a schematic diagram of a device that does not require exhaust.
  • the lower end of the discharge pipe 2 is inserted below the liquid level in the reaction crystallizer 1, the upper end is connected with the upper end of the clear liquid pipe 3 and the lower end of the gas collecting pipe 5, and the lower end of the clear liquid pipe 3 is inserted below the liquid level of the clear liquid tank 4,
  • the upper part of the air pipe 5 is connected with an automatic liquid level control system 7, and the automatic liquid level control system 7 can send a control signal to control the start and stop or the speed of the exhaust pump 6.
  • the solid-liquid mixture in the reaction crystallizer 1 automatically enters the discharge pipe 2 and flows slowly upwards. Due to the low flow rate, the solid particles will gradually settle down and fall back to In the reaction crystallizer 1, the clear liquid continues to move upward, and then enters the clear liquid pipe 3 at the three-way position, and flows into the clear liquid bucket 4.
  • the solid particles in the reaction crystallizer 1 can be trapped in the reactor, but only the clear liquid is discharged, so that the solid content in the reaction crystallizer 1 gradually increases, so that the crystal morphology and particle size distribution are also Will change.
  • the clear liquid When the liquid level in the clear liquid bucket 4 reaches the overflow port, the clear liquid overflows and is discharged. After that, the liquid level in the clear liquid bucket 4 and the reaction crystallizer 1 will no longer change. However, the clear liquid will continuously flow out of the reaction crystallizer 1, and the solid particles will be trapped in the reaction crystallizer 1, causing the solid content in the reaction crystallizer 1 to continuously increase.
  • the gas entrained in the slurry in the reaction crystallizer 1 may enter the discharge pipe 2, gradually escape under negative pressure, and be enriched in the gas collecting pipe 5, causing the liquid level in the gas collecting pipe 5 to drop. After a period of time, This will cause the discharge pipe 2 and the clear liquid pipe 3 to no longer communicate with each other, the clear liquid in the reaction crystallizer 1 cannot be discharged continuously and slowly, and the liquid level will rise.
  • the liquid level automatic control system 7 is set here. When the liquid level automatic control system 7 detects that the liquid level in the gas collecting pipe 5 has dropped to the lower limit, it will automatically turn on the exhaust pump 6 so that the liquid level in the gas collecting pipe 5 rises.
  • the exhaust pump 6 When the liquid level automatic control system 7 detects that the liquid level in the exhaust pipe 5 slowly rises to the upper limit, the exhaust pump 6 will be automatically closed. When the liquid level in the exhaust pipe 5 reaches the lower limit again, the exhaust pump 6 is turned on again, and the cycle repeats. In this way, the liquid level in the exhaust pipe 5 can be made to fluctuate between the upper and lower limits, so that the reaction crystallizer 1 and the clear liquid barrel 4 are always connected, the liquid level is flat, and the clear liquid in the reaction crystallizer 1 can be Continuously discharged, and the solid particles will be trapped in the reaction crystallizer 1, so that the solid content in the reaction crystallizer 1 will increase with the extension of the feeding time, and the crystal morphology and particle size distribution will also occur improve.
  • the lower end of the discharge pipe 2 is inserted below the liquid level in the reaction crystallizer 1, the upper end is connected with the upper end of the clear liquid pipe 3 and the lower end of the gas collecting pipe 5, and the lower end of the clear liquid pipe 3 is inserted below the liquid level of the clear liquid tank 4,
  • the upper part of the air pipe 5 is provided with an enlarged section, and the upper part of the enlarged section is provided with a valve.
  • the solid-liquid slurry in the reaction crystallizer 1 will automatically enter the discharge pipe 2 and flow upward slowly. Due to the low flow rate, the solid particles will gradually settle down and become Falling back into the reaction crystallizer 1, while the clear liquid continues to move upwards, it enters the clear liquid pipe 3 at the three-way position, and flows into the clear liquid bucket 4.
  • the solid particles in the reaction crystallizer can be trapped in the reaction crystallizer 1, but only the clear liquid is discharged, so that the solid content in the reaction crystallizer 1 gradually increases, and the particle morphology and particle size distribution are also Will change.
  • the clear liquid When the liquid level in the clear liquid bucket 4 reaches the overflow port, the clear liquid overflows and is discharged. After that, the liquid level in the clear liquid bucket 4 and the reaction crystallizer 1 are maintained constant. However, the clear liquid will continuously flow out of the reaction crystallizer 1, and the solid particles will be trapped in the reaction crystallizer 1, causing the solid content in the reaction crystallizer 1 to continuously increase.
  • the gas entrained in the slurry in the reaction crystallizer 1 may enter the discharge pipe 2, gradually escape under the negative pressure condition, and be enriched in the gas collecting pipe 5, causing the liquid level in the gas collecting pipe 5 to drop.
  • the volume of the expanded section of the gas collecting pipe 5 should be set reasonably so that the liquid level in the gas collecting pipe 5 is always higher than the junction of the discharge pipe 2 and the clear liquid pipe 3 during the whole reaction process, and the reaction crystallizer 1 and the clear liquid Barrel 4 is always connected and the liquid level is flat.
  • the connection between the reaction crystallizer 1 and the clear liquid tank 4 can ensure the smooth discharge of the clear liquid in the reaction crystallizer 1.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Exhaust Gas After Treatment (AREA)

Abstract

本发明公开了一种提高反应结晶器内固含率的装置和方法，该装置包括出料管、清液管、清液桶和集气管，出料管的上端、清液管的上端及集气管的下端彼此连接，出料管的下端插入结晶器的液面以下，清液管的下端插入清液桶的液面以下，集气管收集进入出料管和清液管的气体，其中液位需高于出料管和清液管的连接处，确保结晶器和清液桶始终联通，液位持平，清液桶通过溢流维持液位恒定，进料时，结晶器内的液固混合物自动进入出料管，在其中向上缓慢流动，固体颗粒逐渐沉降并回落到结晶器内，而清液继续向上流动，进入清液管，流入清液桶，最终溢流排放。该方法具有投资小、操作简便的优点，可有效提高反应结晶器内的固含率并调控晶体形貌和粒度分布。

Description

一种提高反应结晶器内固含率的装置和方法 技术领域
本发明涉及反应结晶器领域，具体的说是一种提高反应结晶器内固含率、调控晶体形貌和粒度分布的技术方案。
背景技术
提高反应结晶器内的固含率不仅可以增大设备体积利用效率，还能够有效改善晶体的表面形貌、微观结构和粒度分布。
对于充分搅拌的反应结晶器，其中固含率的提高通常采用提高进料溶液浓度的方法来实现。然而，这种方法具有如下缺点，进料溶液的浓度一方面受到溶质溶解度的限制，另一方面受到反应结晶器内局部过饱和度不宜太高的限制，不能无限提高，最终限制了反应结晶器内固含率的提高，进而影响晶体颗粒形貌和粒度分布。
此外，将从反应结晶器中采出的浆料在外部进行固液分离后，再将固体颗粒返回反应结晶器也可以提高反应结晶器内的固含率。如授权公告号为CN 100586550C的发明专利提出了一种用于浆态床反应器的液固连续分离方法和设备，原料和催化剂颗粒在浆态床反应器中接触反应，反应后的悬浮浆液引入包括斜板沉降器的分离单元，在斜板沉降器中快速分离为上层清液和浓缩浆液，浓缩浆液返回反应器继续参与反应，清液沿板间的空隙向上流动至斜板沉降器的上部排出。该发明可实现固体催化剂颗粒和液体产品的连续分离和循环利用。然而，这种方法具有设备投资高、操作复杂、运行成本较高、分离不彻底及不易实现连续操作的缺点。
因此，目前为止仍没有较好的方法可以有效提高反应结晶器内的固含率。
发明内容
本发明的目的是为了解决上述技术难题，提供一种有效提高反应结晶器内固含率并调控晶体形貌和粒度分布的方法。该方法具有设备投资小、运行成本低、安全可靠及易实现连续操作和自动化控制的优点。
技术方案的一种提高反应结晶器内固含率的装置，包括出料管、清液管、集气管和清液桶；所述的结晶器和清液桶通过出料管和清液管彼此联 通，液位持平。
优选的，所述出料管上部设置倒锥形的膨大段，降低液速，提高液固分离效率，倒锥段的锥角需大于晶体颗粒的堆积角以防止积料堵塞。
优选的，所述集气管设置排气泵。
一种提高反应结晶器内固含率的方法，基于上述的提高反应结晶器内固含率的装置，结晶器内的浆料在出料管中通过沉降原理实现液固分离，固体颗粒回落入结晶器，而清液通过清液管进入清液桶并溢流排出；集气管收集进入出料管和清液管的气体。
优选的，所述集气管中的液位需要始终高于出料管和清液管的连接处，从而保证结晶器和清液桶始终联通，液位持平。
优选的，所述集气管设置排气泵不定时排出其中气体，确保其中液位始终高于出料管和清液管的连接处。
优选的，所述集气管通过增大横截面积降低其中液位下降的速度，从而使得整个反应过程中无需排气。
本发明的有益效果为：通过三通连接出料管、集气管和清液管，固液混合物在出料管中缓慢上升，固体颗粒通过沉降作用返回反应结晶器内，清液通过清液管可以持续不断地流出反应结晶器，从而不断提高反应结晶器内的固含率并改善晶体形貌和粒度分布。在应用过程中，可通过手动或自动控制抽取集气管的气体以确保集气管中液位始终高于出料管和清液管的衔接处，从而保证反应结晶器和清液桶始终相通，液位持平。该装置设计精妙，结构简单，成本低廉，操作连续性好。
附图说明
图1为自动排气的装置示意图。
图2为无需排气的装置示意图。
具体实施方式
实施方式1
下面结合附图1对本发明方法做进一步说明：
参见图1，出料管2下端插入反应结晶器1内液位之下，上端与清液管3上端和集气管5下端连接，清液管3下端插入清液桶4液面之下，集气管5上部与液位自动控制系统7相连，液位自动控制系统7可以发送控 制信号，控制排气泵6的启停或转速。
首先在清液桶4中加入一定清液，使得清液管3的下端位于液面之下。当反应结晶器1内的液位与清液桶4内的液位接近时，开启液位自动控制系统7，由于集气管5内的液位低于下限值，排气泵6自动开启，通过抽气方式向出料管2、清液管3和集气管5内充入液体，直至集气管5内的液位到达上限液位，排气泵6自动关闭。此时，反应结晶器1和清液桶4联通，根据连通器原理，两者液位持平。
之后，在原料溶液泵入反应结晶器1的过程中，反应结晶器1内的固液混合物自动进入出料管2，并缓慢向上流动，由于流速较低，固体颗粒会逐渐沉降下来并回落到反应结晶器1内，而清液继续向上运动，在三通位置转而进入清液管3，流入清液桶4。通过此方法，可以将反应结晶器1内的固体颗粒截留在反应器内，而只是将清液排出，从而使得反应结晶器1内的固含率逐渐增大，从而晶体形貌和粒度分布也会发生变化。
当清液桶4内的液位到达溢流口后，清液溢流排出，此后，清液桶4和反应结晶器1内的液位均不再变化。但是清液会源源不断地流出反应结晶器1，而固体颗粒会被截留在反应结晶器1内，使得反应结晶器1内的固含率不断增大。
反应结晶器1内浆料中夹带的气体可能会进入出料管2，在负压条件下逐渐逸出，并向集气管5富集，导致集气管5内液位下降，经过一段时间后，将会导致出料管2和清液管3不再彼此联通，反应结晶器1内的清液不能连续缓慢排出，液位将会上升。这里设置液位自动控制系统7，当液位自动控控制系统7检测到集气管5内的液位下降到下限值后，会自动开启排气泵6，使得集气管5内的液位上升，当液位自动控制系统7检测到排气管5内的液位缓慢上升到上限值时，会自动关闭排气泵6。等到排气管5内的液位再次到达下限值时，排气泵6再次开启，周而复始。通过这种方式，可以使得排气管5内的液位在上下限值之间波动，进而使得反应结晶器1和清液桶4始终联通，液位持平，反应结晶器1中的清液可以源源不断地排出，而固体颗粒会被截留在反应结晶器1内，从而使得反应结晶器1内的固含率随着进料时间的延长不断增大，其晶体形貌和粒度分布也会发生改善。
实施方式2
下面结合附图2对本发明方法做进一步说明：
参见图2，出料管2下端插入反应结晶器1内液位之下，上端与清液管3上端和集气管5下端连接，清液管3下端插入清液桶4液面之下，集气管5上部设置膨大段，膨大段上部设置阀门。
首先在清液桶4中加入一定清液，使得清液管3的下端位于液面之下。当反应结晶器1内的液位与清液桶4内的液位接近时，开启阀门6，通过抽气方式向出料管2、清液管3和集气管5内充入液体，直至集气管5膨大段内充满液体，关闭阀门6。此时，反应结晶器1和清液桶4联通，根据连通器原理，两者液位持平。
之后，在原料溶液泵入反应结晶器1的过程中，反应结晶器1内的固液浆料会自动进入出料管2，并缓慢向上流动，由于流速较低，固体颗粒会逐渐沉降下来并回落到反应结晶器1内，而清液继续向上运动，在三通位置转而进入清液管3，流入清液桶4。通过此方法，可以将反应结晶器内的固体颗粒截留在反应结晶器1内，而只是将清液排出，从而使得反应结晶器1内的固含率逐渐增大，颗粒形貌和粒度分布也会发生变化。
当清液桶4内的液位到达溢流口后，清液溢流排出，此后，清液桶4和反应结晶器1内的液位均维持恒定。但是清液会源源不断地流出反应结晶器1，而固体颗粒会被截留在反应结晶器1内，使得反应结晶器1内的固含率不断增大。
反应结晶器1内浆液中夹带的气体可能会进入出料管2，在负压条件下逐渐逸出，并向集气管5富集，导致集气管5内液位下降。此时，应该合理设置集气管5膨大段的体积，使得整个反应过程内集气管5中的液位始终高于出料管2和清液管3的衔接处，而反应结晶器1和清液桶4始终联通，液位持平。反应结晶器1和清液桶4的联通可以保证反应结晶器1内清液的顺利排出。
以上所述仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以所述权力要求的保护范围为准。

Claims (7)

  1. 一种提高反应结晶器内固含率的装置，其装置包括出料管、清液管、集气管和清液桶；所述的结晶器和清液桶通过出料管和清液管彼此联通，液位持平。
  2. 如权利要求1所述的一种提高反应结晶器内固含率的装置，其特征在于，所述出料管上部设置倒锥形的膨大段，降低液速，提高液固分离效率，倒锥段的锥角需大于晶体颗粒的堆积角以防止积料堵塞。
  3. 如权利要求1所述的一种提高反应结晶器内固含率的装置，其特征在于，所述集气管设置排气泵。
  4. 一种提高反应结晶器内固含率的方法，其特征在于，基于权利要求1-3中任意一项所述的提高反应结晶器内固含率的装置，结晶器内的浆料在出料管中通过沉降原理实现液固分离，固体颗粒回落入结晶器，而清液通过清液管进入清液桶并溢流排出；集气管收集进入出料管和清液管的气体。
  5. 如权利要求4所述的一种提高反应结晶器内固含率的方法，其特征在于，所述集气管中的液位需要始终高于出料管和清液管的连接处，从而保证结晶器和清液桶始终联通，液位持平。
  6. 如权利要求5所述的一种提高反应结晶器内固含率的方法，其特征在于，所述集气管设置排气泵不定时排出其中气体，确保其中液位始终高于出料管和清液管的连接处。
  7. 如权利要求5所述的一种提高反应结晶器内固含率的方法，其特征在于，所述集气管通过增大横截面积降低其中液位下降的速度，从而使得整个反应过程中无需排气。
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