WO2011140855A1 - Procédé pour l'obtention directe de sulfate de sodium anhydre par évaporation éclair et cristallisation et appareil correspondant - Google Patents

Procédé pour l'obtention directe de sulfate de sodium anhydre par évaporation éclair et cristallisation et appareil correspondant Download PDF

Info

Publication number
WO2011140855A1
WO2011140855A1 PCT/CN2011/071592 CN2011071592W WO2011140855A1 WO 2011140855 A1 WO2011140855 A1 WO 2011140855A1 CN 2011071592 W CN2011071592 W CN 2011071592W WO 2011140855 A1 WO2011140855 A1 WO 2011140855A1
Authority
WO
WIPO (PCT)
Prior art keywords
flash
acid
stage
crystallizer
crystallization
Prior art date
Application number
PCT/CN2011/071592
Other languages
English (en)
Chinese (zh)
Inventor
许达人
Original Assignee
Xu Daren
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xu Daren filed Critical Xu Daren
Publication of WO2011140855A1 publication Critical patent/WO2011140855A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/16—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/18—Dehydration

Definitions

  • the invention relates to the field of viscose fiber processing and equipment thereof, in particular to a concentrated and crystalline flashing process and device for directly crystallizing anhydrous sodium sulfate (also known as yuan Ming powder) in an acid bath in a chemical fiber plant acid station .
  • anhydrous sodium sulfate also known as yuan Ming powder
  • the acid bath of the chemical fiber plant is used for the coagulation of the viscose.
  • the acid bath is diluted and the composition of sodium sulfate is increased.
  • the waste acid bath should be recycled for recycling.
  • the water added by the acid bath during the coagulation process must be separated from the sodium sulfate.
  • the current technology uses a flashing device to concentrate the acid bath, separates the water, and then cools the concentrated acid bath to crystallize the manganese nitrate, and further melts and crystallizes the mirabilite to obtain the Yuanming powder.
  • the current acid bath flashing devices at home and abroad are all evaporation devices that can only be concentrated and cannot be crystallized. Summary of the invention
  • the present invention aims to change the existing only concentration-concentrated flash concentration process and apparatus to directly crystallize anhydrous sodium sulfate (ie, element Continuous flash crystallization process and apparatus for bright powder).
  • a process for directly obtaining Yuanming powder based on flash crystallization comprising the following steps:
  • Controlling the specific gravity of the acid The specific gravity of the acid bath of the sodium sulfate to be treated is controlled between 1.4 and 1.44;
  • the discharged Yuanming powder slurry is further separated, sprayed or neutralized and dried to directly obtain the finished product of Yuanming powder. Further, the process further includes the following steps:
  • step (3) The crystallization mother liquid produced in the thickening process is mixed with the acid bath of the newly added sodium sulfate to be treated and the specific gravity of the mixed acid bath is controlled to be 1.4 to 1. 44.
  • the flash crystallization is cyclically heated under the action of a circulation pump.
  • the process of directly obtaining the Yuanming powder based on flash crystallization, according to the flashing temperature in the region of 110-5 CTC, is exactly the phase precipitated by anhydrous sodium sulfate (ie, Yuan Ming powder)
  • the theoretical basis of the district the key to its discovery is:
  • the specific gravity is 1.45 (in the case of specific production conditions is not exactly the same);
  • the current flash concentration the specific gravity of the acid bath is about 1. 3;
  • the specific gravity of the acid bath of the flashing apparatus is 1.40 ⁇ 1.
  • the specific gravity is less than 1.40, no crystallization occurs during the flashing process; the specific gravity exceeds 1.44, anhydrous sodium sulfate will precipitate in advance, and the crystal will wear out.
  • Graphite tube for the heater Within the above range, the specific gravity of the acid is low, and the output of Yuanming powder is low; the specific gravity is high, and the output of Yuanming powder is high. Therefore, the specific gravity of the acid should be determined by the required output of the Yuanming powder. When the output is required to be high, the specific gravity control should be increased, so that there is no crystal flow and precipitation in the heat exchanger (including the preheater and the heater); When the output is required to be low, the specific gravity control should be lowered.
  • the method of increasing the acid bath concentration is to reduce the amount of new acid entering and increase the reflux of concentrated acid.
  • the structure of the device in which the flash crystallization directly obtains the Yuanming powder must be capable of evaporating water, continuously crystallization, separating mist, and the like.
  • the present invention further discloses a device for directly obtaining Yuanming powder based on flash crystallization:
  • a device for directly obtaining Yuanming powder based on flash crystallization comprising a preheater, a heater, a final stage flash chamber, a condenser and a circulation pump, characterized in that:
  • the continuous flash crystallization apparatus comprises at least two flash crystallizers connected in series through a pipeline, the flash crystallizer being a vertical, cone-bottom structure; wherein the acid in the first stage of the flash crystallizer The acid discharge port of the mouth and the heater is connected through a pipeline, and the acid discharge port of each stage of the flash crystallizer is respectively connected to the acid inlet port of the flash crystallizer at the lower stage thereof through the pipeline, and the last stage is flash crystallization.
  • the acid discharge port of the device is connected to the central feed pipe of the thickener through a pipeline;
  • the secondary steam outlet of each stage of the flash crystallizer is connected to the inlet of the corresponding preheater through the pipeline, at the end
  • the secondary steam outlet of the two-stage flash crystallizer is connected to the inlet of the condenser through a pipeline;
  • the slurry discharge port of the thickener is connected to the slurry pump, and the thickener is further provided with an acid discharge overflow port.
  • the thickener is further provided with a clear acid port of the crystallization mother liquid, the upper acid port of the crystallization mother liquid is connected to the acid inlet of the final flash chamber, mixed with the new acid and controlling the mixed acid
  • the bath has a specific gravity of 1. 4 ⁇ 1. 44, and continues to participate in the flash crystallization cycle by the circulation pump.
  • the apparatus further includes at least one stage of a flash chamber, wherein the flash chamber is an upper evaporative concentration device located in the first stage flash crystallizer, and the acid inlet of the first stage flash chamber.
  • the acid discharge port of the heater is connected through a pipeline, and the acid discharge port of each stage of the flash chamber is respectively connected to the acid inlet port of the flash crystallizer or the flash chamber at the next stage, and the flash chamber of each stage is connected.
  • the secondary steam outlets are respectively connected to the inlet ports of the corresponding preheaters through the pipelines.
  • FIG. 1 is a schematic view of a current flashing process and apparatus
  • Embodiment 1 of the present invention is a process flow and a device diagram of Embodiment 1 of the present invention.
  • Fig. 3 is a view showing the process flow and apparatus of the embodiment 2 of the present invention. In the picture,
  • thickener 100, 104, 108, 112, 116, secondary steam outlet of flash crystallizer V5J ⁇ V9J; 101, 105, 109, 113, preheater A5 ⁇ A8 inlet port; 102, 106, 110, 114, 118, 122 flash crystallizer V5J ⁇ V10J acid outlet; 103, 107, 111, 115, 119 flash crystallizer V6J ⁇ V9J acid inlet 117, 127, inlet ports of condensers MK2 and MK1; 123, center feeder pipe connection of thickener; 124, acid port on clarified mother liquor of thickener; 125. crystallization mother liquor of final stage flash chamber VI I Import; 126.
  • the current flashing process includes preheater A8-A1, heater H, flash chamber V1-V11, condensers MK1 and MK2, circulation pump XP, and its flash chamber is horizontal.
  • the acid bath is concentrated by a flashing device to separate the water, and then the concentrated acid bath is cooled at a low temperature to crystallize the mirabilite, and then the Glauber's salt is further melted and evaporated to obtain the Yuanming powder.
  • it is absolutely necessary to prevent crystallization from occurring; because, if crystallization occurs, the equipment is quickly blocked by crystals; therefore, during the entire flashing process, it can only be concentrated and cannot be crystallized.
  • the device in order to adapt to flash crystallization, uses a vertical flash crystallizer to completely or partially replace the horizontal flash chamber, so that the crystals are suspended in the crystallizer, the particles grow, and are discharged through the bottom of the cone.
  • a flash crystallizer in order to adapt to flash crystallization, uses a vertical flash crystallizer to completely or partially replace the horizontal flash chamber, so that the crystals are suspended in the crystallizer, the particles grow, and are discharged through the bottom of the cone.
  • a process and apparatus for crystallizing element powder based on an acid bath flashing process as shown in Fig. 2; the device adopts 11-stage flashing, which differs from the current device in that it changes part of the horizontal flashing chamber to
  • the flash crystallizer is equipped with a thickener ZC and a slurry pump JP.
  • V5J ⁇ V9J is a vertical and cone-shaped flash crystallizer that replaces the original horizontal flash chamber. The crystals are pressed into the next stage crystallizer through the bottom of the cone without depositing in the crystallizer.
  • the sodium sulphate bath passes through the preheater and the heater, and enters the multi-stage flashing chamber V1 ⁇ V4, the flash crystallizer V5J ⁇ V10J and the final stage flash chamber VI I, and the water is continuously evaporated and concentrated, crystallizing.
  • the material is suspended in a flash crystallizer, the particles are grown, and continuously discharged from the upper flash crystallizer to the next stage flash crystallizer for continuous crystallization; the acid bath is concentrated in the flash chamber V1 ⁇ V4 to reach sulfuric acid Sodium is saturated and crystallizes from V5J.
  • the equipment of V5J ⁇ V10J is characterized by vertical cone bottom, which can circulate and crystallize without blocking. It can separate secondary steaming. Steam.
  • the pipe connection feature is: the secondary steam outlet 100 of the flash crystallizer V5J is connected to the inlet 101 of the preheater A5, and the acid discharge port 102 is connected to the acid inlet 103 of the crystallizer V6J; the crystallizer V6J
  • the secondary steam outlet 104 is connected to the inlet port 105 of the preheater A6, and the acid discharge port 106 is connected to the acid inlet port 107 of the crystallizer V7J, and the secondary steam outlet 108 of the crystallizer V7J is connected to the preheater.
  • the inlet port 109 of A7 is connected, the acid discharge port 110 is connected to the acid inlet port 111 of the crystallizer V8J, and the secondary steam outlet 112 of the crystallizer V8J is connected to the inlet port 113 of the preheater A8.
  • the acid port 114 is connected to the acid inlet port 115 of the crystallizer V9J, and the secondary steam outlet 116 of the crystallizer V9J is connected to the inlet port 117 of the condenser MK2, and the acid discharge port 118 and the acid inlet port 119 of the crystallizer V10J are connected.
  • the secondary steam outlet 120 of the crystallizer V10J is connected to the inlet port 121 of the condenser MK2, and the acid discharge port 122 is connected to the central feed pipe port 123 of the thickener, and contains a suspension of the crystal powder of the Yuanming powder.
  • the acid discharge port 122 Flowing out of the acid discharge port 122, entering the thickener ZC through the thickener center feed pipe port 123, thickening After the sodium sulfate slurry is thickened ZC from acting in JP thickener slurry pumps slurry discharge port 131 is discharged further isolation, and or spray dried directly to obtain the finished product sodium sulphate.
  • the thickener ZC is further provided with an acid discharge overflow port 130 and a clear crystal mother liquor upper acid port 124, wherein the clear crystal mother liquor upper acid port 124 communicates with the acid inlet port 125 of the final stage flash chamber VI I;
  • the crystallization cycle is carried out by a circulating pump under the action of a circulating pump.
  • the specific acid is mixed with the new acid inlet 128 of the final acid flashing chamber VI I and controlled to have a specific gravity of 1. 4 ⁇ 1.
  • the circulating acid concentration entering the preheater A8 should meet the process requirements.
  • the specific gravity control can adjust the amount of new acid into the clarified mother liquor through the thickener.
  • the proportion of clarified mother liquor from the upper acid port 124 is reached.
  • a process and apparatus for crystallizing powder based on an acid bath flashing process differs from Example 1 in that it is a 14-stage flash, except for the final stage flash chamber V14.
  • the vertical and cone-shaped flash crystallizers V1J ⁇ V13J are used for flashing and flash crystallization, and the thickener ZC does not have the upper acid port of the clarified mother liquor, that is, the concentrated acid produced during the flash crystallization process. , does not directly recycle back to the evaporation crystallization equipment, the amount and specific gravity of the circulating acid bath will be achieved by directly controlling the amount of new acid added and the concentration of new acid.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention porte sur un procédé pour l'obtention directe de sulfate de sodium anhydre par évaporation éclair et cristallisation et sur un appareil correspondant. Le procédé comprend les étapes suivantes : (1) le réglage de la densité du bain acide dans la plage de 1,4-1,44, (2) l'évaporation éclair et la cristallisation en continu dans un dispositif d'évaporation éclair/cristallisation en continu, (3) l'épaississement pour obtenir une suspension épaisse de sulfate de sodium anhydre, (4) la séparation de la suspension épaisse de sulfate de sodium anhydre, le rinçage par pulvérisation ou la neutralisation et le séchage pour obtenir directement le produit fini constitué de sulfate de sodium anhydre. L'appareil comprend un réchauffeur (A1-A8), un dispositif de chauffage (H), une chambre d'évaporation éclair finale (V11), un condenseur (MK1, MK2) et une pompe de circulation (XP) et il comprend en outre un dispositif d'évaporation éclair/cristallisation en continu, un épaississeur (ZC) et une pompe à suspension épaisse (JP). Le dispositif d'évaporation éclair/cristallisation en continu comprend au moins deux cristalliseurs par évaporation éclair (V5J-V10J) en série, qui sont raccordés par une canalisation l'un après l'autre. Les cristalliseurs par évaporation éclair ont une structure verticale et à fond conique. Dans le procédé, les opérations de cristallisation, de séparation, de chauffage et de fusion et d'évaporation de mirabilite sont omises et l'investissement à la construction et le coût sont réduits.
PCT/CN2011/071592 2010-05-10 2011-03-07 Procédé pour l'obtention directe de sulfate de sodium anhydre par évaporation éclair et cristallisation et appareil correspondant WO2011140855A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2010201879244U CN201770493U (zh) 2010-05-10 2010-05-10 基于酸浴闪蒸流程的结晶元明粉装置
CN201020187924.4 2010-05-10

Publications (1)

Publication Number Publication Date
WO2011140855A1 true WO2011140855A1 (fr) 2011-11-17

Family

ID=43750331

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2011/071592 WO2011140855A1 (fr) 2010-05-10 2011-03-07 Procédé pour l'obtention directe de sulfate de sodium anhydre par évaporation éclair et cristallisation et appareil correspondant

Country Status (2)

Country Link
CN (1) CN201770493U (fr)
WO (1) WO2011140855A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102168326B (zh) * 2011-03-24 2012-08-22 南通三圣石墨设备科技股份有限公司 粘胶纤维酸浴系统高效节能闪蒸方法及专用装置
CN103510166B (zh) * 2012-06-20 2016-01-20 杭州奥通科技有限公司 高湿模量粘胶纤维凝固浴处理流水线
CN103241748B (zh) * 2013-04-27 2014-10-08 许达人 一种基于酸浴闪蒸结晶制取元明粉的工艺方法
CN104628016B (zh) * 2015-01-29 2016-08-17 中盐金坛盐化有限责任公司 一种高硝母液硝盐联产设备及工艺
CN104925834A (zh) * 2015-06-03 2015-09-23 郸城县凯杰科技有限公司 一种芒硝水生产元明粉的加工工艺
CN110330039B (zh) * 2019-07-16 2021-05-07 南通三圣石墨设备科技股份有限公司 一种酸浴连续制取元明粉的生产系统及生产工艺

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1111598A (zh) * 1994-08-11 1995-11-15 许达人 酸浴一步法蒸浓提硝新工艺
CN2227513Y (zh) * 1995-05-09 1996-05-22 许达人 石墨块孔式强制循环酸浴蒸发器
US6162408A (en) * 1996-10-31 2000-12-19 Kvaerner Pulping Ab Process for purifying ash which principally consists of sodium sulphate from a recovery boiler
CN101306260A (zh) * 2007-07-12 2008-11-19 项公浩 多功能多效自动连续蒸发结晶工艺及结晶设备
CN201195059Y (zh) * 2008-04-08 2009-02-18 任红兵 真空闪蒸结晶器
CN101372344A (zh) * 2008-04-10 2009-02-25 湖南新澧化工有限公司 一种高纯度大颗粒工业无水硫酸钠的生产方法
CN101391155A (zh) * 2008-10-22 2009-03-25 大连理工大学 一种高效结晶装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1111598A (zh) * 1994-08-11 1995-11-15 许达人 酸浴一步法蒸浓提硝新工艺
CN2227513Y (zh) * 1995-05-09 1996-05-22 许达人 石墨块孔式强制循环酸浴蒸发器
US6162408A (en) * 1996-10-31 2000-12-19 Kvaerner Pulping Ab Process for purifying ash which principally consists of sodium sulphate from a recovery boiler
CN101306260A (zh) * 2007-07-12 2008-11-19 项公浩 多功能多效自动连续蒸发结晶工艺及结晶设备
CN201195059Y (zh) * 2008-04-08 2009-02-18 任红兵 真空闪蒸结晶器
CN101372344A (zh) * 2008-04-10 2009-02-25 湖南新澧化工有限公司 一种高纯度大颗粒工业无水硫酸钠的生产方法
CN101391155A (zh) * 2008-10-22 2009-03-25 大连理工大学 一种高效结晶装置

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
LIU XIAOHONG ET AL.: "A Study Of Direct Preparation of Anhydrous Sodium Sulfate By Recovering Acid Bath", GUANGXI CHEMICAL FIBER NEWSLETTER, no. 1-2, 1998, pages 8 - 11 *
LIU XIAOHONG ET AL.: "A Study Of Technology In Recovering Sodium Sulfate By One Step Crystallization", GUANGDONG CHEMICAL FIBER, no. 3, September 1998 (1998-09-01), pages 13 - 15, 18 *
LU FANGYI ET AL.: "Direct Preparation Of Anhydrous Sodium Sulfate From Waste Liquid Containing Sodium Sulfate", ENVIRONMENTAL PROTECTION OF CHEMICAL INDUSTRY, vol. 17, no. 2, 1997, pages 105 - 108 *

Also Published As

Publication number Publication date
CN201770493U (zh) 2011-03-23

Similar Documents

Publication Publication Date Title
CN106007133B (zh) 一种脱硫废水浓缩蒸发、结晶、盐分离工艺
WO2011140855A1 (fr) Procédé pour l'obtention directe de sulfate de sodium anhydre par évaporation éclair et cristallisation et appareil correspondant
CN103588225B (zh) 多级闪蒸降温连续结晶生产食品级氯化钾的方法
CN201770492U (zh) 酸浴蒸发器体外结晶元明粉装置
CN108439434B (zh) 一种生产小苏打的方法和装置
CN104692415B (zh) 一种生产硝酸钾时对氯化铵的蒸发结晶方法
CN104445306B (zh) 制造硫酸镁的装置与方法
CN103510166B (zh) 高湿模量粘胶纤维凝固浴处理流水线
CN106422399A (zh) 一种盐溶液节能蒸发浓缩结晶系统及其控制方法
CN106310704A (zh) 连续单效真空蒸发结晶系统、应用及工艺
CN106115740B (zh) 一种制盐方法和制盐系统
CN109289233A (zh) 用于蒸发结晶的装置、甲硫氨酸的结晶方法
CN103241748B (zh) 一种基于酸浴闪蒸结晶制取元明粉的工艺方法
CN107758698B (zh) 一种芒硝脱水制元明粉工艺及设备
CN113929148B (zh) 一种铼粉还原用的超细高纯铼酸铵的制备方法
CN104030261B (zh) 一种高纯度电子级磷酸的生产方法
CN108557894A (zh) 一种硫酸锰溶液结晶装置和方法
CN113666393A (zh) 一种氯化钾精制工艺及生产系统
CN103588223B (zh) 多级闪蒸降温连续结晶生产高纯度氯化铵的方法
CN106629938A (zh) 高浓度含盐废水四效真空节能蒸发结晶处理系统
CN105480990B (zh) 一种制备无水硫酸钠的设备和方法
CN104261437A (zh) 一种与液体硝酸铵生产相结合的连续式硝酸钾生产系统
CN214218200U (zh) 粘胶纤维酸浴一体化生产元明粉的系统
CN112811441B (zh) 一种利用制盐废液生产精制盐的工艺及系统
CN206167974U (zh) 连续单效真空蒸发结晶系统

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 11780077

Country of ref document: EP

Kind code of ref document: A1

WWE Wipo information: entry into national phase

Ref document number: 2118/MUMNP/2012

Country of ref document: IN

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 11780077

Country of ref document: EP

Kind code of ref document: A1