[go: up one dir, main page]

CN220485340U - High purity phosphorus pentasulfide preparation system - Google Patents

High purity phosphorus pentasulfide preparation system Download PDF

Info

Publication number
CN220485340U
CN220485340U CN202320107952.8U CN202320107952U CN220485340U CN 220485340 U CN220485340 U CN 220485340U CN 202320107952 U CN202320107952 U CN 202320107952U CN 220485340 U CN220485340 U CN 220485340U
Authority
CN
China
Prior art keywords
distillation tower
crude
residual liquid
phosphorus pentasulfide
liquid
Prior art date
Legal status (The legal status 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 status listed.)
Active
Application number
CN202320107952.8U
Other languages
Chinese (zh)
Inventor
刘周恩
华超
陆平
路明清
屈云
王东
苗刚
郑雄飞
路明彪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hubei Jixing Chemical Industry Group Corp ltd
Institute of Process Engineering of CAS
Original Assignee
Hubei Jixing Chemical Industry Group Corp ltd
Institute of Process Engineering of CAS
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 Hubei Jixing Chemical Industry Group Corp ltd, Institute of Process Engineering of CAS filed Critical Hubei Jixing Chemical Industry Group Corp ltd
Application granted granted Critical
Publication of CN220485340U publication Critical patent/CN220485340U/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Landscapes

  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The high-purity phosphorus pentasulfide preparation system comprises a synthesis reaction device, a crude product rectifying tower and a residual liquid rectifying tower, wherein a crude product port at the top of the synthesis reaction device is connected with a crude product inlet of a crude product rectifying tower body at the lower part of the crude product rectifying tower; the bottom of the crude product rectifying tower is connected with a liquid inlet in the middle of the residual liquid rectifying tower through a residual liquid discharge port of the crude product rectifying tower body; the sulfur-phosphorus material lateral line air outlet of the residual liquid rectifying tower body at the upper part of the residual liquid rectifying tower is connected with the sulfur-phosphorus material air inlet of the crude product rectifying tower body of the crude product rectifying tower; the bottom of the residual liquid rectifying tower is connected with a liquid outlet of a condenser of the residual liquid rectifying tower body through a kettle liquid outlet. The device can greatly improve the purity of the phosphorus pentasulfide product, particularly can greatly reduce the content of organic impurities in the phosphorus pentasulfide product, and can produce the high-purity phosphorus pentasulfide of lubricating oil which can meet the lubricating oil industry, and the quality of the phosphorus pentasulfide product is better than that of the phosphorus pentasulfide product produced by adopting a traditional distillation device or rare earth.

Description

高纯五硫化二磷制备系统High purity phosphorus pentasulfide preparation system

技术领域Technical field

本实用新型提供本技术属于五硫化二磷生产技术领域,尤其涉及到一种高纯五硫化二磷制备系统。The technology provided by the utility model belongs to the technical field of phosphorus pentasulfide production, and particularly relates to a high-purity phosphorus pentasulfide preparation system.

背景技术Background technique

五硫化二磷[P2S5,又称为四硫化十磷(P4S10)]是一种使用广泛的非常重要的化学品,主要用于有机磷农药(乐果、辛硫磷、乙基1605 等)、润滑油添加剂(起抗氧化、耐磨擦、防腐蚀等作用)、有色金属选矿浮选剂及医药等行业。但是,随着对有机磷农药残留毒性的认识,有机磷农药因其固有的特性,其用量正在受到限制,增长乏力。但与之相反,随着汽车、石油、润滑油和医药等行业的发展,对高质量五硫化二磷需求量迅速增加,并对产品质量提出更高的要求,高纯五硫化二磷产品市场前景非常良好。Phosphorus pentasulfide [P 2 S 5 , also known as decaphosphorus tetrasulfide (P 4 S 10 )] is a widely used and very important chemical, mainly used in organophosphorus pesticides (dimethoate, phoxim, ethyl 1605 etc.), lubricating oil additives (functioning as antioxidant, friction-resistant, anti-corrosion, etc.), non-ferrous metal mineral processing flotation agents and pharmaceutical industries. However, with the recognition of the toxicity of organophosphorus pesticide residues, the use of organophosphorus pesticides is being limited due to their inherent characteristics, and growth is sluggish. But on the contrary, with the development of automobile, petroleum, lubricants and pharmaceutical industries, the demand for high-quality phosphorus pentasulfide has increased rapidly, and higher requirements have been put forward for product quality. The market prospects for high-purity phosphorus pentasulfide products are very good.

高纯五硫化二磷产品品质不但与其中五硫化二磷含量纯度、硫和磷元素含量(即其中多硫化磷P4Sx含量,x=2,3,5,6,7,9)有关[见国标GB/T 13258-2016(《工业五硫化二磷》)],而且还受其中有机杂质的影响。尤其是有机杂质,对五硫化二磷的性质有很大的影响,有机杂质含量越高,五硫化二磷品质越差,当有机杂质含量超过0.3 %时,五硫化二磷的色泽、物性等会发生严重的变化,品质严重变差,尤其对于像润滑油等行业,对五硫化二磷中有机杂质特别敏感,要求有机杂质一般不超过0.1%。The quality of high-purity phosphorus pentasulfide products is not only related to the purity of phosphorus pentasulfide content, but also the content of sulfur and phosphorus elements (i.e., the content of phosphorus pentasulfide P 4 S x , x=2,3,5,6,7,9) [see national standard GB/T 13258-2016 ("Industrial Phosphorus Pentasulfide")], and is also affected by organic impurities. Especially organic impurities have a great impact on the properties of phosphorus pentasulfide. The higher the content of organic impurities, the worse the quality of phosphorus pentasulfide. When the organic impurity content exceeds 0.3%, the color, physical properties, etc. of phosphorus pentasulfide will undergo serious changes, and the quality will seriously deteriorate. Poor, especially for industries such as lubricants, which are particularly sensitive to organic impurities in phosphorus pentasulfide, requiring organic impurities to generally not exceed 0.1%.

因此,高纯五硫化二磷的不仅与合成过程有关,而且还与五硫化二磷纯化过程有关。其中,目前五硫化二磷粗品的纯化主要采用蒸馏纯化装置系统,根据蒸馏压力的不同,又可分为简单蒸馏系统和减压蒸馏系统,比如专利200610019731.6采用简单蒸馏系统在常压下和515 ℃条件下对合成出的五硫化二磷产品进行分离提纯,该系统比较简单,且为常压操作(微正压),操作较为简便,设备气密性要求较低。但蒸馏分离提纯效果较差,所产五硫化二磷产品中硫磷化合物纯度较低,多硫磷化物含量较高,尤其是有机杂质无法彻底脱除,这严重地降低了五硫化二磷品质。专利CN101712464A、200810233489.1、CN101844755A和CN101402450B均采用减压蒸馏系统,在负压和380 ℃左右对合成出的五硫化二磷粗品进行纯化,与常压蒸馏系统相比,减压蒸馏的操作温度较低,能耗较低,五硫化二磷纯度较高,但有机杂质也无法彻底脱除,这严重影响了五硫化二磷产品的纯度和品质。Therefore, the high purity of phosphorus pentasulfide is not only related to the synthesis process, but also to the purification process of phosphorus pentasulfide. Among them, the current purification of crude phosphorus pentasulfide mainly uses a distillation purification device system. According to the difference in distillation pressure, it can be divided into a simple distillation system and a vacuum distillation system. For example, patent 200610019731.6 uses a simple distillation system to purify phosphorus pentasulfide under normal pressure and 515 ℃. The synthesized phosphorus pentasulfide product is separated and purified. The system is relatively simple and operates at normal pressure (slightly positive pressure). The operation is relatively simple and the air tightness requirements of the equipment are low. However, the effect of distillation, separation and purification is poor. The purity of sulfur and phosphorus compounds in the phosphorus pentasulfide products produced is low, and the content of polysulfide phosphide is high. In particular, organic impurities cannot be completely removed, which seriously reduces the quality of phosphorus pentasulfide. Patents CN101712464A, 200810233489.1, CN101844755A and CN101402450B all use a vacuum distillation system to purify the synthesized crude phosphorus pentasulfide at negative pressure and around 380°C. Compared with the normal pressure distillation system, the operating temperature of vacuum distillation is lower and the energy consumption is lower. The purity of phosphorus pentasulfide is relatively high, but organic impurities cannot be completely removed, which seriously affects the purity and quality of phosphorus pentasulfide products.

因此,开发能脱除有机杂质的五硫化二磷纯化系统具有重要的意义。Therefore, it is of great significance to develop a phosphorus pentasulfide purification system that can remove organic impurities.

发明内容Contents of the invention

针对现有五硫化二磷纯化系统存在的不足,本实用新型的目的在于提供一种高纯五硫化二磷制备系统,本实用新型采用常压精馏的装置或减压精馏的装置对合成的五硫化二磷粗品进行纯化,既提高产品中五硫化二磷含量,降低多硫磷化物含量,又将其中有机杂质脱除,提高了五硫化二磷产品品质,可生产出低有机杂质的高纯五硫化二磷产品。In view of the shortcomings of the existing phosphorus pentasulfide purification system, the purpose of this utility model is to provide a high-purity phosphorus pentasulfide preparation system. This utility model uses a normal pressure distillation device or a vacuum distillation device to purify the synthesized crude phosphorus pentasulfide. It not only increases the content of phosphorus pentasulfide in the product, reduces the content of polysulfide phosphide, but also removes organic impurities, improves the quality of phosphorus pentasulfide products, and can produce high-purity phosphorus pentasulfide products with low organic impurities.

一种高纯五硫化二磷制备系统,所述的系统主要包括:所述的系统要包括合成反应装置、粗品精馏塔、残液精馏塔。A high-purity phosphorus pentasulfide preparation system, the system mainly includes: the system includes a synthesis reaction device, a crude product distillation tower, and a residual liquid distillation tower.

其中,合成反应装置可为气相反应装置,也可为液相反应装置,优选为液相反应装置;既可为连续式反应装置,也可为间歇式反应装置,优选为间歇式反应装置。Wherein, the synthesis reaction device can be a gas phase reaction device or a liquid phase reaction device, preferably a liquid phase reaction device; it can be a continuous reaction device or a batch reaction device, preferably a batch reaction device.

合成反应装置顶部的粗品口与粗品精馏塔下部的粗品精馏塔体进粗品口相连;The crude product inlet at the top of the synthesis reaction device is connected to the crude product inlet of the crude product rectification tower at the bottom of the crude product rectification tower;

粗品精馏塔底部经粗品精馏塔体排残液口与残液精馏塔中部的进液口相连;The bottom of the crude distillation tower is connected to the liquid inlet in the middle of the crude distillation tower body through the residual liquid discharge port;

残液精馏塔上部的残液精馏塔体硫磷物料侧线出气口与粗品精馏塔的粗品精馏塔体进硫磷物料气口相连;The sulfur and phosphorus material side outlet of the residual liquid distillation tower in the upper part of the residual liquid distillation tower is connected to the sulfur and phosphorus material inlet of the crude distillation tower;

残液精馏塔底部经出釜液口与残液精馏塔体冷凝器排液口相连。The bottom of the residual liquid distillation tower is connected to the liquid outlet of the condenser of the residual liquid distillation tower through the liquid outlet of the kettle.

粗品精馏塔中部经粗品精馏塔体五硫化二磷侧线出气口与粗品精馏塔体五硫化二磷侧线上冷凝器连接后一路经粗品精馏塔体五硫化二磷侧线回流口回流连接至粗品精馏塔,一路经粗品精馏塔体五硫化二磷侧线出液口连接至高纯五硫化二磷储罐。The middle part of the crude distillation tower is connected to the condenser on the side line of phosphorus pentasulfide of the crude distillation tower body through the phosphorus pentasulfide side line outlet of the crude distillation tower body, and then is refluxed to the crude product distillation tower through the reflux port of the phosphorus pentasulfide side line of the crude distillation tower body. The phosphorus pentasulfide side line outlet of the distillation tower is connected to the high-purity phosphorus pentasulfide storage tank.

粗品精馏塔上部经粗品精馏塔体硫磷轻组分侧线出气口与粗品精馏塔体硫磷轻组分侧线上冷凝器连接后一路经粗品精馏塔体硫磷轻组分侧线回流口回流连接至粗品精馏塔,一路经粗品精馏塔体硫磷轻组分侧线出液口连接至硫磷轻组分储罐。The upper part of the crude distillation tower is connected to the condenser on the side line of the sulfur and phosphorus light components in the crude distillation tower body through the side outlet of the sulfur and phosphorus light components in the crude distillation tower body, and then flows back through the side line of the sulfur and phosphorus light components in the crude product rectification tower body. The outlet reflux is connected to the crude distillation tower, and all the way is connected to the sulfur and phosphorus light component storage tank through the sulfur and phosphorus light component side liquid outlet of the crude distillation tower body.

粗品精馏塔顶部经粗品精馏塔体有机杂质侧线出气口与粗品精馏塔体有机杂质侧线上冷凝器连接后一路经粗品精馏塔体有机杂质侧线回流口回流连接至粗品精馏塔,一路经粗品精馏塔体有机杂质侧线出液口连接至有机杂质储罐。The top of the crude distillation tower is connected to the condenser on the organic impurity side line of the crude distillation tower through the organic impurity side outlet of the crude distillation tower, and then is refluxed to the crude distillation tower through the organic impurity side reflux port of the crude distillation tower. One line is connected to the organic impurity storage tank through the organic impurity side outlet of the crude distillation tower.

粗品精馏塔底部经粗品精馏塔体出釜液口与粗品精馏塔体再沸器连接,粗品精馏塔体再沸器经粗品精馏塔体进釜液蒸汽口与粗品精馏塔下部连接,形成循环回路;The bottom of the crude distillation tower is connected to the reboiler of the crude distillation tower through the still liquid outlet of the crude distillation tower. The reboiler of the crude distillation tower is connected to the crude distillation tower through the liquid inlet vapor port of the crude distillation tower. The lower part is connected to form a circulation loop;

残液精馏塔顶部经残液精馏塔体有机杂质气侧线出气口与残液精馏塔体有机杂质侧线冷凝器连接后一路经残液精馏塔体有机杂质侧线回流口与残液精馏塔上部连接,一路经残液精馏塔有机杂质侧线排液口连接至有机杂质储罐。The top of the residual liquid distillation tower is connected to the organic impurity side line condenser of the residual liquid distillation tower body through the organic impurity gas side outlet of the residual liquid distillation tower body, and then passes through the organic impurity side line reflux port of the residual liquid distillation tower body and the residual liquid essence. The upper part of the distillation tower is connected, and all the way is connected to the organic impurity storage tank through the organic impurity side drain port of the residual liquid distillation tower.

残液精馏塔底部经残液精馏塔体出釜液口与残液精馏塔体再沸器连接,残液精馏塔体再沸器经残液精馏塔体进釜液汽口与残液精馏塔下部连接。The bottom of the residual liquid distillation tower is connected to the reboiler of the residual liquid distillation tower through the still liquid outlet of the residual liquid distillation tower, and the reboiler of the residual liquid distillation tower enters the still liquid vapor port through the residual liquid distillation tower. Connected to the lower part of the residual liquid distillation tower.

所述的粗品精馏塔和残液精馏塔是常压精馏装置,或是减压精馏装置;是连续式反应装置,或是间歇式反应装置。The crude product distillation tower and residual liquid distillation tower are normal pressure distillation devices or vacuum distillation devices; they are continuous reaction devices or batch reaction devices.

与现有技术相比,采用本实用新型的装置可较大幅度的提高五硫化二磷产品纯度,尤其是可大幅降低五硫化二磷产品中有机杂质的含量,生产出能满足润滑油行业的润滑油级高纯五硫化二磷,比采用传统的蒸馏技术生产的五硫化二磷产品的品质要好。Compared with the existing technology, the device of the present invention can greatly improve the purity of phosphorus pentasulfide products, especially the content of organic impurities in phosphorus pentasulfide products, and produce high-purity phosphorus pentasulfide that can meet the needs of the lubricating oil industry. , which is of better quality than phosphorus pentasulfide products produced using traditional distillation technology.

附图说明Description of the drawings

图1为高纯五硫化二磷制备系统。1: 合成反应装置,1-1: 合成反应装置进磷口,1-2: 合成反应装置进硫口,1-3: 合成反应装置出粗品口,2: 粗品精馏塔,2A: 粗品精馏塔体,2A-1: 粗品精馏塔体进粗品口,2A-2: 粗品精馏塔体出釜液口,2A-3: 粗品精馏塔体进釜液蒸汽口,2A-4: 粗品精馏塔体进硫磷物料气口,2A-5: 粗品精馏塔体五硫化二磷侧线出气口,2A-6: 粗品精馏塔体五硫化二磷侧线回流口,2A-7: 粗品精馏塔体硫磷轻组分侧线出气口,2A-8: 粗品精馏塔体硫磷轻组分侧线回流口,2A-9: 粗品精馏塔体有机杂质侧线出气口,2A-10: 粗品精馏塔体有机杂质侧线回流口,2B: 粗品精馏塔体再沸器,2B-1:粗品精馏塔体排残液口,2C: 粗品精馏塔体五硫化二磷侧线上冷凝器,2C-1: 粗品精馏塔体五硫化二磷侧线出液口,2D: 粗品精馏塔体硫磷轻组分侧线上冷凝器,2D-1: 粗品精馏塔体硫磷轻组分侧线出液口,2E: 粗品精馏塔体有机杂质侧线上冷凝器,2E-1: 粗品精馏塔体有机杂质侧线出液口,3: 残液精馏装置,3A: 残液精馏塔体,3A-1: 残液精馏塔体进液口,3A-2: 残液精馏塔体出釜液口,3A-3: 残液精馏塔体进釜液汽口,3A-4: 残液精馏塔体硫磷物料侧线出气口,3A-5: 残液精馏塔体有机杂质气侧线出气口,3A-6: 残液精馏塔体有机杂质侧线回流口,3B: 残液精馏塔体再沸器,3B-1: 残液精馏塔体再沸器排液口,3C: 残液精馏塔体有机杂质侧线冷凝器,Figure 1 shows the high-purity phosphorus pentasulfide preparation system. 1: synthesis reaction device, 1-1: phosphorus inlet of the synthesis reaction device, 1-2: sulfur inlet of the synthesis reaction device, 1-3: crude product outlet of the synthesis reaction device, 2: crude product distillation tower, 2A: crude product concentrate Distillation tower body, 2A-1: crude product inlet port, 2A-2: crude product rectification tower body outlet for still liquid, 2A-3: crude product rectification tower body into still liquid steam port, 2A-4: Crude distillation tower body sulfur and phosphorus material gas inlet, 2A-5: crude distillation tower body phosphorus pentasulfide side outlet, 2A-6: crude distillation tower body phosphorus pentasulfide side line reflux port, 2A-7: crude distillation tower body sulfur and phosphorus Light component side outlet, 2A-8: Side line reflux port of sulfur and phosphorus light components in the crude distillation tower, 2A-9: Side outlet for organic impurities in the crude distillation tower, 2A-10: Organic impurities in the crude distillation tower Impurity side line reflux port, 2B: crude distillation tower reboiler, 2B-1: crude distillation tower residual liquid discharge port, 2C: crude distillation tower phosphorus pentasulfide side line condenser, 2C-1: crude distillation Side line liquid outlet of phosphorus pentasulfide in the tower body, 2D: Condenser on the side line of the sulfur and phosphorus light component in the crude distillation tower body, 2D-1: Side line liquid outlet of the sulfur and phosphorus light component in the crude distillation tower body, 2E: Crude distillation tower Side line condenser for organic impurities, 2E-1: Side line outlet for organic impurities in crude distillation tower, 3: Residual liquid distillation device, 3A: Residual liquid distillation tower, 3A-1: Residual liquid distillation tower Body liquid inlet, 3A-2: raffinate distillation tower body kettle liquid outlet, 3A-3: raffinate rectification tower body kettle liquid inlet vapor port, 3A-4: raffinate distillation tower body sulfur and phosphorus material side line Gas outlet, 3A-5: Side outlet of organic impurity gas in raffinate distillation tower, 3A-6: Side reflux port of organic impurities in raffinate distillation tower, 3B: Reboiler of raffinate distillation tower, 3B- 1: Drain port of the reboiler in the raffinate distillation tower, 3C: Side line condenser of organic impurities in the raffinate distillation tower,

3C-1: 残液精馏塔有机杂质侧线排液口。3C-1: Side drain port for organic impurities in the residual liquid distillation tower.

a: 液态黄磷,b: 液态硫磺,c: 五硫化二磷粗品,d: 粗品精馏塔釜液,e: 进再沸器2B的釜液,f: 粗品精馏塔釜液蒸汽,g: 粗品精馏塔残液,h: 粗品精馏塔五硫化二磷蒸汽,i: 粗品精馏塔五硫化二磷液体,j: 粗品精馏塔五硫化二磷回流液,k: 粗品精馏塔五硫化二磷产品,l: 粗品精馏塔硫磷轻组分蒸汽,m: 粗品精馏塔硫磷轻组分液体,n: 粗品精馏塔硫磷轻组分回流液,o: 粗品精馏塔硫磷轻组分产物,p: 粗品精馏塔有机杂质蒸汽,q: 粗品精馏塔有机杂质液体,r: 粗品精馏塔有机杂质回流液,s: 粗品精馏塔有机杂质产物,t: 残液精馏塔釜液,u: 进再沸器3B的釜液,v: 残液精馏塔釜液蒸汽,w: 残液精馏塔残液,x: 残液精馏塔硫磷物料蒸汽,y: 残液精馏塔有机杂质蒸汽,z: 残液精馏塔有机杂质液,α: 残液精馏塔有机杂质回流液,β: 残液精馏塔有机杂质产物,γ: 有机杂质。a: Liquid yellow phosphorus, b: Liquid sulfur, c: Crude phosphorus pentasulfide, d: Crude distillation tower still liquid, e: Still liquid entering reboiler 2B, f: Crude distillation tower still liquid steam, g: Crude essence Distillation tower residue, h: phosphorus pentasulfide vapor in crude distillation tower, i: phosphorus pentasulfide liquid in crude distillation tower, j: phosphorus pentasulfide reflux liquid in crude distillation tower, k: phosphorus pentasulfide product in crude distillation tower, l: phosphorus pentasulfide in crude distillation tower Light component steam, m: sulfur and phosphorus light component liquid in crude distillation tower, n: sulfur and phosphorus light component reflux liquid in crude distillation tower, o: sulfur and phosphorus light component product in crude distillation tower, p: crude distillation Tower organic impurity vapor, q: crude distillation tower organic impurity liquid, r: crude distillation tower organic impurity reflux liquid, s: crude distillation tower organic impurity product, t: residual liquid distillation tower still liquid, u: feed Still liquid of boiler 3B, v: raffinate distillation tower still liquid vapor, w: raffinate distillation tower raffinate, x: raffinate distillation tower sulfur and phosphorus material vapor, y: raffinate distillation tower organic impurity vapor , z: organic impurity liquid in the raffinate distillation tower, α: organic impurity reflux liquid in the raffinate distillation tower, β: organic impurity product in the raffinate distillation tower, γ: organic impurity.

具体实施方式Detailed ways

实施例1Example 1

高纯五硫化二磷制备系统,包括合成反应装置1、粗品精馏塔2、残液精馏塔3,合成反应装置1顶部的粗品口1-3与粗品精馏塔2下部的粗品精馏塔体进粗品口2A-1相连;The high-purity phosphorus pentasulfide preparation system includes a synthesis reaction device 1, a crude product distillation tower 2, and a residual liquid distillation tower 3. The crude product ports 1-3 at the top of the synthesis reaction device 1 are connected to the crude product distillation tower body at the bottom of the crude product distillation tower 2. The coarse product port is connected to 2A-1;

粗品精馏塔2底部经粗品精馏塔体排残液口2B-1与残液精馏塔3中部的进液口3A-1相连;The bottom of the crude product distillation tower 2 is connected to the liquid inlet 3A-1 in the middle of the crude product distillation tower 3 through the residual liquid discharge port 2B-1 of the crude product distillation tower body;

残液精馏塔3上部的残液精馏塔体硫磷物料侧线出气口3A-4与粗品精馏塔2的粗品精馏塔体进硫磷物料气口2A-4相连;The sulfur and phosphorus material side outlet 3A-4 in the upper part of the residual liquid distillation tower 3 is connected to the sulfur and phosphorus material inlet port 2A-4 in the crude distillation tower 2;

残液精馏塔3底部经出釜液口3A-2与残液精馏塔体冷凝器排液口3B-1相连。The bottom of the residual liquid distillation tower 3 is connected to the liquid outlet 3B-1 of the condenser of the residual liquid distillation tower body through the kettle liquid outlet 3A-2.

粗品精馏塔2中部经粗品精馏塔体五硫化二磷侧线出气口2A-5与粗品精馏塔体五硫化二磷侧线上冷凝器2C连接后一路经粗品精馏塔体五硫化二磷侧线回流口2A-6回流连接至粗品精馏塔2,一路经粗品精馏塔体五硫化二磷侧线出液口2C-1连接至高纯五硫化二磷储罐。The middle part of the crude distillation tower 2 is connected to the condenser 2C on the side line of phosphorus pentasulfide of the crude distillation tower body through the phosphorus pentasulfide side line outlet 2A-5 of the crude distillation tower body. The crude distillation tower 2 is connected to the high-purity phosphorus pentasulfide storage tank through the phosphorus pentasulfide side liquid outlet 2C-1 of the crude distillation tower body.

粗品精馏塔2上部经粗品精馏塔体硫磷轻组分侧线出气口2A-7与粗品精馏塔体硫磷轻组分侧线上冷凝器2D连接后一路经粗品精馏塔体硫磷轻组分侧线回流口2A-8回流连接至粗品精馏塔2,一路经粗品精馏塔体硫磷轻组分侧线出液口2D-1连接至硫磷轻组分储罐。The upper part of the crude distillation tower 2 is connected to the condenser 2D on the side line of the sulfur and phosphorus light components in the crude distillation tower through the side line outlet 2A-7 of the sulfur and phosphorus light components in the crude distillation tower, and then passes through the sulfur and phosphorus in the crude distillation tower. The light component side reflux port 2A-8 is connected to the crude distillation tower 2, and is connected to the sulfur and phosphorus light component storage tank through the sulfur and phosphorus light component side outlet 2D-1 of the crude distillation tower body.

粗品精馏塔2顶部经粗品精馏塔体有机杂质侧线出气口2A-9与粗品精馏塔体有机杂质侧线上冷凝器2E连接后一路经粗品精馏塔体有机杂质侧线回流口2A-10 回流连接至粗品精馏塔2,一路经粗品精馏塔体有机杂质侧线出液口2E-1连接至有机杂质储罐。The top of the crude distillation tower 2 is connected to the organic impurity side line condenser 2E of the crude distillation tower through the organic impurity side outlet 2A-9 of the crude distillation tower, and then passes through the organic impurity side reflux port 2A-10 of the crude distillation tower. The reflux is connected to the crude distillation tower 2, and all the way is connected to the organic impurity storage tank through the organic impurity side outlet 2E-1 of the crude distillation tower body.

粗品精馏塔2底部经粗品精馏塔体出釜液口2A-2与粗品精馏塔体再沸器2B连接,粗品精馏塔体再沸器2B经粗品精馏塔体进釜液蒸汽口2A-3与粗品精馏塔2下部连接,形成循环回路;The bottom of the crude distillation tower 2 is connected to the crude distillation tower reboiler 2B through the crude distillation tower body outlet 2A-2, and the crude distillation tower reboiler 2B enters the still liquid steam through the crude distillation tower body. Port 2A-3 is connected to the lower part of crude distillation tower 2 to form a circulation loop;

残液精馏塔3顶部经残液精馏塔体有机杂质气侧线出气口3A-5与残液精馏塔体有机杂质侧线冷凝器3C连接后一路经残液精馏塔体有机杂质侧线回流口3A-6与残液精馏塔3上部连接,一路经残液精馏塔有机杂质侧线排液口3C-1连接至有机杂质储罐。The top of the residual liquid distillation tower 3 is connected to the organic impurity side line condenser 3C of the residual liquid distillation tower body through the organic impurity gas side outlet 3A-5 of the residual liquid distillation tower body, and then refluxes through the organic impurity side line of the residual liquid distillation tower body. Port 3A-6 is connected to the upper part of the residual liquid distillation tower 3, and is connected to the organic impurity storage tank through the organic impurity side drain port 3C-1 of the residual liquid distillation tower.

残液精馏塔3底部经残液精馏塔体出釜液口3A-2与残液精馏塔体再沸器3B连接,残液精馏塔体再沸器3B经残液精馏塔体进釜液汽口3A-3与残液精馏塔3下部连接。The bottom of the residual liquid distillation tower 3 is connected to the residual liquid distillation tower reboiler 3B through the residual liquid distillation tower body outlet 3A-2, and the residual liquid distillation tower reboiler 3B passes through the residual liquid distillation tower. The body inlet liquid vapor port 3A-3 is connected to the lower part of the residual liquid distillation tower 3.

实施例2Example 2

本实施例以气相连续合成和常压精馏提纯的方式为实施例来详细阐述。工艺流程见图1,所用的装置系统见图1,主要包括:合成反应装置1、粗品精馏塔2、残液精馏塔3。This embodiment uses gas phase continuous synthesis and atmospheric pressure distillation purification as an example to explain in detail. The process flow is shown in Figure 1, and the device system used is shown in Figure 1, which mainly includes: synthesis reaction device 1, crude product distillation tower 2, and residual liquid distillation tower 3.

其中,合成反应装置1为连续式气相反应装置,其进磷口1-1与供磷系统相连,其进硫口1-2与供硫磺系统相连,其出粗品口1-3与粗品精馏塔体进粗品口2A-1相连。Among them, the synthesis reaction device 1 is a continuous gas phase reaction device, its phosphorus inlet 1-1 is connected to the phosphorus supply system, its sulfur inlet 1-2 is connected to the sulfur supply system, and its crude product outlet 1-3 is connected to the crude product distillation The tower body is connected to the crude product inlet 2A-1.

粗品精馏塔2为常压塔板式装置,其共有五硫化二磷侧线、硫磷轻组分侧线和有机杂质侧线,其进粗品口2A-1与合成反应装置1出粗品口1-3相连,其粗品精馏塔体出釜液口2A-2与粗品精馏塔体再沸器2B相连,其粗品精馏塔体进釜液蒸汽口2A-3与粗品精馏塔体再沸器2B相连,粗品精馏塔体进硫磷物料气口2A-4与残液精馏塔体3硫磷物料侧线出气口3A-4相连,粗品精馏塔体五硫化二磷侧线出气口2A-5与粗品精馏塔体五硫化二磷侧线上冷凝器2C相连,粗品精馏塔体五硫化二磷侧线回流口2A-6与粗品精馏塔体五硫化二磷侧线上冷凝器2C相连, 粗品精馏塔体硫磷轻组分侧线出气口2A-7与粗品精馏塔体硫磷轻组分侧线上冷凝器2D相连,粗品精馏塔体硫磷轻组分侧线回流口2A-8与粗品精馏塔体硫磷轻组分侧线上冷凝器2D相连,粗品精馏塔体有机杂质侧线出气口2A-9与粗品精馏塔体有机杂质侧线上冷凝器2E相连,粗品精馏塔体有机杂质侧线回流口2A-10与粗品精馏塔体有机杂质侧线上冷凝器2E相连,粗品精馏塔体排残液口2B-1与残液精馏塔体进液口3A-1相连,粗品精馏塔体五硫化二磷侧线出液口2C-1与五硫化二磷产品存储系统相连,粗品精馏塔体硫磷轻组分侧线出液口2D-1与硫磷轻组分处理存储系统相连,粗品精馏塔体有机杂质侧线出液口2E-1与残液精馏塔有机杂质侧线排液口3C-1和有机杂质处理系统相连。The crude product rectification tower 2 is a normal pressure tray device, which has a phosphorus pentasulfide side line, a sulfur and phosphorus light component side line and an organic impurity side line. Its crude product inlet 2A-1 is connected to the crude product outlet 1-3 of the synthesis reaction device 1, and its crude product The liquid outlet 2A-2 of the distillation tower is connected to the reboiler 2B of the crude distillation tower, and the steam outlet 2A-3 of the liquid inlet of the crude distillation tower is connected to the reboiler 2B of the crude distillation tower. The sulfur and phosphorus material inlet port 2A-4 of the distillation tower body is connected to the sulfur and phosphorus material side outlet port 3A-4 of the residual liquid distillation tower body 3, and the phosphorus pentasulfide side outlet port 2A-5 of the crude distillation tower body is connected to the phosphorus pentasulfide of the crude distillation tower body. The side line condenser 2C is connected, the crude distillation tower body phosphorus pentasulfide side line reflux port 2A-6 is connected to the crude product rectification tower body phosphorus pentasulfide side line condenser 2C, the crude product rectification tower body sulfur and phosphorus light component side line outlet 2A-7 is connected to the side line condenser 2C of the crude product rectification tower body phosphorus pentasulfide. The condenser 2D on the side line of the sulfur and phosphorus light components in the crude distillation tower is connected to the condenser 2D on the side line of the sulfur and phosphorus light components in the crude distillation tower. , the crude distillation tower organic impurities side line outlet 2A-9 is connected to the crude distillation tower organic impurities side line condenser 2E, the crude distillation tower organic impurities side line reflux port 2A-10 is connected to the crude distillation tower organic impurities side line reflux port 2A-10 The condenser 2E on the side line is connected, the residual liquid discharge port 2B-1 of the crude distillation tower is connected with the liquid inlet 3A-1 of the residual liquid distillation tower, and the phosphorus pentasulfide side liquid outlet 2C-1 of the crude distillation tower is connected with the phosphorus pentasulfide product The storage system is connected. The sulfur and phosphorus light component side outlet 2D-1 of the crude distillation tower is connected to the sulfur and phosphorus light component treatment and storage system. The organic impurity side outlet 2E-1 of the crude distillation tower is connected to the residual liquid essence. The organic impurity side drain port 3C-1 of the distillation tower is connected to the organic impurity treatment system.

残液精馏塔3为常压填料式装置,其进液口3A-1与粗品精馏塔体排残液口2B-1相连,其出釜液口3A-2与残液精馏塔体再沸器3B相连,其进釜液汽口3A-3与残液精馏塔体再沸器3B相连,3A-4: 残液精馏塔体硫磷物料侧线出气口3A-4与粗品精馏塔体进硫磷物料气口2A-4相连,其硫磷物料侧线出气口3A-5与残液精馏塔体硫磷侧线冷凝器3C相连,其硫磷物料侧线回流口3A-6与残液精馏塔体冷凝器相连, 残液精馏塔有机杂质侧线排液口3C-1与粗品精馏塔体有机杂质侧线出液口2E-1和有机杂质处理系统相连。The raffinate distillation tower 3 is a normal-pressure packing device. Its liquid inlet 3A-1 is connected to the raffinate discharge port 2B-1 of the crude distillation tower body, and its liquid outlet 3A-2 is connected to the raffinate distillation tower body. Reboiler 3B is connected, and its liquid vapor inlet port 3A-3 is connected to the reboiler 3B of the residual liquid distillation tower body. 3A-4: The side outlet 3A-4 of the sulfur and phosphorus material in the residual liquid distillation tower body is connected to the crude product and refined product. The sulfur and phosphorus material inlet port 2A-4 of the distillation tower body is connected, its sulfur and phosphorus material side outlet port 3A-5 is connected to the sulfur and phosphorus side line condenser 3C of the residual liquid distillation tower body, and its sulfur and phosphorus material side line return port 3A-6 is connected to the residual liquid rectification tower body sulfur and phosphorus side line condenser 3A-6. The liquid distillation tower condenser is connected, and the organic impurity side outlet 3C-1 of the residual liquid distillation tower is connected to the organic impurity side outlet 2E-1 of the crude distillation tower and the organic impurity treatment system.

将300 ℃的有机杂质含量为0.2 %的气态黄磷a和470 ℃的有机杂质含量为0.6%的气态硫磺b分别以0.7 t和1.8 t/h的供料速率分别从合成反应装置1进磷口1-1和进硫口1-2加入到500 ℃的合成反应装置1进行反应而生成2.5 t/h五硫化二磷粗品c,生成的五硫化二磷粗品c从合成反应装置1出粗品口1-3排出。Gaseous yellow phosphorus a with an organic impurity content of 0.2% at 300°C and gaseous sulfur b with an organic impurity content of 0.6% at 470°C are fed into phosphorus from the synthesis reaction device 1 at feed rates of 0.7 t and 1.8 t/h respectively. Port 1-1 and sulfur inlet 1-2 are added to the synthesis reaction device 1 at 500°C for reaction to generate 2.5 t/h crude phosphorus pentasulfide c. The generated crude phosphorus pentasulfide c is discharged from the crude product outlet 1-3 of the synthesis reaction device 1.

从合成反应装置1排出的五硫化二磷粗品c通过粗品精馏塔体2A进粗品口2A-1进入常压粗品精馏塔体2A塔釜内(塔内压:101.2 KPa)被加热至525 ℃左右而气化成气体,气体依次进入到提馏段和精馏段,在上升过程中与从塔上部下来的液态物料进行热质交换,当温度逐步降至515 ℃时,分离出的五硫化二磷气体h通过粗品精馏塔体2A五硫化二磷侧线出气口2A-5排出并进入粗品精馏塔体五硫化二磷侧线上冷凝器2C内进行冷却,冷凝出的粗品精馏塔五硫化二磷液体i经粗品精馏塔体2A五硫化二磷侧线回流口2A-6以粗品精馏塔五硫化二磷回流液j返回粗品精馏塔体2A内进一步提纯,当粗品精馏塔五硫化二磷液体i中五硫化二磷含量99.2%、磷含量27.85%、硫含量71.8 %、有机杂质含量0.001%时,作为粗品精馏塔五硫化二磷产品k从粗品精馏塔体2A五硫化二磷侧线出液口2C-1排出,从而得到五硫化二磷产品并输送至五硫化二磷存储系统内存储。The crude phosphorus pentasulfide c discharged from the synthesis reaction device 1 passes through the crude product inlet 2A-1 of the crude distillation tower 2A and enters the atmospheric pressure crude distillation tower 2A still (internal pressure of the tower: 101.2 KPa), where it is heated to about 525°C. The gas is vaporized into gas, and the gas enters the stripping section and the rectifying section in turn. During the rising process, it exchanges heat and mass with the liquid material coming down from the upper part of the tower. When the temperature gradually drops to 515°C, the separated phosphorus pentasulfide gas h passes through the crude product The phosphorus pentasulfide side line outlet 2A-5 of the rectification tower body 2A is discharged and enters the phosphorus pentasulfide side line condenser 2C of the crude distillation tower body for cooling. The condensed phosphorus pentasulfide liquid i of the crude distillation tower refluxes through the phosphorus pentasulfide side line of the crude distillation tower body 2A. Port 2A-6 returns the crude distillation tower phosphorus pentasulfide reflux liquid j to the crude distillation tower body 2A for further purification. When the crude distillation tower phosphorus pentasulfide liquid i contains 99.2% phosphorus pentasulfide, 27.85% phosphorus, 71.8% sulfur and 71.8% organic impurities. When the content is 0.001%, the phosphorus pentasulfide product k of the crude distillation tower is discharged from the phosphorus pentasulfide side outlet 2C-1 of the crude distillation tower body 2A, thereby obtaining the phosphorus pentasulfide product and transporting it to the phosphorus pentasulfide storage system for storage.

分离出五硫化二磷产品的气体粗品继续上升并与精馏塔体2A上部下来的液态物料进一步进行热质传递而温度逐步降至286 ℃左右时(有机杂质沸点:280 ℃),分离出的含有多硫化物(P4Sx)和残留的硫磺等组分的粗品精馏塔硫磷轻组分蒸汽l通过粗品精馏塔体2A五硫化二磷侧线出气口2A-7排出并进入粗品精馏塔体硫磷化物轻组分侧线上冷凝器2D内进行冷却,冷凝出的粗品精馏塔硫磷化物轻组分液体m经粗品精馏塔体2A五硫化二磷侧线回流口2A-8以粗品精馏塔硫磷化物轻组分回流液n返回粗品精馏塔体2A内进一步提纯,当粗品精馏塔硫磷化物轻组分液体m中有机杂质含量≤0.01 %时,作为粗品精馏塔硫磷化物轻组分产物o从粗品精馏塔体2A五硫化二磷侧线出液口2D-1排出,从而得到硫磷化物轻组分产物并输送至硫磷化物轻组分处理存储系统,经过处理后作为原料返回合成反应装置1回用。The crude gas from which the phosphorus pentasulfide product is separated continues to rise and further undergoes heat and mass transfer with the liquid material coming down from the upper part of the distillation tower body 2A. When the temperature gradually drops to about 286°C (boiling point of organic impurities: 280°C), the separated polysulfide-containing The sulfur and phosphorus light component steam l of the crude distillation tower of the crude product (P 4 S The chemical light component side line condenser 2D is cooled, and the condensed crude distillation tower sulfur phosphide light component liquid m passes through the crude distillation tower body 2A phosphorus pentasulfide side line reflux port 2A-8 to the crude distillation tower sulfur phosphide The light component reflux liquid n is returned to the crude distillation tower body 2A for further purification. When the organic impurity content in the crude distillation tower sulfur phosphide light component liquid m is ≤0.01%, it is used as the crude distillation tower sulfur phosphide light component Product o is discharged from the phosphorus pentasulfide side outlet 2D-1 of the crude distillation tower body 2A, thereby obtaining the sulfur phosphide light component product and transporting it to the sulfur phosphide light component processing and storage system. After treatment, it is returned to the synthesis reaction device as raw material 1 time use.

分离出五硫化二磷和硫磷化物轻组分的剩余气体p(主要成分是有机杂质)通过粗品精馏塔体2A有机杂质侧线出气口2A-9排出并进入粗品精馏塔体有机杂质侧线上冷凝器2E内进行冷却,冷凝出的粗品精馏塔有机杂质液体q经粗品精馏塔体2A有机杂质侧线回流口2A-10以粗品精馏塔有机杂质回流液r返回粗品精馏塔体2A内进一步提纯,当粗品精馏塔有机杂质液体q达到纯度要求时作为粗品精馏塔有机杂质产物o从粗品精馏塔体2A有机杂质侧线出液口2E-1排出,然后与残液精馏塔3来的残液精馏塔有机杂质产物β混合成有机杂质γ并运至有机杂质处理系统进行集中处理。The remaining gas p (the main component is organic impurity) after separating the light components of phosphorus pentasulfide and sulfur phosphide is discharged through the organic impurity side outlet 2A-9 of the crude distillation tower body 2A and enters the organic impurity side line condenser of the crude distillation tower body Cooling is carried out in 2E, and the condensed organic impurity liquid q of the crude distillation tower is returned to the crude distillation tower body 2A for further use through the organic impurity side reflux port 2A-10 of the crude distillation tower body 2A as the organic impurity reflux liquid r of the crude distillation tower body 2A. Purification, when the organic impurity liquid q of the crude distillation tower reaches the purity requirement, it is discharged from the organic impurity side outlet 2E-1 of the crude distillation tower body 2A as the organic impurity product o of the crude distillation tower, and then mixed with the residual liquid distillation tower 3 The organic impurity product β from the residual liquid distillation tower is mixed into organic impurity γ and transported to the organic impurity treatment system for centralized treatment.

在分离过程中不断富集杂质的液体从粗品精馏塔1上部流下并以粗品精馏塔釜液d形式排出,一部分作为进再沸器2B的釜液e进入再沸器并被加热蒸发成粗品精馏塔釜液蒸汽f而重新进入粗品精馏塔体2A内精馏,精馏后形成的粗品精馏塔残液g排出。During the separation process, the liquid continuously enriched with impurities flows down from the upper part of the crude distillation tower 1 and is discharged in the form of crude distillation tower still liquid d. A part of it enters the reboiler as the still liquid e entering the reboiler 2B and is heated and evaporated into The crude rectification tower still liquid steam f re-enters the crude rectification tower body 2A for rectification, and the crude rectification tower residual liquid g formed after rectification is discharged.

从粗品精馏塔2排出的粗品精馏塔残液g经残液精馏塔体3A进液口3A-1进入残液精馏塔体3A进行再次精馏,从残液精馏塔体3A硫磷物料侧线出气口3A-4排出的残液精馏塔硫磷物料蒸汽x返回粗品精馏塔体2A内在286 ℃和101.2 KPa的条件下再次精馏以回收其中的硫磷物料,而剩余的气体在280 ℃和101.2 KPa下经残液精馏塔体3A有机杂质气侧线出气口3A-5作为残液精馏塔有机杂质蒸汽y排出,排出的残液精馏塔有机杂质蒸汽y进入残液精馏塔体有机杂质侧线冷凝器3C内冷却而成残液精馏塔有机杂质液z,残液精馏塔有机杂质液z经粗品精馏塔体2A有机杂质侧线回流口3A-6以残液精馏塔有机杂质回流液α返回粗品精馏塔体2A内进一步提纯,当残液精馏塔有机杂质液体z达到纯度要求时作为残液精馏塔有机杂质产物β从残液精馏塔体3A有机杂质侧线出液口3C-1排出,然后与粗品精馏塔2来的粗品精馏塔有机杂质产物s混合成有机杂质γ并运至有机杂质处理系统进行集中处理。The crude distillation tower residue g discharged from the crude distillation tower 2 enters the residue distillation tower 3A through the liquid inlet 3A-1 of the residue distillation tower 3A for re-distillation. The sulfur and phosphorus material steam x discharged from the side outlet 3A-4 of the residual liquid distillation tower returns to the crude distillation tower body 2A and is distilled again under the conditions of 286°C and 101.2 KPa to recover the sulfur and phosphorus material, and the remaining The gas is discharged as organic impurity vapor y of the residual liquid distillation tower through the organic impurity gas side outlet 3A-5 of the residual liquid distillation tower body 3A at 280 ℃ and 101.2 KPa. The discharged organic impurity steam y of the residual liquid distillation tower enters The residual liquid distillation tower organic impurity side line condenser 3C is cooled to form the residual liquid distillation tower organic impurity liquid z, and the residual liquid distillation tower organic impurity liquid z passes through the crude product distillation tower body 2A organic impurity side line reflux port 3A-6 The organic impurity reflux liquid α of the residual liquid distillation tower is returned to the crude distillation tower body 2A for further purification. When the organic impurity liquid z of the residual liquid distillation tower reaches the purity requirement, it is refined from the residual liquid as the organic impurity product β of the residual liquid distillation tower. The organic impurities are discharged from the side outlet 3C-1 of the distillation tower body 3A, and then mixed with the crude distillation tower organic impurity products s from the crude distillation tower 2 to form organic impurities γ and transported to the organic impurity treatment system for centralized treatment.

通过本实施例,可以获得纯度五硫化二磷含量99.2%、磷含量27.85%、硫含量71.8%、有机杂质含量0.001%的高纯五硫化二磷。所产的五硫化二磷产品完全达到了国标《工业五硫化二磷》(GB/T 13258-2016)中优级品标准,且其中有机质含量为0.005%,低于0.01%,获得高纯低有机杂质含量的五硫化二磷,远比利用传统蒸馏制五硫化二磷技术所产五硫化二磷的产品的品质要好,具有非常强的技术创新和优势。Through this embodiment, high-purity phosphorus pentasulfide with a purity of 99.2%, a phosphorus content of 27.85%, a sulfur content of 71.8%, and an organic impurity content of 0.001% can be obtained. The phosphorus pentasulfide products produced fully meet the national standard "Industrial phosphorus pentasulfide" (GB/T 13258-2016) for superior grade products, and the organic matter content is 0.005%, lower than 0.01%. High purity phosphorus pentasulfide with low organic impurity content is obtained. The quality of phosphorus pentasulfide products produced by traditional distillation technology is far better than that of phosphorus pentasulfide, and it has very strong technological innovation and advantages.

Claims (7)

1.高纯五硫化二磷制备系统,包括合成反应装置(1)、粗品精馏塔(2)、残液精馏塔(3),其特征在于,1. A high-purity phosphorus pentasulfide preparation system, including a synthesis reaction device (1), a crude distillation tower (2), and a residual liquid distillation tower (3), which is characterized by: 合成反应装置(1)顶部的粗品口(1-3)与粗品精馏塔(2)下部的粗品精馏塔体进粗品口(2A-1)相连;The crude product inlet (1-3) at the top of the synthesis reaction device (1) is connected to the crude product inlet (2A-1) of the crude product rectification tower body at the lower part of the crude product rectification tower (2); 粗品精馏塔(2)底部经粗品精馏塔体排残液口(2B-1)与残液精馏塔(3)中部的进液口(3A-1)相连,粗品精馏塔(2)顶部经粗品精馏塔体有机杂质侧线出气口(2A-9)与粗品精馏塔体有机杂质侧线上冷凝器(2E)连接后一路经粗品精馏塔体有机杂质侧线回流口(2A-10)回流连接至粗品精馏塔(2),一路经粗品精馏塔体有机杂质侧线出液口(2E-1)连接至有机杂质储罐;The bottom of the crude distillation tower (2) is connected to the liquid inlet (3A-1) in the middle of the crude distillation tower (3) through the residual liquid discharge port (2B-1) of the crude distillation tower body. ) The top of the crude distillation tower is connected to the organic impurity side line outlet (2A-9) of the crude distillation tower and the organic impurity side line condenser (2E) of the crude distillation tower, and then passes through the organic impurity side reflux port of the crude distillation tower (2A- 10) The reflux is connected to the crude distillation tower (2), and all the way is connected to the organic impurity storage tank through the organic impurity side outlet (2E-1) of the crude distillation tower body; 残液精馏塔(3)上部的残液精馏塔体硫磷物料侧线出气口(3A-4)与粗品精馏塔(2)的粗品精馏塔体进硫磷物料气口(2A-4)相连,残液精馏塔(3)顶部经残液精馏塔体有机杂质气侧线出气口(3A-5)与残液精馏塔体有机杂质侧线冷凝器(3C)连接后一路经残液精馏塔体有机杂质侧线回流口(3A-6)与残液精馏塔(3)上部连接,一路经残液精馏塔有机杂质侧线排液口(3C-1)连接至有机杂质储罐;The sulfur and phosphorus material side outlet (3A-4) in the upper part of the residual liquid distillation tower (3) and the sulfur and phosphorus material inlet (2A-4) in the crude distillation tower (2) ) are connected, the top of the residual liquid distillation tower (3) is connected to the organic impurity side line condenser (3C) of the residual liquid distillation tower body through the organic impurity gas side outlet (3A-5) of the residual liquid distillation tower body, and then passes through the residual liquid distillation tower body. The organic impurity side reflux port (3A-6) of the liquid distillation tower is connected to the upper part of the residual liquid distillation tower (3), and is connected to the organic impurity storage through the organic impurity side drain port (3C-1) of the residual liquid distillation tower. Can; 残液精馏塔(3)底部经出釜液口(3A-2)与残液精馏塔体冷凝器排液口(3B-1)相连。The bottom of the residual liquid distillation tower (3) is connected to the liquid outlet (3B-1) of the condenser of the residual liquid distillation tower body through the liquid outlet of the kettle (3A-2). 2.根据权利要求1所述的高纯五硫化二磷制备系统,其特征在于,粗品精馏塔(2)中部经粗品精馏塔体五硫化二磷侧线出气口(2A-5)与粗品精馏塔体五硫化二磷侧线上冷凝器(2C)连接后一路经粗品精馏塔体五硫化二磷侧线回流口(2A-6)回流连接至粗品精馏塔(2),一路经粗品精馏塔体五硫化二磷侧线出液口(2C-1)连接至高纯五硫化二磷储罐。2. The high-purity phosphorus pentasulfide preparation system according to claim 1, characterized in that the middle part of the crude distillation tower (2) is connected to the phosphorus pentasulfide side line of the crude distillation tower body through the gas outlet (2A-5) of the phosphorus pentasulfide side of the crude distillation tower body. After the upper condenser (2C) is connected, the reflux is connected to the crude distillation tower (2) through the phosphorus pentasulfide side line reflux port (2A-6) of the crude distillation tower body, and the reflux is connected to the phosphorus pentasulfide side line liquid outlet (2C- 1) Connect to the high-purity phosphorus pentasulfide storage tank. 3.根据权利要求2所述的高纯五硫化二磷制备系统,其特征在于,粗品精馏塔(2)上部经粗品精馏塔体硫磷轻组分侧线出气口(2A-7)与粗品精馏塔体硫磷轻组分侧线上冷凝器2D连接后一路经粗品精馏塔体硫磷轻组分侧线回流口(2A-8)回流连接至粗品精馏塔(2),一路经粗品精馏塔体硫磷轻组分侧线出液口(2D-1)连接至硫磷轻组分储罐。3. The high-purity phosphorus pentasulfide preparation system according to claim 2, characterized in that the upper part of the crude distillation tower (2) is connected to the crude distillation tower through the sulfur and phosphorus light component side outlet (2A-7). After the condenser 2D on the sulfur and phosphorus side line of the tower body is connected, the sulfur and phosphorus light component side line reflux port (2A-8) of the crude distillation tower body is refluxed and connected to the crude distillation tower (2). The sulfur and phosphorus light component side liquid outlet (2D-1) of the tower body is connected to the sulfur and phosphorus light component storage tank. 4.根据权利要求1所述的高纯五硫化二磷制备系统,其特征在于,粗品精馏塔(2)底部经粗品精馏塔体出釜液口(2A-2)与粗品精馏塔体再沸器(2B)连接,粗品精馏塔体再沸器(2B)经粗品精馏塔体进釜液蒸汽口(2A-3)与粗品精馏塔(2)下部连接,形成循环回路。4. The high-purity phosphorus pentasulfide preparation system according to claim 1, characterized in that the bottom of the crude distillation tower (2) is reboiled with the crude distillation tower body through the liquid outlet (2A-2) of the crude distillation tower body. The reboiler (2B) of the crude distillation tower is connected to the lower part of the crude distillation tower (2) through the still liquid steam port (2A-3) of the crude distillation tower to form a circulation loop. 5.根据权利要求1所述的高纯五硫化二磷制备系统,其特征在于,残液精馏塔(3)底部经残液精馏塔体出釜液口(3A-2)与残液精馏塔体再沸器(3B)连接,残液精馏塔体再沸器(3B)经残液精馏塔体进釜液汽口(3A-3)与残液精馏塔(3)下部连接。5. The high-purity phosphorus pentasulfide preparation system according to claim 1, characterized in that the bottom of the residual liquid distillation tower (3) is connected to the bottom of the residual liquid distillation tower through the residual liquid distillation tower body outlet (3A-2). The raffinate distillation tower body reboiler (3B) is connected to the lower part of the raffinate distillation tower (3) through the raffinate distillation tower body inlet liquid vapor port (3A-3). 6.根据权利要求1所述的高纯五硫化二磷制备系统,其特征在于,所述的合成反应装置是气相反应装置,或是液相反应装置;是连续式反应装置,或是间歇式反应装置。6. The high-purity phosphorus pentasulfide preparation system according to claim 1, characterized in that the synthesis reaction device is a gas phase reaction device or a liquid phase reaction device; a continuous reaction device or an intermittent reaction device. 7.根据权利要求1所述的高纯五硫化二磷制备系统,其特征在于,所述的粗品精馏塔和残液精馏塔是常压精馏装置,或是减压精馏装置;是连续式反应装置,或是间歇式反应装置。7. The high-purity phosphorus pentasulfide preparation system according to claim 1, characterized in that the crude product distillation tower and the residual liquid distillation tower are normal pressure distillation devices or vacuum distillation devices; they are continuous Reaction device, or batch reaction device.
CN202320107952.8U 2022-11-28 2023-02-03 High purity phosphorus pentasulfide preparation system Active CN220485340U (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2022231565963 2022-11-28
CN202223156596 2022-11-28

Publications (1)

Publication Number Publication Date
CN220485340U true CN220485340U (en) 2024-02-13

Family

ID=89837295

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202320107952.8U Active CN220485340U (en) 2022-11-28 2023-02-03 High purity phosphorus pentasulfide preparation system

Country Status (1)

Country Link
CN (1) CN220485340U (en)

Similar Documents

Publication Publication Date Title
CN105229119B (en) Purification equipment and purification method using the purification equipment
JP6518233B2 (en) Method and apparatus for the separation of ternary or multicomponent mixtures by distillation
TWI546113B (en) Process and apparatus for distillative separation of a mixture of three or more components
CN104968636B (en) For preparing the device of alkanol
CN101920964B (en) Method for purifying silicon tetrachloride by double-effect distillation
JPH025442B2 (en)
CN102675029B (en) A kind of differential pressure heat coupling separation of extractive distillation hexahydrotoluene and the method for toluene
CN110591752B (en) Method and device for recycling and purifying dichloromethane-white oil mixture
CN107188199A (en) It is a kind of that ammonium sulfate, the Processes and apparatus of sodium sulphate are reclaimed from waste water
CN101249312A (en) Separation device and method for purifying trichlorosilane by high-precision rectification
CN104744194B (en) A thermal integration process of de-light and de-heavy tower of isobutene unit
CN109438500B (en) Device and method for separating methyl chlorosilane by using internal thermally coupled rectifying tower
CN220485340U (en) High purity phosphorus pentasulfide preparation system
CN101519206A (en) Process for purifying trichlorosilane and silicon tetrachloride
EP0031097B1 (en) Method for distilling ethyl alcohol
CN111116522B (en) Device and method for single-column extraction and rectification separation of tetrahydrofuran-water mixture
CN102126958B (en) Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization
CN116281902B (en) High-purity phosphorus pentasulfide preparation process and system
CN105621370B (en) The recovery process and equipment of sulphur in a kind of diethylaluminum monochloride
CN106748883A (en) A kind of method for being thermally integrated three tower variable-pressure rectification separating acetonitrile methyl alcohol-benzene ternary azeotropes
CN107311871B (en) A kind of separation and purification method of monomethylamine dimethylamine mixture in methylamine synthesis system
CN116374970B (en) Purification process and device for preparing high-purity phosphorus pentasulfide
CN102134080A (en) Heat-pump energy-saving separating device for extracting trichlorosilane by adopting static mixing booster and method
CN105217654B (en) Alkylation waste sulfuric acid recycling treatment device and method
CN109529394A (en) Partition wall rectifying device and rectifying method thereof

Legal Events

Date Code Title Description
GR01 Patent grant
GR01 Patent grant