CN220485340U - High purity phosphorus pentasulfide preparation system - Google Patents
High purity phosphorus pentasulfide preparation system Download PDFInfo
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- 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
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- CYQAYERJWZKYML-UHFFFAOYSA-N phosphorus pentasulfide Chemical compound S1P(S2)(=S)SP3(=S)SP1(=S)SP2(=S)S3 CYQAYERJWZKYML-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 286
- 239000007788 liquid Substances 0.000 claims abstract description 163
- 239000012535 impurity Substances 0.000 claims abstract description 106
- 239000012043 crude product Substances 0.000 claims abstract description 52
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 19
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 58
- 239000011593 sulfur Substances 0.000 claims description 58
- 229910052717 sulfur Inorganic materials 0.000 claims description 58
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 55
- 239000011574 phosphorus Substances 0.000 claims description 55
- 229910052698 phosphorus Inorganic materials 0.000 claims description 55
- 238000010992 reflux Methods 0.000 claims description 34
- 238000003860 storage Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000005292 vacuum distillation Methods 0.000 claims description 6
- 238000010574 gas phase reaction Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 35
- 239000010687 lubricating oil Substances 0.000 abstract description 4
- QCJQWJKKTGJDCM-UHFFFAOYSA-N [P].[S] Chemical compound [P].[S] QCJQWJKKTGJDCM-UHFFFAOYSA-N 0.000 abstract 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract 1
- 150000002910 rare earth metals Chemical class 0.000 abstract 1
- 238000000746 purification Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000005077 polysulfide Substances 0.000 description 3
- 229920001021 polysulfide Polymers 0.000 description 3
- 150000008117 polysulfides Polymers 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001577 simple distillation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 2
- 239000005947 Dimethoate Substances 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003987 organophosphate pesticide Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- ATROHALUCMTWTB-OWBHPGMISA-N phoxim Chemical compound CCOP(=S)(OCC)O\N=C(\C#N)C1=CC=CC=C1 ATROHALUCMTWTB-OWBHPGMISA-N 0.000 description 1
- 229950001664 phoxim Drugs 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
Description
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.
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