CN115611784A - A method for removing nitrogen dioxide in dimethyl sulfoxide - Google Patents
A method for removing nitrogen dioxide in dimethyl sulfoxide Download PDFInfo
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 title claims abstract description 127
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 title claims abstract description 73
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000007872 degassing Methods 0.000 claims abstract description 7
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 abstract description 18
- 238000000926 separation method Methods 0.000 abstract description 10
- 238000007086 side reaction Methods 0.000 abstract description 2
- 229960001760 dimethyl sulfoxide Drugs 0.000 abstract 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 10
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 9
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 235000010344 sodium nitrate Nutrition 0.000 description 5
- 239000004317 sodium nitrate Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- XOCUXOWLYLLJLV-UHFFFAOYSA-N [O].[S] Chemical group [O].[S] XOCUXOWLYLLJLV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- -1 organic synthesis Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明属于二甲基亚砜分离二氧化氮技术领域，具体地而言为一种脱除二甲基亚砜中二氧化氮的方法，该方法包括在脱气塔设备中二氧化氮与二甲基亚砜的混合溶液连续从二氧化氮脱除塔顶部进入，塔顶连续脱除二氧化氮的气体；塔底连续脱除的二甲基亚砜液体的分离方法。本发明溶解在二甲基亚砜中的二氧化氮在特定的脱除塔设备中进行连续脱除。脱除塔温度通过脱除塔中的换热设施控制，降低安全隐患、减少二甲基亚砜生成二甲基砜副反应产生。
The invention belongs to the technical field of separating nitrogen dioxide from dimethyl sulfoxide, and specifically relates to a method for removing nitrogen dioxide in dimethyl sulfoxide, which comprises combining nitrogen dioxide and nitrogen dioxide in a degassing tower equipment. The mixed solution of methyl sulfoxide enters continuously from the top of the nitrogen dioxide removal tower, and the nitrogen dioxide gas is continuously removed from the top of the tower; the separation method of the dimethyl sulfoxide liquid that is continuously removed from the bottom of the tower. In the present invention, nitrogen dioxide dissolved in dimethyl sulfoxide is continuously removed in a specific removal tower device. The temperature of the removal tower is controlled by the heat exchange facilities in the removal tower to reduce potential safety hazards and reduce the side reaction of dimethyl sulfoxide to dimethyl sulfone.
Description
技术领域technical field
本发明属于二甲基亚砜分离二氧化氮技术领域，具体地而言为一种脱除二甲基亚砜中二氧化氮的方法。The invention belongs to the technical field of nitrogen dioxide separation by dimethyl sulfoxide, and specifically relates to a method for removing nitrogen dioxide in dimethyl sulfoxide.
背景技术Background technique
二甲基亚砜是典型的精细化工产品。是电子、碳纤维、医药、农药、有机合成等领域中的重要中间体，具有广泛的使用用途。二甲基亚砜是20世纪60年代发展起来的高效有机溶剂及新兴萃取剂，二甲基亚砜分子中含有半极性的硫-氧基团，此基团能有效地与金属离子生成配位络合物或溶剂化物。因此二甲基亚砜在盐酸、硫酸介质中能萃取金、银、铂等贵金属，也能萃取铀、钍等稀土元素。更为可贵的是，它又是极性有机溶剂，对有机物、无机物都有良好的溶解性且渗透性强等特点。所以被广泛的应有在电子、碳纤维、医药、农药、有机合成、贵金属提取等领域。Dimethyl sulfoxide is a typical fine chemical product. It is an important intermediate in the fields of electronics, carbon fiber, medicine, pesticide, organic synthesis, etc., and has a wide range of uses. Dimethyl sulfoxide is a high-efficiency organic solvent and emerging extractant developed in the 1960s. The dimethyl sulfoxide molecule contains a semi-polar sulfur-oxygen group, which can effectively form a complex with metal ions. complexes or solvates. Therefore, dimethyl sulfoxide can extract precious metals such as gold, silver, and platinum in hydrochloric acid and sulfuric acid media, and can also extract rare earth elements such as uranium and thorium. What's more valuable is that it is also a polar organic solvent, which has the characteristics of good solubility and strong permeability to organic and inorganic substances. Therefore, it is widely used in the fields of electronics, carbon fiber, medicine, pesticides, organic synthesis, and precious metal extraction.
在二甲基亚砜制备过程中，是采用二氧化氮为氧化剂、纯氧、二甲基硫醚为原料的氧化制备方法。此方法，二甲基硫醚被氧化为二甲基亚砜过程中，二氧化氮会大量溶解在二甲基亚砜中。在传统的脱除二氧化氮过程为，向二甲基亚砜混合溶液中加碱进行中和，生成硝酸钠废盐。然后在二甲基亚砜精馏过程中采用蒸发脱除硝酸钠废盐。在蒸发脱盐过程中安全隐患大；国内外出现很多安全事故，并且又带来大量的含二甲基亚砜硝酸钠废盐排放。所以发展安全高效、无“三废”排放的新方法，从安全和环境影响两个方面都具有重要意义。In the preparation process of dimethyl sulfoxide, it is an oxidation preparation method using nitrogen dioxide as oxidant, pure oxygen and dimethyl sulfide as raw materials. In this method, during the oxidation of dimethyl sulfide to dimethyl sulfoxide, a large amount of nitrogen dioxide will be dissolved in dimethyl sulfoxide. In the traditional nitrogen dioxide removal process, alkali is added to the mixed solution of dimethyl sulfoxide for neutralization to generate sodium nitrate waste salt. Then use evaporation to remove sodium nitrate waste salt in the rectification process of dimethyl sulfoxide. There are great potential safety hazards in the process of evaporative desalination; many safety accidents have occurred at home and abroad, and a large amount of waste salt containing dimethyl sulfoxide and sodium nitrate has been discharged. Therefore, it is of great significance to develop new methods that are safe, efficient, and free of "three wastes" from the aspects of safety and environmental impact.
发明内容Contents of the invention
本发明所要解决的技术问题在于提供一种脱除二甲基亚砜中二氧化氮的方法，解决安全隐患，并不会产生氮氧化物尾气排放。The technical problem to be solved by the present invention is to provide a method for removing nitrogen dioxide in dimethyl sulfoxide, which solves potential safety hazards and does not generate nitrogen oxide tail gas emissions.
本发明是这样实现的，The present invention is achieved like this,
一种脱除二甲基亚砜中二氧化氮的方法，该方法包括在脱气塔设备中二氧化氮与二甲基亚砜的混合溶液连续从二氧化氮脱除塔顶部进入，塔顶连续脱除二氧化氮的气体；塔底连续脱除的二甲基亚砜液体的分离方法。A method for removing nitrogen dioxide in dimethyl sulfoxide, the method comprises that the mixed solution of nitrogen dioxide and dimethyl sulfoxide in the degassing tower equipment continuously enters from the top of the nitrogen dioxide removal tower, and the top of the tower The gas of nitrogen dioxide is continuously removed; the separation method of dimethyl sulfoxide liquid which is continuously removed at the bottom of the tower.
进一步地，脱除条件为压力：0.0MPa～0.3MPa，温度：15～180℃。Further, the removal conditions are pressure: 0.0MPa-0.3MPa, temperature: 15-180°C.
进一步地，脱除体系温度为：20～120℃、压力为：0.0MPa～0.2MPa。Further, the temperature of the removal system is 20-120° C., and the pressure is 0.0 MPa-0.2 MPa.
进一步地，混合液体进脱除塔的流速0.01～10.0t/h；对应处理的二氧化氮在二甲基亚砜中的质量比为1％～40％的混合溶液。Further, the flow rate of the mixed liquid into the removal tower is 0.01-10.0 t/h; the mass ratio of the corresponding nitrogen dioxide in dimethyl sulfoxide is 1%-40% of the mixed solution.
进一步地，所述脱除塔设备为板式塔，脱除塔长径比范围(1～20):1，包括沿着垂直方向设置的多个塔盘以及设置在脱除塔轴向上的升气管，二氧化氮与二甲基亚砜在塔盘中分离，分离出的二氧化氮由塔的升气管到塔的顶部放出。Further, the removal tower equipment is a plate tower, and the length-to-diameter ratio of the removal tower ranges from (1 to 20): 1, including a plurality of trays arranged in the vertical direction and a riser arranged in the axial direction of the removal tower. In the gas pipe, nitrogen dioxide and dimethyl sulfoxide are separated in the tray, and the separated nitrogen dioxide is released from the gas riser of the tower to the top of the tower.
本发明与现有技术相比，有益效果在于：Compared with the prior art, the present invention has the beneficial effects of:
1.溶解在二甲基亚砜中的二氧化氮在特定的脱除塔设备中进行连续脱除。脱除塔温度通过脱除塔中的换热设施控制，降低安全隐患、减少二甲基亚砜生成二甲基砜副反应产生。1. Nitrogen dioxide dissolved in dimethyl sulfoxide is continuously removed in a specific removal tower equipment. The temperature of the removal tower is controlled by the heat exchange facilities in the removal tower to reduce potential safety hazards and reduce the side reaction of dimethyl sulfoxide to dimethyl sulfone.
2.本发明分离产物为二甲基亚砜和二氧化氮。二氧化氮会再次被利用在二甲基硫醚氧化中，分离出的二甲基亚砜直接去二甲基亚砜精馏。相比较，本发明的方法不会产生氮氧化物尾气排放；也不会有二甲基亚砜与二氧化氮分离过程所产生的大量含有有机物的硝酸钠废盐；还有分离硝酸钠废盐所产生的安全隐患。2. The separation products of the present invention are dimethyl sulfoxide and nitrogen dioxide. Nitrogen dioxide will be used again in the oxidation of dimethyl sulfide, and the separated dimethyl sulfoxide will go directly to dimethyl sulfoxide for rectification. In comparison, the method of the present invention will not produce nitrogen oxide tail gas emissions; there will not be a large amount of sodium nitrate waste salt containing organic matter produced by the separation process of dimethyl sulfoxide and nitrogen dioxide; there is also separation of sodium nitrate waste salt resulting safety hazards.
3.本发明的脱除塔为长径比大的脱除塔设备。通入含有二氧化氮的二甲基亚砜混合溶液的位置位于脱除塔顶部，脱除的二氧化氮气体通过升气管连续从塔的顶部放出；脱除二氧化氮气体的二甲基亚砜通过降液盘连续从塔的底部排放。避免二氧化氮与二甲基亚砜再次接触，有利于二氧化氮脱除能连续进行，有利于大规模、连续化工业生产。3. The removal tower of the present invention is a removal tower device with a large aspect ratio. The position where the dimethyl sulfoxide mixed solution containing nitrogen dioxide is introduced is located at the top of the removal tower, and the removed nitrogen dioxide gas is continuously released from the top of the tower through the gas riser; the dimethyl sulfoxide for removal of nitrogen dioxide gas Sulfone is continuously discharged from the bottom of the column through the downcomer. Avoiding the re-contact of nitrogen dioxide and dimethyl sulfoxide is conducive to continuous removal of nitrogen dioxide and large-scale and continuous industrial production.
4.通过控制脱除体系的温度、压力、液位及混合液体进料量。使得脱除过程始终保持连续、稳定的生产状态。且分离产物二氧化氮会再次利用不进行排放。达到二氧化氮脱除率：80％以上。4. By controlling the temperature, pressure, liquid level and mixed liquid feed volume of the removal system. Make the removal process always maintain a continuous and stable production state. And the separated product nitrogen dioxide will be reused without discharge. Reach nitrogen dioxide removal rate: more than 80%.
附图说明Description of drawings
图1为本发明方法提供的方法的工艺图；Fig. 1 is the process diagram of the method that the inventive method provides;
图2为本发明方法采用的脱硫塔的部分塔节的结构示意图。Fig. 2 is a structural schematic diagram of some tower sections of the desulfurization tower used in the method of the present invention.
具体实施方式detailed description
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。In order to make the object, technical solution and advantages of the present invention more clear, the present invention will be further described in detail below in conjunction with the examples. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
参见图1所示，本发明提供一种脱除二甲基亚砜中二氧化氮的方法，该方法包括在脱气塔设备中二氧化氮与二甲基亚砜的混合溶液连续从二氧化氮脱除塔顶部进入，塔顶连续脱除二氧化氮的气体；塔底连续脱除的二甲基亚砜液体的分离方法。脱除条件为压力：0.0MPa～0.3MPa，温度：15～180℃。优选地，脱除体系温度为：20～120℃、压力为：0.0MPa～0.2MPa。Referring to shown in Fig. 1, the present invention provides a kind of method of removing nitrogen dioxide in dimethyl sulfoxide, and the method comprises that the mixed solution of nitrogen dioxide and dimethyl sulfoxide continuously from The top of the nitrogen removal tower enters, and the nitrogen dioxide gas is continuously removed from the top of the tower; the separation method of the dimethyl sulfoxide liquid that is continuously removed from the bottom of the tower. The removal conditions are pressure: 0.0MPa～0.3MPa, temperature: 15～180℃. Preferably, the temperature of the removal system is 20-120° C., and the pressure is 0.0 MPa-0.2 MPa.
混合液体进脱除塔的流速0.01～10.0t/h；对应处理的二氧化氮在二甲基亚砜中的质量比为1％～40％的混合溶液。The flow rate of the mixed liquid into the removal tower is 0.01-10.0 t/h; the mass ratio of nitrogen dioxide to dimethyl sulfoxide is 1%-40% of the mixed solution.
参见图2所示，脱除塔设备为板式塔，脱除塔长径比范围(1～20):1，包括沿着垂直方向设置的多个塔盘以及设置在脱除塔轴向上的升气管1，二氧化氮与二甲基亚砜在塔盘3中分离，分离出的二氧化氮由塔的升气管2到塔的顶部放出。脱除塔中有换热管及夹套加热设施2，有测温、测压、液位等设施。As shown in Figure 2, the removal tower equipment is a plate tower, the length-to-diameter ratio of the removal tower ranges from (1 to 20): 1, and includes a plurality of trays arranged along the vertical direction and a set of trays arranged in the axial direction of the removal tower. Gas riser 1, nitrogen dioxide and dimethyl sulfoxide are separated in
本发明在压力：0.0MPa～0.3MPa，温度：15～120℃的脱气条件下，在大长径比脱气塔中进行连续脱气。过程中被脱除的二氧化氮气体被重新利用，已脱除二氧化氮的二甲基亚砜去精馏处理。通过控制脱除体系的温度、压力、液位来实现连续进料、出料。二氧化氮脱除率达到80％以上。本发明是建立连续高效、安全、环境友好的溶解在二甲基亚砜中二氧化氮脱除的方法。In the present invention, under the degassing conditions of pressure: 0.0MPa-0.3MPa, temperature: 15-120 DEG C, continuous degassing is carried out in a degassing tower with a large aspect ratio. The nitrogen dioxide gas removed during the process is reused, and the dimethyl sulfoxide that has been removed from the nitrogen dioxide is subjected to rectification treatment. Continuous feeding and discharging are realized by controlling the temperature, pressure and liquid level of the removal system. The removal rate of nitrogen dioxide reaches more than 80%. The present invention is to establish a continuous efficient, safe and environment-friendly method for removing nitrogen dioxide dissolved in dimethyl sulfoxide.
溶解在二甲基亚砜的二氧化氮混合液连续通入大长径比脱气塔(见塔节简图)中，在本发明限定的压力及温度条件下，使二氧化氮与二甲基亚砜在塔盘中分离，分离出的二氧化氮由塔的升气管到塔的顶部放出；分离的二甲基亚砜由降液塔盘连续从塔的底部排出；控制塔釜液位从而得到一种连续脱除二甲基亚砜中二氧化氮的方法。The mixed solution of nitrogen dioxide dissolved in dimethyl sulfoxide is continuously passed into a large length-to-diameter ratio degassing tower (see the tower section diagram), and under the pressure and temperature conditions limited by the present invention, nitrogen dioxide and dimethyl The base sulfoxide is separated in the tray, and the separated nitrogen dioxide is released from the riser of the tower to the top of the tower; the separated dimethyl sulfoxide is continuously discharged from the bottom of the tower through the downcomer tray; the liquid level of the tower still is controlled Thereby a method for continuously removing nitrogen dioxide in dimethyl sulfoxide is obtained.
(1)本发明的反应机理：(1) reaction mechanism of the present invention:
控制反应温度及压力，防止发生二甲基亚砜被氧化反应成二甲基砜Control the reaction temperature and pressure to prevent dimethyl sulfoxide from being oxidized to dimethyl sulfone
C2H6SO+NO2→C2H6SO2+NOC2H6SO+NO2→C2H6SO2+NO
(2)本发明的二氧化氮脱除率定义：(2) Nitrogen dioxide removal rate definition of the present invention:
脱除率＝(脱除的二甲基亚砜中二氧化氮的质量/脱除前的二甲基亚砜中二氧化氮的质量)*100％。Removal rate=(mass of nitrogen dioxide in removed dimethyl sulfoxide/mass of nitrogen dioxide in dimethyl sulfoxide before removal)*100%.
(3)结合本发明的方法及附图，脱除塔中以二甲基亚砜、二氧化氮为介质，配制二甲基亚砜质量浓度50～90％的混合溶液。二甲基亚砜质量浓度更优选为70～90％。(3) In combination with the method and accompanying drawings of the present invention, a mixed solution with a mass concentration of dimethyl sulfoxide of 50-90% is prepared in the removal tower using dimethyl sulfoxide and nitrogen dioxide as a medium. The mass concentration of dimethyl sulfoxide is more preferably 70-90%.
(4)本发明脱除压力：0.0MPa～0.3MPa，温度：15～180℃；脱除体系温度更优选为20～120℃。(4) The removal pressure of the present invention: 0.0MPa-0.3MPa, temperature: 15-180°C; the temperature of the removal system is more preferably 20-120°C.
(5)二甲基亚砜、二氧化氮混合溶液，自脱除塔顶部向每块塔盘扩散。为了增大混合液中塔盘的停留时间，根据脱除塔高度及塔盘数量来调整。调节混合液的进料流量。比选出脱除塔高度及塔盘数量的最优方案，最优方案是塔高6米、塔盘10块。(5) The mixed solution of dimethyl sulfoxide and nitrogen dioxide diffuses from the top of the removal tower to each tray. In order to increase the residence time of the trays in the mixed liquid, it is adjusted according to the height of the removal tower and the number of trays. Adjust the feed flow rate of the mixed liquor. Compare and select the optimal solution for the height of the removal tower and the number of trays. The optimal solution is a tower height of 6 meters and 10 trays.
(6)控制脱除体系的温度、压力、液位及混合液进料量。使得混合液分离阶段，始终保持已分离的二氧化氮与二甲基亚砜不在接触，且二甲基亚砜作为氧化产物不再参与氧化反应。加入脱除塔中的混合溶液压力：0.0MPa～0.3MPa，更优选为0.0MPa～0.2MPa。(6) Control the temperature, pressure, liquid level and feed volume of the mixed liquid in the removal system. In the separation stage of the mixed liquid, the separated nitrogen dioxide and dimethyl sulfoxide are always kept out of contact, and dimethyl sulfoxide, as an oxidation product, no longer participates in the oxidation reaction. The pressure of the mixed solution fed into the removal tower: 0.0MPa-0.3MPa, more preferably 0.0MPa-0.2MPa.
(7)不同浓度的混合溶液在温度、压力及每块塔盘的作用下，二甲基亚砜、二氧化氮分离快速进行。破坏溶解度的分离时间为0.01s～100s。(7) The separation of dimethyl sulfoxide and nitrogen dioxide is carried out rapidly under the action of temperature, pressure and each tray of mixed solutions of different concentrations. The separation time to destroy the solubility is 0.01s～100s.
实施例Example
实施例1，以100mL/min的流速进入脱除塔。保持脱除温度为50℃，压力为0.05MPa，持续脱除30min。检测及计算：二氧化氮脱除率为76.5％，二甲基砜生成率0.1％。Example 1, enter the removal tower with a flow rate of 100mL/min. Keep the removal temperature at 50°C and the pressure at 0.05 MPa, and continue the removal for 30 minutes. Detection and calculation: the removal rate of nitrogen dioxide is 76.5%, and the generation rate of dimethyl sulfone is 0.1%.
实施例2，本实施例中二甲基亚砜、二氧化氮混合试剂(质量比：5:1)：以100mL/min的流速进入脱除塔。保持脱除温度为50℃，压力为0.02MPa，持续脱除30min。检测及计算：二氧化氮脱除率为79.1％，二甲基砜生成率0.08％。Example 2, in this example, the mixed reagent of dimethyl sulfoxide and nitrogen dioxide (mass ratio: 5:1): enters the removal tower at a flow rate of 100 mL/min. Keep the removal temperature at 50°C and the pressure at 0.02MPa, and continue the removal for 30 minutes. Detection and calculation: the removal rate of nitrogen dioxide is 79.1%, and the generation rate of dimethyl sulfone is 0.08%.
实施例3，本实施例中二甲基亚砜、二氧化氮混合试剂(质量比：5:1)：以100mL/min的流速进入脱除塔。保持脱除温度为80℃，压力为0.05MPa，持续脱除30min。检测及计算：二氧化氮脱除率为85.2％，二甲基砜生成率0.15％。Example 3, in this example, the mixed reagent of dimethyl sulfoxide and nitrogen dioxide (mass ratio: 5:1): enters the removal tower at a flow rate of 100 mL/min. Keep the removal temperature at 80°C and the pressure at 0.05MPa, and continue the removal for 30 minutes. Detection and calculation: the removal rate of nitrogen dioxide is 85.2%, and the generation rate of dimethyl sulfone is 0.15%.
实施例4，本实施例中二甲基亚砜、二氧化氮混合试剂(质量比：5:1)：以100mL/min的流速进入脱除塔。保持脱除温度为80℃，压力为0.02MPa，持续脱除30min。检测及计算：二氧化氮脱除率为93.4％，二甲基砜生成率0.12％。Example 4, in this example, the mixed reagent of dimethyl sulfoxide and nitrogen dioxide (mass ratio: 5:1): enters the removal tower at a flow rate of 100 mL/min. Keep the removal temperature at 80°C and the pressure at 0.02MPa, and continue the removal for 30 minutes. Detection and calculation: the removal rate of nitrogen dioxide is 93.4%, and the generation rate of dimethyl sulfone is 0.12%.
实施例5，本实施例中二甲基亚砜、二氧化氮混合试剂(质量比：5:1)：以100mL/min的流速进入脱除塔。保持脱除温度为120℃，压力为0.05MPa，持续脱除30min。检测及计算：二氧化氮脱除率为95.2％，二甲基砜生成率0.21％。Example 5, in this example, the mixed reagent of dimethyl sulfoxide and nitrogen dioxide (mass ratio: 5:1): enters the removal tower at a flow rate of 100 mL/min. Keep the removal temperature at 120°C and the pressure at 0.05 MPa, and continue the removal for 30 minutes. Detection and calculation: the removal rate of nitrogen dioxide is 95.2%, and the generation rate of dimethyl sulfone is 0.21%.
实施例6，本实施例中二甲基亚砜、二氧化氮混合试剂(质量比：5:1)：以100mL/min的流速进入脱除塔。保持脱除温度为120℃，压力为0.02MPa，持续脱除30min。检测及计算：二氧化氮脱除率为96.6％，二甲基砜生成率0.16％。Example 6, in this example, the mixed reagent of dimethyl sulfoxide and nitrogen dioxide (mass ratio: 5:1): enters the removal tower at a flow rate of 100 mL/min. Keep the removal temperature at 120°C and the pressure at 0.02MPa, and continue the removal for 30 minutes. Detection and calculation: the removal rate of nitrogen dioxide is 96.6%, and the generation rate of dimethyl sulfone is 0.16%.
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the protection of the present invention. within range.
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