CN201406388Y - Equipment for preparing aromatic sulfonic acid by utilizing gas-phase sulfonation of aromatic organic matters - Google Patents
Equipment for preparing aromatic sulfonic acid by utilizing gas-phase sulfonation of aromatic organic matters Download PDFInfo
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- CN201406388Y CN201406388Y CN2009201027542U CN200920102754U CN201406388Y CN 201406388 Y CN201406388 Y CN 201406388Y CN 2009201027542 U CN2009201027542 U CN 2009201027542U CN 200920102754 U CN200920102754 U CN 200920102754U CN 201406388 Y CN201406388 Y CN 201406388Y
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Abstract
The utility model relates to equipment for preparing aromatic sulfonic acid by utilizing a rotating packed bed by adopting gas-phase sulfur trioxide to sulfonate aromatic organic matters, solving theproblems of the existing method for preparing the aromatic sulfonic acid by using gas sulfur trioxide as a sulfonating agent to sulfonate the aromatic organic matters. The equipment comprises a rotating packed bed, wherein a liquid inlet of the rotating packed bed is connected with a material storing tank, a gas inlet of the rotating packed bed is connected with a sulfur trioxide mixed gas source,and a liquid outlet of the rotating packed bed is connected with a product storing tank by a tube type heat exchanger. The equipment has the beneficial effects of easily controlling reaction temperature, reducing the occurrence of side reaction, improving selectivity of reaction, avoiding environmental pollution, saving energy, and having light mass, convenient installation and maintenance and convenient turning on and turning off.
Description
Technical field
The utility model relates to a kind of rotary packed bed equipment that is prepared aromatics sulfonic acid by gas phase sulfur trioxide sulfonated aromatic type organic that utilizes.
Background technology
Aromatics sulfonic acid is with sulphonating agent generation sulfonation reactions such as fragrant type organic matter and the vitriol oil, oleum or sulphur trioxides and the sulfonic acid type organic that obtains.With the vitriol oil or oleum is sulphonating agent when carrying out sulfonation reaction, has water to generate in the reaction process, can form spent acid, contaminate environment, and etching apparatus is unfavorable for the carrying out of sulfonation reaction; And be that sulphonating agent is when carrying out sulfonation reaction with the gas sulphur trioxide, have that the sulfonation ability is strong, transformation efficiency is high, product purity is high and does not produce characteristics such as spent acid, but its technology and method are confined to the organic sulfonation of macromolecule more at present, for small molecular weight organism such as benzene, toluene, especially the organic sulfonation of thermo-sensitivity is then studied less.Sulfonation reactor commonly used at present has still formula, pot group type, membrane type, jet-type etc.Wherein still formula and the alternate contact area of pot group type sulfonation reactor are little, the mass-and heat-transfer weak effect, and production efficiency is low; The film sulfonation reactor complex structure, the processing of equipment, manufacturing and setting accuracy require all higher, investment cost is big, turndown ratio is little, start-stop car inconvenience, and heat interchanging area is limited, some quick strong exothermal reaction is easy to generate local superheating, the carrying out that is unfavorable for sulfonation reaction especially for the organic sulfonation of some thermo-sensitivity, can reduce the selectivity of product.
The patent of invention of carrying out sulfonation reaction with jet sulfonation reactor mainly contains: (US 4113438 in U.S. Chemithon company, 1978) ram-jet formula sulfonation reactor (ImpactJet Reactor), this reactor atomizes high speed charging organism by Venturi, form huge surface-area, and with the SO that introduces simultaneously
3-air mixture carries out violent sulfonation reaction of moment in nozzle trunnion portion, and and then reaction mixture by the cooling of cold cycle material chilling, avoids system temperature too high, influences product color.According to patent report, this device can be used for the sulfonation of plurality of raw materials such as dodecylbenzene, alcohol ether and alpha-olefin; The injection circulation reactor of University Of Tianjin (CN96107060) sprays sulfonation reaction with high speed liquid phase workmanship as medium, adopt and force the outer circulation interchanger, and the sulfonation of toluene studied, it is reported that this technology has solved the problem of heat extraction cooling, the products obtained therefrom quality is better, and this device can be used for the sulfonation of plurality of raw materials such as benzene, alkylbenzene, fatty alcohol-ether and alpha-olefin.More than the common ground of several reactors are the purposes that must repeatedly circulate and just can reach the cooling heat extraction and improve transformation efficiency sulfonated products, and sulfonation reaction is a fast strong exothermic process, comprise a series of complex reaction (parallel reactor and consecutive reaction), repeatedly circulation causes the generation of side reaction easily, influence quality product, and the viscosity of sulfonated products also is unfavorable for circulation and injection far above raw material under high conversion.So according to reaction characteristics, the sulfonation reactor that exploitation is suitable is optimized technology, has very important significance to obtain the highly purified sulfonic acid product of high quality.
Summary of the invention
The utility model is that sulphonating agent sulfonated aromatic type organic prepares the problems referred to above that exist in the method for aromatics sulfonic acid in order to solve in the prior art with the gas sulphur trioxide, a kind of equipment of preparing aromatic sulfonic acid by gas-phase sulphonation of aromatic organic compound is provided, it utilizes rotary packed bed efficient mass transfer characteristic that sulfonation reaction is once finished, liquid product does not circulate to suppress the generation of side reaction, thereby improve the purity and the yield of aromatics sulfonic acid, reach the purpose of enhancing productivity, cutting down the consumption of energy and reducing environmental pollution.
The utility model adopts following technical scheme to realize:
The equipment of preparing aromatic sulfonic acid by gas-phase sulphonation of aromatic organic compound, comprise rotary packed bed, rotary packed bed liquid-inlet links to each other with the raw material storage tank, and rotary packed bed gas feed links to each other with sulphur trioxide mixing source of the gas, and rotary packed bed liquid exit links to each other with the product storage tank through tubular heat exchange.
Rotary packed bed shell is generally round shape, and shell is provided with the heat-eliminating medium chuck outward.
The raw material storage tank links to each other with rotary packed bed liquid-inlet by interchanger, pump and the liquid meter that is connected successively.
Rotary packed bed pneumatic outlet links to each other with the gas inlet of gas drier with the distribution mixing tank through gas-liquid separation device, and the pneumatic outlet of distribution mixing tank links to each other with rotary packed bed gas feed through gas meter.
The relative prior art of method and apparatus described in the utility model has following beneficial effect:
What (1) the utility model adopted rotary packed bedly has a mass-transfer efficiency efficiently, can make gas-liquid contact mixing fast, increased the gas-to-liquid contact area, strengthened the contact effect, gas-liquid contact time is short, makes gas liquid reaction in this procedure division reaction, thermal discharge is little, temperature of reaction is controlled easily,, can be controlled at temperature well 0～10 ℃ optimum range especially for the sulfonation reaction of some heat-sensitive substances such as toluene.
(2) subsequent reactions is finished in tubular heat exchange, because interchanger is not easy to produce back-mixing, has reduced the generation of side reaction.In the sulfonation reaction of toluene, can effectively cut off the consecutive reaction approach, under the situation that does not add the agent of any resistance sulfone sulfonated products in the growing amount of ditolyl sulfone be controlled at below 1.3%; On the other hand, liberated heat shifts out rapidly easily, easy control of temperature, the carrying out that helps sulfonation reaction, the content that can make tosic acid in the sulfonated products is near 90%, and the content of m-toluene sulfonic acid can be controlled in below 1.0%, thereby improved the selectivity of reaction.
(3) the gas phase recycle system has realized that tail gas does not discharge in this reactor, and sulphur trioxide recycles, and the distribution amount greatly reduces.Avoided contaminate environment, resource is recycled, and has saved the energy.
(4) the utility model adopted rotary packed bedly has advantages such as equipment volume is little, light weight, installation and maintenance are convenient, the start-stop car is convenient.
Description of drawings
Fig. 1 is a structural representation of the present utility model
Among the figure: 1-raw material storage tank; The 2-interchanger; The 3-pump; 4,11,17,20-valve; The 5-liquid meter; The rotary packed bed liquid exit of 6-; 7-heat-eliminating medium chuck; The rotary packed bed liquid-inlet of 8-; 9-is rotary packed bed; The rotary packed bed pneumatic outlet of 10-; The 12-gas-liquid separation device; The outlet of 13-heat-eliminating medium; The 14-motor; The rotary packed bed gas feed of 15-; The 16-gas meter; 18-distribution mixing tank; The 19-gas meter, the 21-gas drier; 22-product storage tank; The 23-tubular heat exchange, the 24-cooling medium inlet.
Embodiment
In conjunction with the accompanying drawings embodiment of the present utility model is described further.
The equipment of preparing aromatic sulfonic acid by gas-phase sulphonation of aromatic organic compound method, comprise rotary packed bed 9, rotary packed bed liquid-inlet 8 links to each other with raw material storage tank 1, rotary packed bed gas feed 15 links to each other with sulphur trioxide mixing source of the gas, and rotary packed bed liquid exit 6 links to each other with product storage tank 22 through tubular heat exchange 23.
Rotary packed bed 9 shell is a round shape, and shell is provided with heat-eliminating medium chuck 7 outward, has cooling medium inlet 24 and heat-eliminating medium outlet 13 on the heat-eliminating medium chuck 7.
Raw material storage tank 1 links to each other with rotary packed bed liquid-inlet 8 by interchanger 2, pump 3 and the liquid meter 5 that is connected successively.The sulfonation of thermo-sensitivity fragrant type organic matter, raw material will be through interchanger 2 processing of lowering the temperature before entering rotary packed bed 9.
Rotary packed bed pneumatic outlet 10 links to each other with the gas inlet of gas drier 21 with distribution mixing tank 18 through gas-liquid separation device 12, and the pneumatic outlet of distribution mixing tank 18 links to each other with rotary packed bed gas feed 10 through gas meter 19.
Utilize the method for the preparing aromatic sulfonic acid by gas-phase sulphonation of aromatic organic compound of the utility model realization, specific embodiment is as follows:
Open rotary packed bed 9, regulate rotating speed at 500r/min～3000r/min, fragrant type organic matter is entered rotary packed bed 9 with certain flow velocity by rotary packed bed liquid-inlet 8 through liquid meter by pump 3, the sulphur trioxide mixed gas of certain volume concentration is fed rotary packed bed 9 from rotary packed bed gas inlet 15 through gas meter 19, it is 0.3～1.05 that the volumetric concentration of regulating the flow velocity of fragrant type organic matter and sulphur trioxide mixed gas makes the mol ratio of sulphur trioxide and fragrant type organic matter: 1 gets final product.Gas phase and liquid phase rapid mixing the in rotary packed bed 9 carried out partial reaction, reacted liquid product enters tubular heat exchange 23 by rotary packed bed liquid exit 6 and lowers the temperature rapidly, in suitable temperature (according to the processing requirement of the fragrant type organic matter that is sulfonated, temperature range in the shell-and-tube reactor is controlled at 0 ℃～60 ℃) under continue to finish reaction, obtain product, enter product storage tank 22, the gaseous product that rotary packed bed internal reaction produces enters gas-liquid separation device 12 through rotary packed bed pneumatic outlet 9, enters distribution mixing tank 18 again after gas drier 21 (in adorn 98.3% vitriol oil) drying treatment and recycles.
Above-mentioned fragrant type organic matter is benzene or toluene or dodecylbenzene.The concentration of sulphur trioxide is 4%～12% (v/v) in the sulphur trioxide gas mixture, and this sulphur trioxide gas mixture is to be got by nitrogen, rare gas element or dry air dilution sulphur trioxide, and rotary packed bed and temperature of reaction tubular heat exchange is 0 ℃～60 ℃
Embodiment 1: the sulfonation of toluene
Adopt device flow process shown in Figure 1 to carry out the sulfonation of toluene.Adjusting rotary packed bed 9 rotating speed is 3000r/min, raw material toluene cools to-5 ℃～0 ℃ through interchanger 2 before entering rotary packed bed 9, the flow that enters the toluene of system is 6kg/h, and the flow of the gas mixture of trioxygen-containing sulphur 6% (v/v) (all the other are dry air) is 7Nm
3/ h, reaction is after liquid exit 6 enters tubular heat exchange 23 to two kinds of raw materials rapidly in rotary packed bed 9, and the cooling holding temperature is at 0 ℃～10 ℃, and reacted product enters product storage tank 22.The mol ratio that described sulphur trioxide and toluene add in this reactive system is 0.3: 1.The content of para-isomeride accounts for 87%-90% in the toluenesulphonic acids that reaction produces, and meta-isomer content is not more than 1.0%.
Embodiment 2: the sulfonation of benzene
Adopt device flow process shown in Figure 1 to carry out the sulfonation of benzene.Adjusting rotary packed bed 9 rotating speed is 500r/min, and the flow that enters the benzene of system is 5kg/h, and the flow of the gas mixture of trioxygen-containing sulphur 8% (v/v) (all the other are dry air) is 9N m
3/ h, reaction is after liquid exit 6 enters external heat exchanger 23 to two kinds of raw materials rapidly in rotary packed bed 9, and the cooling holding temperature is at 20 ℃～60 ℃, and reacted product enters product storage tank 22.The mol ratio that described sulphur trioxide and described benzene add in this reactive system is 0.5: 1.
Embodiment 3: the sulfonation of benzene
Adopt device flow process shown in Figure 1 to carry out the sulfonation of benzene.Adjusting rotary packed bed 9 rotating speed is 1500r/min, and the flow that enters the benzene of system is 5kg/h, and the flow of the gas mixture of trioxygen-containing sulphur 4% (v/v) (all the other are dry air) is 36Nm
3/ h, reaction is after liquid exit 6 enters external heat exchanger 23 to two kinds of raw materials rapidly in rotary packed bed 9, and the cooling holding temperature is at 20 ℃～30 ℃, and reacted product enters product storage tank 22.The mol ratio that described sulphur trioxide and described benzene add in this reactive system is 1: 1.
Embodiment 4: the sulfonation of dodecylbenzene
Adopt device flow process shown in Figure 1 to carry out the sulfonation of dodecylbenzene.Used alkylbenzene is that the rotating speed of industrial alkylbenzene (average molar mass is 240) adjustment rotary packed bed 9 is 1000r/min, the flow that enters the alkylbenzene of system is 6kg/h, and the flow of the gas mixture of trioxygen-containing sulphur 12% (v/v) (all the other are dry air) is 5Nm
3/ h, reaction is after liquid exit 6 enters external heat exchanger 23 to two kinds of raw materials rapidly in rotary packed bed 9, and the cooling holding temperature is at 50 ℃～60 ℃, and reacted product enters product storage tank 22.The mol ratio that described sulphur trioxide and described alkylbenzene add in this reactive system is 1.05: 1.
Embodiment 5: the sulfonation of dodecylbenzene
Adopt device flow process shown in Figure 1 to carry out the sulfonation of dodecylbenzene.Used alkylbenzene is that the rotating speed of industrial alkylbenzene (average molar mass is 240) adjustment rotary packed bed 9 is 2000r/min, the flow that enters the alkylbenzene of system is 6kg/h, and the flow of the gas mixture of trioxygen-containing sulphur 6% (v/v) (all the other are dry air) is 10Nm
3/ h, reaction is after liquid exit 6 enters external heat exchanger 23 to two kinds of raw materials rapidly in rotary packed bed 9, and the cooling holding temperature is at 50 ℃～55 ℃, and reacted product enters product storage tank 22.The mol ratio that described sulphur trioxide and described alkylbenzene add in this reactive system is 1.03: 1.
Claims (4)
1, a kind of equipment of preparing aromatic sulfonic acid by gas-phase sulphonation of aromatic organic compound, it is characterized in that comprising rotary packed bed (9), rotary packed bed liquid-inlet (8) links to each other with raw material storage tank (1), rotary packed bed gas feed (15) links to each other with sulphur trioxide mixing source of the gas, and rotary packed bed liquid exit (6) links to each other with product storage tank (22) through tubular heat exchange (23).
2, the equipment of preparing aromatic sulfonic acid by gas-phase sulphonation of aromatic organic compound as claimed in claim 1, the shell that it is characterized in that rotary packed bed (9) is a round shape, shell is provided with heat-eliminating medium chuck (7) outward.
3, the equipment of preparing aromatic sulfonic acid by gas-phase sulphonation of aromatic organic compound as claimed in claim 1 is characterized in that raw material storage tank (1) links to each other with rotary packed bed liquid-inlet (8) by interchanger (2), pump (3) and the liquid meter (5) that is connected successively.
4, as the equipment of claim 1 or 2 or 3 described preparing aromatic sulfonic acid by gas-phase sulphonation of aromatic organic compound, it is characterized in that rotary packed bed pneumatic outlet (10) links to each other with the gas inlet of gas drier (21) with distribution mixing tank (18) through gas-liquid separation device (12), the pneumatic outlet of distribution mixing tank (18) links to each other with rotary packed bed gas feed (15) through gas meter (19).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009201027542U CN201406388Y (en) | 2009-05-11 | 2009-05-11 | Equipment for preparing aromatic sulfonic acid by utilizing gas-phase sulfonation of aromatic organic matters |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009201027542U CN201406388Y (en) | 2009-05-11 | 2009-05-11 | Equipment for preparing aromatic sulfonic acid by utilizing gas-phase sulfonation of aromatic organic matters |
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| CN201406388Y true CN201406388Y (en) | 2010-02-17 |
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| CN2009201027542U Expired - Fee Related CN201406388Y (en) | 2009-05-11 | 2009-05-11 | Equipment for preparing aromatic sulfonic acid by utilizing gas-phase sulfonation of aromatic organic matters |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437336A (en) * | 2014-11-22 | 2015-03-25 | 中北大学 | Sulfonation equipment and method for preparing p-toluenesulfonic acid by using gaseous sulfur trioxide sulfonated toluene |
| CN106606991A (en) * | 2015-10-27 | 2017-05-03 | 北京化工大学 | System device for preparing sulphonate surfactant through supergravity sulfonating method and application |
| CN108355587A (en) * | 2018-03-09 | 2018-08-03 | 中建安装工程有限公司 | A kind of modularization is rotary packed bed |
| CN113045370A (en) * | 2019-12-27 | 2021-06-29 | 辽宁奥克化学股份有限公司 | Sulfonation method |
-
2009
- 2009-05-11 CN CN2009201027542U patent/CN201406388Y/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437336A (en) * | 2014-11-22 | 2015-03-25 | 中北大学 | Sulfonation equipment and method for preparing p-toluenesulfonic acid by using gaseous sulfur trioxide sulfonated toluene |
| CN106606991A (en) * | 2015-10-27 | 2017-05-03 | 北京化工大学 | System device for preparing sulphonate surfactant through supergravity sulfonating method and application |
| CN108355587A (en) * | 2018-03-09 | 2018-08-03 | 中建安装工程有限公司 | A kind of modularization is rotary packed bed |
| CN108355587B (en) * | 2018-03-09 | 2023-08-29 | 中建安装集团有限公司 | Modularized rotary packed bed |
| CN113045370A (en) * | 2019-12-27 | 2021-06-29 | 辽宁奥克化学股份有限公司 | Sulfonation method |
| CN113045370B (en) * | 2019-12-27 | 2023-07-18 | 辽宁奥克化学股份有限公司 | Sulfonation method |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100217 Termination date: 20130511 |