CN211946873U - Apparatus for producing of high-purity dodecylbenzene sulfonic acid - Google Patents
Apparatus for producing of high-purity dodecylbenzene sulfonic acid Download PDFInfo
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- CN211946873U CN211946873U CN201922393321.3U CN201922393321U CN211946873U CN 211946873 U CN211946873 U CN 211946873U CN 201922393321 U CN201922393321 U CN 201922393321U CN 211946873 U CN211946873 U CN 211946873U
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Abstract
The utility model belongs to the technical field of fine chemistry industry. Aims to provide a production device of high-quality dodecylbenzene sulfonic acid with light color and low sulfuric acid content. The technical scheme is as follows: the production device of high-purity dodecyl benzene sulfonic acid is characterized by comprising a Venturi tube, a sulfur furnace and SO which are communicated in sequence through pipelines2Conversion column, SO3The device comprises a cooler, a sulfonator, a gas-liquid separator, an acid ester delivery pump, a vacuum aging device, a vacuum pump, a hydrolysis delivery pump and a hydrolyzer; the sulfonationThe device is provided with a dodecylbenzene inlet; the gas-liquid separator is provided with a tail gas outlet for outputting tail gas; the outlet of the hydrolyzer is a product outlet; the inlet end of the Venturi tube is communicated with a dry air inlet, the suction end of the Venturi tube is communicated with the exhaust end of the vacuum pump, and the outlet section of the Venturi tube is communicated with a gas phase inlet of the sulfur burning furnace; the vacuum aging device is a conventional overflow column, and the bottom of the vacuum aging device is provided with a material inlet communicated with an outlet of an acid ester conveying pump.
Description
Technical Field
The utility model belongs to the technical field of fine chemical industry, concretely relates to apparatus for producing of high-purity dodecylbenzene sulfonic acid.
Background
Dodecyl benzene sulfonic acid has the performances of decontamination, wetting, foaming, emulsification, dispersion and the like, and the biodegradation degree is more than 90 percent, so that the dodecyl benzene sulfonic acid is the most important anionic surfactant; the product can be used for producing various detergents and emulsifiers, such as washing powder, tableware detergent, light and heavy dirt detergent in daily chemical industry, cleaning agent in textile industry, dyeing auxiliary agent, degreasing agent in electroplating and tanning industry, deinking agent in paper industry, etc.
Dodecylbenzene sulfonic acid is an anionic surfactant product obtained by sulfonating linear dodecylbenzene. Most of the prior sulfonation processes adopt gas-phase SO3The membrane sulfonation method mainly comprises burning sulfur to obtain SO with a gas concentration of about 2-6%3Gas, then sulfonation, aging and hydrolysis are carried out on the gas and the straight-chain dodecyl benzene.
Because of the limitation of production technology, the alkylbenzene sulfonic acid products produced industrially at present contain a certain amount of free sulfuric acid and unreacted raw material alkylbenzene besides alkylbenzene sulfonic acid as a main component, and the product quality is influenced to a certain extent. Especially free sulfuric acid, which is highly corrosive; has adverse effects on the color, stability and the like of the alkylbenzene sulfonic acid in the storage process; benzene ring on alkylbenzene sulfonic acid can be oxidized by sulfuric acid, the oxidation product is usually a black quinoid compound, and after the alkyl chain on the benzene ring is oxidized, a black product which is difficult to bleach is easily generated; fourthly, the free sulfuric acid also can cause the alkyl benzene sulfonic acid to have dealkylation and desulfation reactions, so that the smell of the product is easily deteriorated and the color is deepened in the storage process.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defects in the prior art and provide a production device of high-quality dodecylbenzene sulfonic acid with light color and low sulfuric acid content.
The utility model provides a technical scheme is:
the production device of high-purity dodecyl benzene sulfonic acid is characterized by comprising a Venturi tube, a sulfur furnace and SO which are communicated in sequence through pipelines2Conversion column, SO3The device comprises a cooler, a sulfonator, a gas-liquid separator, an acid ester delivery pump, a vacuum aging device, a vacuum pump, a hydrolysis delivery pump and a hydrolyzer;
the sulfonator is provided with a dodecylbenzene inlet; the gas-liquid separator is provided with a tail gas outlet for outputting tail gas; the outlet of the hydrolyzer is a product outlet;
the inlet end of the Venturi tube is communicated with a dry air inlet, the suction end of the Venturi tube is communicated with the exhaust end of the vacuum pump, and the outlet section of the Venturi tube is communicated with a gas phase inlet of the sulfur burning furnace;
the vacuum aging device is a conventional overflow column, the bottom of the vacuum aging device is provided with a material inlet which is communicated with an outlet of the acid ester conveying pump, an air outlet at the top of the vacuum aging device is communicated with an air exhaust end of the vacuum pump, and a material outlet at the upper part of the side edge of the vacuum aging device is communicated with an inlet of the hydrolysis conveying pump.
The hydrolyzer is provided with two inlets, one inlet is communicated with the outlet of the hydrolysis transfer pump, and the other inlet is a process water inlet.
The hydrolyzer is a static mixer, or a centrifugal pump, or a homogenizing reactor with high shear.
The vacuum pump is a roots vacuum pump or a screw vacuum pump.
The utility model has the advantages that:
1) the sulfonic acid produced by the process of the utility model can obviously reduce the residual free sulfuric acid and the residual unreacted alkylbenzene in the product. The main reason is that under the aging process condition provided by the utility model, the reaction speed of converting the pyrosulfonic acid and the sulfonic anhydride into the sulfonic acid is obviously improved, and the reaction of the free sulfuric acid, the unreacted alkylbenzene and the sulfonic anhydride in the acid ester is more thorough; simultaneously, residual SO in the acid ester is removed under vacuum condition3Can also be removed effectively. The free alkylbenzene in the sulfonic acid product obtained by the utility model can be reduced to below 0.5 percent from about 1.5 percent of the prior art; free sulfuric acid can also be reduced from 1.5% to below 0.5% of conventional processes.
2) The utility model discloses under the process condition, the promotion of ageing reaction rate makes ageing time obviously shorten. Reduction of aging time, free sulfuric acid in acid ester, free SO3The reduction of content can effectively reduce the emergence of side reaction, improves the product color and luster, utilizes the utility model discloses the sulfonic acid color and luster of technology production can be reduced to within 10Hazen from the 30 ~ 40Hazen of conventional technology.
3) The reduction of the content of free sulfuric acid in the sulfonic acid produced by the process of the utility model can obviously improve the storage stability of the product. Experiments show that the color of the sulfonic acid produced by the process of the utility model is improved within 10Hazen after being stored for 30 days at 50 ℃, and the data of the conventional process reaches more than 30 Hazen.
4) The utility model discloses sneak into dry gas with the tail gas after the ageing desorption of vacuum, get into the burning of sulfur burner, utilize the burning of sulfur burner high temperature thoroughly to burn, avoided the difficult problem of processing of vacuum desorption tail gas, can be with the SO of desorption simultaneously3And returning to the system again to reduce waste. Compared with the conventional process, the utility model discloses the sulfur consumption of ton product can be reduced about 3 &intechnical scheme5kg。
Drawings
Fig. 1 is a schematic diagram of a system structure of a dodecylbenzene sulfonic acid production device provided by the present invention.
In the figure: 1 is a dry air inlet, 2 is a liquid sulfur inlet, 3 is a dodecyl benzene inlet, 4 is a venturi tube, 5 is a sulfur furnace, 6 is a conversion tower, 7 is a cooler, 8 is a sulfonator, 9 is a gas-liquid separator, 10 is an acid ester delivery pump, 11 is a vacuum aging device, 12 is a vacuum pump, 13 is a hydrolysis delivery pump, 14 is a hydrolyzer, 15 is a process water inlet, 16 is a product outlet, and 17 is a tail gas outlet.
Detailed Description
The following further description is made with reference to the embodiments shown in the drawings.
The production device of dodecyl benzene sulfonate shown in the attached figure comprises a Venturi tube 4, a sulfur burning furnace 5 and SO which are communicated with each other in sequence by pipelines2Conversion tower 6, SO3A cooler 7, a sulfonator 8, a gas-liquid separator 9, an acid ester conveying 10 pump, a vacuum aging device 11, a vacuum pump 12, a hydrolysis conveying pump 13 and a hydrolyzer 14;
the sulfonator is provided with a dodecylbenzene inlet; the gas-liquid separator is provided with a tail gas outlet for outputting tail gas; the outlet of the hydrolyzer is a product outlet;
the inlet end of the Venturi tube is communicated with a dry air inlet, the suction end of the Venturi tube is communicated with the exhaust end of the vacuum pump, and the outlet section of the Venturi tube is communicated with a gas phase inlet of the sulfur burning furnace;
the vacuum aging device is a conventional overflow column, the bottom of the vacuum aging device is provided with a material inlet which is communicated with an outlet of the acid ester conveying pump, an air outlet at the top of the vacuum aging device is communicated with an air exhaust end of the vacuum pump, and a material outlet at the upper part of the side edge of the vacuum aging device is communicated with an inlet of the hydrolysis conveying pump.
The hydrolyzer is provided with two inlets, one inlet is communicated with the outlet of the hydrolysis transfer pump, and the other inlet is a process water inlet. The hydrolyzer is a static mixer, or a centrifugal pump, or a homogenizing reactor with high shear.
The vacuum pump is a roots vacuum pump or a screw vacuum pump.
Example 1:
4500m3about/h of dry air is mixed with the desorption gas input by the vacuum aging device in the Venturi tube and then enters the sulfur burning furnace; simultaneously, liquid sulfur enters a sulfur burning furnace according to the flow of 400kg/h, and is contacted and burned in the sulfur burning furnace to generate SO with the temperature of about 600 DEG C2A gas; the high-temperature gas is converted in a conversion tower and cooled in a cooler according to the conventional process to obtain SO with the volume concentration of 5.5 percent and the temperature of 60 DEG C3The gas enters a falling film type sulfonation reactor; simultaneously, the dodecylbenzene enters the sulfonator at the flow rate of 2800kg/h and is mixed with SO3The gas contacts to carry out sulfonation reaction.
And (3) separating the sulfonated product by a gas-liquid separator, outputting the gas phase, removing a tail gas treatment system for treatment so as to achieve the standard and discharge, and conveying the liquid-phase acid ester from the bottom by a pump to enter a vacuum ageing device for ageing. The vacuum aging device has an effective volume of 1.5m3The aging temperature of the overflow column is controlled to be 50 ℃, and the aging vacuum degree is controlled to be-80 kPa. The vacuum pump for realizing vacuum is a screw vacuum pump, and the gas removed in vacuum is mixed into dry air by using a Venturi tube and enters a sulfur furnace to completely burn organic matters in the dry air.
And after overflowing from the aging device, the aged dodecyl benzene sulfonate is conveyed into a static mixer by using a hydrolysis conveying pump, meanwhile, the process water enters the static mixer at the same time according to the flow of 15kg/h and is hydrolyzed with the dodecyl benzene sulfonate, and the finished product of dodecyl benzene sulfonic acid is obtained after hydrolysis.
The comparative indices of the final product are as follows:
example 2:
5500m3about/h dry air is mixed with the desorption gas input by the vacuum aging device in the Venturi tube and then enters the sulfur burning deviceA furnace; simultaneously, liquid sulfur enters a sulfur burning furnace according to the flow of 400kg/h, and is combusted in the sulfur burning furnace in a contact way to generate SO with the temperature of about 500 DEG C2A gas; the high-temperature gas is converted by a conversion tower and cooled by a cooler in sequence according to the conventional process to obtain SO with the volume concentration of 3.5 percent and the temperature of 55 DEG C3The gas enters a falling film sulfonation reactor; simultaneously, the dodecylbenzene enters the sulfonator at the flow rate of 2850kg/h and is mixed with SO3The gas contacts to carry out sulfonation reaction.
And (3) separating the sulfonated product by a gas-liquid separator, outputting the gas phase, removing a tail gas treatment system for treatment so as to achieve the standard and discharge, and conveying the liquid-phase acid ester from the bottom by a pump to enter a vacuum ageing device for ageing. The vacuum aging device has an effective volume of 1.5m3The aging temperature of the overflow column is controlled to be 47 ℃, and the aging vacuum degree is controlled to be-85 kPa. The vacuum pump for realizing vacuum adopts a screw vacuum pump, and the gas removed in vacuum is mixed into dry air by using a Venturi tube and enters a sulfur furnace to completely burn organic matters in the dry air.
And after the aged dodecyl benzene sulfonate overflows from the aging device, conveying the aged dodecyl benzene sulfonate into a static mixer by using a hydrolysis conveying pump, simultaneously conveying process water into the static mixer at the same time according to the flow of 15kg/h to hydrolyze with the dodecyl benzene sulfonate, and obtaining a finished product of dodecyl benzene sulfonic acid after hydrolysis.
The comparative indices of the final product are as follows:
example 3:
4000m3about/h of dry air is mixed with the desorption gas input by the vacuum aging device in the Venturi tube and then enters the sulfur burning furnace; simultaneously, liquid sulfur enters a sulfur burning furnace according to the flow of 400kg/h, and is contacted and burned in the sulfur burning furnace to generate SO with the temperature of about 680 DEG C2Gas, this part of high temperature gas as usualThe SO with the volume concentration of 6 percent and the temperature of 65 ℃ is obtained by the conventional process through the conversion of a conversion tower and the cooling of a cooler in sequence3The gas enters a falling film sulfonation reactor; simultaneously, dodecylbenzene enters the sulfonator at the flow rate of 2750kg/h and is mixed with SO3The gas contacts to carry out sulfonation reaction.
And (3) separating the sulfonated product by a gas-liquid separator, outputting the gas phase, removing a tail gas treatment system for treatment so as to achieve the standard and discharge, and conveying the liquid-phase acid ester from the bottom by a pump to enter a vacuum ageing device for ageing. The vacuum aging device has an effective volume of 1.5m3The aging temperature of the overflow column is controlled to be 53 ℃, and the aging vacuum degree is controlled to be-75 kPa. The vacuum pump for realizing vacuum adopts a screw vacuum pump, and the gas removed in vacuum is mixed into dry air by using a Venturi tube and enters a sulfur furnace to completely burn organic matters in the dry air.
And after the aged dodecyl benzene sulfonate overflows from the aging device, conveying the aged dodecyl benzene sulfonate into a static mixer by using a hydrolysis conveying pump, simultaneously conveying process water into the static mixer at the same time according to the flow of 15kg/h to hydrolyze with the dodecyl benzene sulfonate, and obtaining a finished product of dodecyl benzene sulfonic acid after hydrolysis.
The comparative indices of the final product are as follows:
Claims (4)
1. the production device of the high-purity dodecyl benzene sulfonic acid is characterized by comprising a Venturi tube (4), a sulfur furnace (5) and an SO pipe which are communicated in sequence through pipelines2Conversion tower (6), SO3A cooler (7), a sulfonator (8), a gas-liquid separator (9), an acid ester delivery pump (10), a vacuum aging device (11), a vacuum pump (12), a hydrolysis delivery pump (13) and a hydrolyzer (14);
the sulphonator is provided with a dodecylbenzene inlet (3); the gas-liquid separator is provided with a tail gas outlet (17) for outputting tail gas; the outlet (16) of the hydrolyzer is a product outlet;
the inlet end of the Venturi tube is communicated with a dry air inlet (1), the suction end of the Venturi tube is communicated with the exhaust end of the vacuum pump, and the outlet section of the Venturi tube is communicated with a gas phase inlet of the sulfur burning furnace;
the vacuum aging device is a conventional overflow column, the bottom of the vacuum aging device is provided with a material inlet which is communicated with an outlet of the acid ester conveying pump, an air outlet at the top of the vacuum aging device is communicated with an air exhaust end of the vacuum pump, and a material outlet at the upper part of the side edge of the vacuum aging device is communicated with an inlet of the hydrolysis conveying pump.
2. The apparatus for producing highly pure dodecylbenzene sulfonic acid according to claim 1, wherein: the hydrolyzer is provided with two inlets, one inlet is communicated with the outlet of the hydrolysis transfer pump, and the other inlet is a process water inlet.
3. The apparatus for producing highly pure dodecylbenzene sulfonic acid according to claim 2, wherein: the hydrolyzer is a static mixer, or a centrifugal pump, or a homogenizing reactor with high shear.
4. The apparatus for producing highly pure dodecylbenzene sulfonic acid according to claim 3, wherein: the vacuum pump is a roots vacuum pump or a screw vacuum pump.
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