CN112795004B - Production process and production system of fatty alcohol polyoxyethylene ether sodium sulfate - Google Patents
Production process and production system of fatty alcohol polyoxyethylene ether sodium sulfate Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/321—Polymers modified by chemical after-treatment with inorganic compounds
- C08G65/326—Polymers modified by chemical after-treatment with inorganic compounds containing sulfur
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Abstract
The invention belongs to the technical field of fine chemical industry, and aims to provide a production process of fatty alcohol polyoxyethylene ether sodium sulfate, wherein a sulfonating agent SO is used in the process 3 The gas is burnt by liquid sulfur and compressed and cooled process air to obtain SO 2 Air mixture, which is oxidized in a conversion tower by catalyst to form SO 3 And (3) cooling the air mixed gas, atomizing and deacidifying the air mixed gas at the outlet of the conversion tower by an atomizing tank, filtering the air mixed gas by a demister, and directly using the air mixed gas in sulphonating fatty alcohol polyoxyethylene ether to obtain the fatty alcohol polyoxyethylene ether sodium sulfate meeting the requirements. Compared with the currently reported process, the process technology has low dew point requirement on process air, simplified production equipment, shortened process flow and low process energy consumption, and therefore, the process technology has wide application prospect in actual production.
Description
Technical Field
The invention belongs to the technical field of fine chemical industry, relates to a production process of fatty alcohol polyoxyethylene ether sodium sulfate, in particular to a method for preparing sodium sulfateSO with proper gas concentration obtained by optimizing sulfur burning method 3 Air mixed gas is used for the production process and production system of sulfonated fatty alcohol polyoxyethylene ether.
Background
Sulfonation/sulfation reactions (collectively referred to as sulfonation reactions) are widely studied both at home and abroad as the main chemical methods employed in the industrial production of pigments, dyes, pesticides, organic intermediates, and the like. By using different sulphonating agents to carry out the reaction (-SO) 3 ) The group is introduced into the organic molecule to make the organic molecule have (-CS (O) 2 ) OX) structure, various products are obtained, including sulfonic acid (x=h), sulfate (x=m, M is a metal cation), sulfonyl halide (X is halogen), etc., and various surface activities such as emulsification, foaming, wetting, etc. are provided for organic molecules; at the same time utilize (-CS (O) 2 ) OX) group, giving the organic molecules better water solubility; selective sulfonation is used in the field of pharmaceutical production to separate isomers, giving a series of intermediate products. However, the most industrially used sulfonation reaction is also in the field of anionic surfactants for producing sulfonation products, among which mainly alkylbenzenesulfonic acid, fatty alcohol polyoxyethylene ether sulfate and the like, the former is widely used for preparing detergents, the latter is widely used in shampoos, body washes and dish detergents, and data show that more than 200 ten thousand tons of sulfonation products are used for household washing products to be sold worldwide in 2015 only, which occupies a very high proportion in the whole surfactant product. The sulfonating agents adopted in the industrial sulfonation process are various, and the common sulfonating agents are SO 3 Sulfuric acid, fuming sulfuric acid, sulfite, chlorosulfonic acid and the like with different concentrations, different sulfonating agents have different performances, different occasions and different SO (sulfur dioxide) 3 Sulfonation is widely popularized and used due to advanced technology and high quality of sulfonated products.
SO 3 Is the most direct sulfonating agent theoretically used for sulfonating organic raw materials, and the use proportion of reactant raw materials is closer to a theoretical value. SO (SO) 3 Divided into liquid SO 3 And gas SO 3 Liquid SO 3 The sulfonation reaction is intense, only applicable to partial inactive aromatic compounds, and the product is sticky at the reaction temperatureHas strict requirements on the degree, and the liquid SO 3 The temperature requirement is high in the storage process, and the solidification of liquid caused by low temperature must be avoided; the reaction process is intense, SO in the actual control process 3 The dosage is difficult to control accurately, so that the whole process is complex, and only a few enterprises use the dosage in China. Gas SO 3 The method does not generate waste acid in the use process, does not corrode equipment and pollute the environment, and is usually diluted by gas or solution for controlling the reaction rate and then used, so that the violent and difficult control of the reaction process is avoided. Due to SO 3 The self-polymerization trend exists, and the self-polymerization trend is gradually changed into a high-melting-point crystal form under the influence of temperature, SO that under the premise of considering the use cost, SO with certain gas concentration is obtained by burning sulfur, converting and diluting with dry air 3 The sulfur burning method sulfonation generation process of the air mixed gas becomes the first choice of enterprises.
On the production device of the sulfonation process, the method comprises the steps of SO from companies such as Ballestra, chemithen, messaniche, moderne and Lion 3 The air generation process is very little different, and the general flow is as follows: cooling and drying the compressed air to obtain dry air with dew point below-60 ℃, putting the dry air into a sulfur burning furnace to contact with liquid sulfur, igniting and burning to obtain SO carrying a large amount of heat 2 Mixing the gases; then the mixed gas enters a conversion tower after being cooled to 450 ℃, and is continuously oxidized into SO under the action of a catalyst 3 ，SO 3 And cooling the air to 45-55 ℃ by a multistage cooler, filtering a small amount of acid mist by a demister, and then entering a sulfonator to participate in the reaction. Dried SO 3 Air is extremely important for obtaining a high quality and high yield of sulphonated product, moisture in the air can lead to the formation of sulphuric acid and fuming sulphuric acid which can cause corrosion to equipment, and further, entering the sulphonator can cause darkening of the product and side reactions which can produce unintended by-products which affect product quality, thus ensuring that the process air is dried to a dew point of between-60 ℃ and-70 ℃. The drying of the process air is carried out in a drying tower filled with regenerated filler (silica gel and activated alumina), the drying tower is divided into an upper layer and a lower layer which are alternately used, and the filler is used again after being dehydrated and cooled after absorbing the moisture, so that two layers of drying layers are used one by one and one layer of regeneration is carried outThe preparation causes the complexity of the whole process, and the dew point fluctuation of the dry air can have a great influence on the quality of subsequent products, which is unfavorable for continuous production.
SO due to combustion of sulfur 3 The air mixed gas generating process has strict requirement on the dew point of dry air, long process flow, complex operation and more influencing factors on the quality of products, mainly the moisture in the process air has larger influence on the quality of sulfonated products, and the cooling air is directly used for SO at present 3 The sulfonation process with air has not been reported.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a production process of fatty alcohol polyoxyethylene ether sodium sulfate; the process can be used for sulfonation of the fatty alcohol polyoxyethylene ether after cooling air and liquid sulfur are combusted, converted by a conversion tower, cooled and atomized and sprayed, and filtered by a demister without drying process air with low dew point, and the quality of the obtained product is the same as that of the product produced under the existing process conditions; the process has simple control conditions, and can be conveniently realized by modifying the existing production device.
The invention also provides a production system used by the production process.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a production process of fatty alcohol polyoxyethylene ether sodium sulfate, which comprises the following steps:
1) The external air enters a Roots blower for heating and pressurizing after being subjected to impurity removal by an air filter, then is conveyed into an air low-temperature condenser, most of water vapor in the air is removed through cooling treatment of two cooling mediums, and the obtained cooling air enters a sulfur burning furnace from a gas phase inlet of the sulfur burning furnace; simultaneously, liquid sulfur enters the sulfur burning furnace from a liquid phase inlet of the sulfur burning furnace through a liquid sulfur conveying pump, contacts with cooling air in countercurrent, ignites and burns to generate SO 2 A gas;
2) Diluted SO 2 The gas enters a conversion tower to be catalyzed to obtain SO 3 Mixing the gas with cooling air for dilution, and diluting SO 3 The air mixture is cooled by a primary air cooler and then enters an atomization tank, and fuming sulfuric acid or liquid SO is sprayed through atomization 3 SO removal 3 Sulfuric acid liquid drops separated out from the air mixed gas;
3) SO after sulfuric acid liquid drop removal 3 The air is further cooled by a secondary air cooler, a small amount of acid mist is removed by a demister, and then enters a sulfonator to carry out sulfonation reaction with fatty alcohol polyoxyethylene ether;
4) And removing gas from the reacted sulfate through a cyclone separator, then conveying the process water and the liquid alkali to a neutralization mixer through a neutralization mixing pump, and obtaining the product fatty alcohol polyoxyethylene ether sodium sulfate after neutralization.
As a preferable scheme of the invention, the temperature of the cooling gas at the outlet of the air cryocondenser in the step 1) is 4-8 ℃.
As a preferable scheme of the invention, the molar ratio of the flow of the liquid sulfur to the flow of the fatty alcohol-polyoxyethylene ether entering the sulfonator is 1.02-1.12:1.
As a preferred embodiment of the invention, the SO at the outlet of the sulfur burner in the step 1) is 2 The gas temperature is 450-700 ℃.
As a preferred embodiment of the present invention, the step 2) is a step of converting the output SO of the column 3 The temperature of the air mixture is 440-470 ℃.
As a preferred embodiment of the present invention, the SO in step 2) is 3 The cooling temperature of the air mixed gas is 270 ℃ after passing through a primary air cooler, and fuming sulfuric acid or liquid SO is atomized and sprayed 3 The flow rate of the jet liquid drops is 0.1-0.5 per mill of the inlet gas flow rate, and the particle size of the jet liquid drops is controlled to be 20-80 mu m.
As a preferred embodiment of the present invention, the SO in step 3) is 3 The cooling temperature of the air mixture after passing through the secondary air cooler is 45-60deg.C, and SO is obtained at this time 3 The gas volume concentration is 3-6%.
As a preferable scheme of the invention, the process water flow in the step 4) is 15-20% of the acid ester flow, and the 32% liquid alkali flow is 35-40% of the acid ester flow.
The invention also provides a production system of the fatty alcohol polyoxyethylene ether sodium sulfate, and all devices are connected by pipelines in sequence, wherein the production system comprises an air filter, a Roots blower, an air low-temperature condenser, a sulfur burner, a conversion tower, a primary air cooler, an atomizing tank, a secondary air cooler, a demister, a sulfonator, a gas-liquid separator, a neutralization mixing pump and a neutralization mixer.
The sulfur burning furnace is provided with a liquid sulfur inlet; the primary air cooler is provided with a nicotinic acid outlet; the atomization tank is provided with a nicotinic acid outlet; the secondary air cooler is provided with a nicotinic acid outlet; the demister is provided with a nicotinic acid outlet; the sulfonator is provided with an inlet of fatty alcohol polyoxyethylene ether; the gas-liquid separator is provided with an acid gas outlet; the neutralizing mixer has a gas outlet.
As a preferable scheme of the invention, two cooling medium flow pipelines are arranged in the air low-temperature condenser, circulating cooling water and a frozen glycol water solution pipeline, and compressed air sequentially passes through the two cooling medium heat exchange pipelines in the condenser; the atomization tank is provided with an atomization nicotinic acid injection port, and the atomization tank has a larger volume to ensure enough gas residence time, and receives SO from the primary air cooler 3 Air mixture, the top of which is communicated with a secondary air cooler.
Compared with the prior art, the process technology related by the invention has the following advantages:
1) The process provided by the invention has the advantages that after cooling air with the temperature of 4-8 ℃ is obtained through the air low-temperature condenser, a silica gel drying tower is not needed to further dry and remove water, and the dew point requirement on the used process air is low. This is because the sulfur combustion method gas SO provided by the invention 3 In the air generation process, the cooling air and the liquid sulfur are directly used for combustion and conversion to obtain SO 3 After the air is mixed, the temperature of the mixed gas is reduced by a primary air cooler, the temperature is controlled above the boiling point of sulfuric acid, at the moment, the relative humidity of the gas is greatly changed due to the temperature reduction, and the residual moisture is gradually separated out and SO is carried out 3 Forming sulfuric acid droplets by action, i.e. oleumThe method comprises the steps of carrying out a first treatment on the surface of the Spraying fuming sulfuric acid or liquid SO in an atomization tank through atomization 3 The particle size of the separated sulfuric acid droplets is changed by controlling the spraying flow, so that the separated sulfuric acid droplets are polymerized with each other, the particle size is rapidly enlarged, the separated sulfuric acid droplets are gradually separated from the gas under the action of gravity sedimentation, the separated sulfuric acid droplets are settled and fall in an atomization tank, and the light component gas is continuously discharged from the top of the tank, so that the influence of residual moisture in the process air on sulfonated products is avoided;
2) The invention does not need a silica gel tower drying link in the gas generation process flow, greatly reduces the use equipment cost and energy consumption, and can shorten the start-up and stop time;
3) The invention has the advantages of short process flow, simple control and SO (sulfur dioxide) obtaining 3 The quality of the product fatty alcohol-polyoxyethylene ether sulfuric acid obtained by using the air mixed gas to sulfonate the fatty alcohol-polyoxyethylene ether is the same as that of the product obtained by using the original process, and the product qualification standard is reached.
Drawings
Fig. 1 is a schematic diagram of a production system according to the present invention.
In the figure, 1 is an air filter, 2 is a Roots blower, 3 is an air low-temperature condenser, 4 is a sulfur burner liquid sulfur inlet, 5 is a sulfur burner, 6 is a conversion tower, 7 is a primary air cooler, 8 is an atomization tank, 9 is a secondary air cooler, 10 is a demister, 11 is a sulfonator, 12 is an air low-temperature condenser cooling water pipeline, 13 is a frozen glycol water solution pipeline in the air low-temperature condenser, 14 is a primary air cooler nicotinic acid outlet, 15 is an atomization tank nicotinic acid outlet, 16 is a secondary air cooler nicotinic acid outlet, 17 is a demister nicotinic acid outlet, 18 is an atomization tank atomization fuming sulfuric acid injection port, 19 is a sulfonator fatty alcohol polyoxyethylene ether inlet, 20 is a gas-liquid separator, 21 is a neutralization mixing pump, 22 is a neutralization mixer, and 23 is a gas-liquid separator acid gas outlet; 24 is a neutralizer mixer gas vent; 25 is the product outlet.
Detailed Description
The present invention will be described in detail with reference to the following examples, which are given as detailed embodiments and specific operation procedures based on the technical scheme of the present invention, but the scope of the present invention is not limited to the following examples.
Referring to fig. 1, the invention provides a production system of sodium fatty alcohol polyoxyethylene ether sulfate, all devices are connected by pipelines in sequence, and the production system comprises an air filter 1, a Roots blower 2, an air low-temperature condenser 3, a sulfur burning furnace 5, a conversion tower 6, a primary air cooler 7, an atomization tank 8, a secondary air cooler 9, a demister 10, a sulfonator 11, a gas-liquid separator 20, a neutralization mixing pump 21 and a neutralization mixer 22.
The sulfur burning furnace 5 is provided with a liquid sulfur inlet 4; the primary air cooler 7 is provided with a nicotinic acid outlet 14; the atomization tank 8 is provided with a nicotinic acid outlet 15; the secondary air cooler 9 is provided with a nicotinic acid outlet 16; the demister 10 is provided with a nicotinic acid outlet 17; the sulfonator 11 is provided with a fatty alcohol polyoxyethylene ether inlet 19; the gas-liquid separator 20 has an acid gas discharge port 23; the neutralizing mixer 22 has a gas outlet 24.
Two cooling medium flow pipelines are arranged in the air low-temperature condenser 3, a circulating cooling water pipeline 12 and a frozen glycol water solution pipeline 13, and compressed air sequentially passes through the two cooling medium flow pipelines for heat exchange in the air low-temperature condenser 3;
the atomization tank 8 is provided with an atomized nicotinic acid injection port 18, the atomization tank 8 has a larger volume to ensure enough gas residence time, and the atomization tank 8 receives SO from the primary air cooler 7 3 Air mixture, the top of which is connected to the secondary air cooler 9.
Example 1
The embodiment provides a production process of fatty alcohol polyoxyethylene ether sodium sulfate, the flow is 4580m 3 The external air of/h enters the Roots blower for compression after impurity removal through the filter, the pressure at the outlet of the blower is increased to about 56KPa, and then the air enters the low-temperature air condenser; the hot air in the low-temperature air condenser is sequentially cooled by two cooling mediums, namely cooling water and ethylene glycol solution with the temperature of 0+/-4 ℃, and the hot air is cooled by the two cooling mediums to obtain cooling air with the temperature of 8 ℃; the cooling air directly enters the sulfur burning furnace and is conveyed by a liquid sulfur conveying pump with the flow rate of 240kg/hBurning liquid sulfur in a sulfur burning furnace to form SO 2 Air mixed gas, sulfur burning furnace outlet temperature is 600 ℃; SO (SO) 2 The air mixture is cooled to about 450 ℃ by an air cooler at the upper part of the conversion tower, and then is loaded with V in the conversion tower 2 O 5 Catalytic bed of (2) SO 2 Catalytic conversion to SO 3 Finally SO with the temperature of 480 ℃ is obtained at the outlet of the conversion tower 3 Air-mixed gas; SO (SO) 3 The air mixture enters a primary air cooler to be cooled to 270 ℃ and then enters an atomization tank, the upper part of the atomization tank is atomized and sprayed with 60 percent fuming sulfuric acid (liquid SO for another production line) 3 Control) by adjusting the flow rate of the sprayed fuming sulfuric acid to 200L/h, controlling the particle size of the atomized fuming sulfuric acid to be about 60 mu m, and at this time SO 3 The fuming sulfuric acid is separated out from the air mixed gas, and combined with the fuming sulfuric acid sprayed by atomization, the particle size is increased, and the fuming sulfuric acid is settled to the bottom of the tank under the action of gravity SO 3 Air flows out from the top of the atomization tank; SO passing through atomization tank 3 The air mixture enters a secondary air cooler to be cooled to 55 ℃, and the SO is generated at the moment 3 The gas volume concentration is 5.5%, and simultaneously the flow rate of the fatty alcohol-polyoxyethylene ether is adjusted to 1745kg/h, and the gas volume concentration is equal to SO 3 The air mixture enters a sulfonator together for reaction. By burning sulfur-method gas SO 3 The mixed gas obtained by the air generation process enters a distributor from the top of a sulphonater and reacts with the fatty alcohol-polyoxyethylene ether conveyed by an organic material pump in the sulphonater, the reaction heat release amount is large, the reaction heat is removed in time by using circulating water, the temperature of the circulating cooling water of the sulphonater is controlled to be about 32 ℃, and sulfuric acid ester is obtained at the bottom of the sulphonater; the sulfuric acid ester is separated from acid gas by a gas-liquid separator and a cyclone separator, the gas goes to a tail gas absorption section, the liquid acid ester is conveyed to a neutralization mixer together with 32% liquid alkali (920 kg/h) and process water (450 kg/h) by a neutralization mixing pump, and the product fatty alcohol polyoxyethylene ether sodium sulfate is obtained after neutralization.
Comparative example: the only difference is that no sample is atomized without going through the atomizing tank as in example 1.
The product detection data obtained are shown in Table 1:
TABLE 1 detection data
Example 2
The embodiment provides a production process of fatty alcohol polyoxyethylene ether sodium sulfate, the flow is 4200m 3 The external air of/h enters the Roots blower for compression after impurity removal through the filter, the pressure at the outlet of the blower is increased to about 55KPa, and then the air enters the low-temperature air condenser; the hot air in the low-temperature air condenser is sequentially cooled by two cooling mediums, namely cooling water and ethylene glycol solution with the temperature of 0+/-4 ℃, and the hot air is cooled by the two cooling mediums to obtain cooling air with the temperature of 8 ℃; the cooling air directly enters a sulfur burning furnace and burns with 240kg/h liquid sulfur conveyed by a liquid sulfur conveying pump in the sulfur burning furnace to form SO 2 Air mixed gas, sulfur burning furnace outlet temperature is 610 ℃; SO (SO) 2 The air mixture is cooled to about 450 ℃ by an air cooler at the upper part of the conversion tower, and then is loaded with V in the conversion tower 2 O 5 Catalytic bed of (2) SO 2 Conversion to SO 3 Finally SO with the temperature of 480 ℃ is obtained at the outlet of the conversion tower 3 Air-mixed gas; SO (SO) 3 The air mixture enters a primary air cooler to be cooled to 270 ℃ and then enters an atomization tank, the upper part of the atomization tank is atomized and sprayed with 60 percent fuming sulfuric acid (liquid SO for another production line) 3 Control) by adjusting the flow rate of the sprayed fuming sulfuric acid to 210L/h, controlling the particle size of the atomized fuming sulfuric acid to about 65 μm, and at this time SO 3 The fuming sulfuric acid is separated out from the air mixed gas, and combined with the fuming sulfuric acid sprayed by atomization, the particle size is increased, and the fuming sulfuric acid is settled to the bottom of the tank under the action of gravity SO 3 Air flows out from the top of the atomization tank; SO passing through atomization tank 3 The air mixture enters a secondary air cooler to be cooled to 55 ℃, and the SO is generated at the moment 3 The gas volume concentration is 6%, and the flow rate of the fatty alcohol-polyoxyethylene ether is regulated to 2050kg/h, and the gas volume concentration is equal to SO 3 The air mixture enters a sulfonator together for reaction. By burning sulfurGas SO 3 The mixed gas obtained by the air generation process enters a distributor from the top of a sulphonater and reacts with the fatty alcohol-polyoxyethylene ether conveyed by an organic material pump in the sulphonater, the reaction heat release amount is large, the reaction heat is removed in time by using circulating water, the temperature of the circulating cooling water of the sulphonater is controlled to be about 32 ℃, and sulfuric acid ester is obtained at the bottom of the sulphonater; the sulfuric acid ester is separated from acid gas by a gas-liquid separator and a cyclone separator, the gas goes to a tail gas absorption section, the liquid acid ester is conveyed to a neutralization mixer together with 32% liquid alkali (990 kg/h) and process water (460 kg/h) by a neutralization mixing pump, and the product fatty alcohol polyoxyethylene ether sodium sulfate is obtained after neutralization.
The product detection data obtained are shown in Table 2:
TABLE 2 detection data
Example 3
The embodiment provides a production process of fatty alcohol polyoxyethylene ether sodium sulfate, the flow is 5775m 3 The external air of/h enters the Roots blower for compression after impurity removal through the filter, the pressure at the outlet of the blower is increased to about 56KPa, and then the air enters the low-temperature air condenser; the hot air in the low-temperature air condenser is sequentially cooled by two cooling mediums, namely cooling water and ethylene glycol solution with the temperature of 0+/-4 ℃, and the hot air is cooled by the two cooling mediums to obtain cooling air with the temperature of 8 ℃; the cooling air directly enters a sulfur burning furnace and burns with the liquid sulfur with the flow rate of 330kg/h conveyed by a liquid sulfur conveying pump in the sulfur burning furnace to form SO 2 Air mixed gas, sulfur burning furnace outlet temperature is 600 ℃; SO (SO) 2 The air mixture is cooled to about 450 ℃ by an air cooler at the upper part of the conversion tower, and then is loaded with V in the conversion tower 2 O 5 Catalytic bed of (2) SO 2 Conversion to SO 3 Finally SO with the temperature of 480 ℃ is obtained at the outlet of the conversion tower 3 Air-mixed gas; SO (SO) 3 The air mixture enters a primary air cooler to be cooled to 270 ℃ and then enters fogA melting tank, wherein the upper part of the melting tank is sprayed with 60% fuming sulfuric acid (liquid SO for another production line) by spray nozzle 3 ) The particle size of the atomized fuming sulfuric acid is controlled to be about 750 mu m by adjusting the flow rate of the fuming sulfuric acid to be 320L/h, and at the moment, SO 3 The fuming sulfuric acid is separated out from the air mixed gas, and combined with the fuming sulfuric acid sprayed by atomization, the particle size is increased, and the fuming sulfuric acid is settled to the bottom of the tank under the action of gravity SO 3 Air flows out from the top of the atomization tank; SO passing through atomization tank 3 The air mixture enters a secondary air cooler to be cooled to 55 ℃, and the SO is generated at the moment 3 The volume concentration of the gas is 6 percent, and simultaneously, the flow rate of the fatty alcohol-polyoxyethylene ether is 2510kg/h, and the gas is mixed with SO 3 The air mixture enters a sulfonator together for reaction. By burning sulfur-method gas SO 3 The mixed gas obtained by the air generation process enters a distributor from the top of a sulphonater and reacts with the fatty alcohol-polyoxyethylene ether conveyed by an organic material pump in the sulphonater, the reaction heat release amount is large, the reaction heat is removed in time by using circulating water, the temperature of the circulating cooling water of the sulphonater is controlled to be about 32 ℃, and sulfuric acid ester is obtained at the bottom of the sulphonater; the sulfuric acid ester is separated from acid gas by a gas-liquid separator and a cyclone separator, the gas goes to a tail gas absorption section, the liquid acid ester is conveyed to a neutralization mixer together with 32% liquid alkali (1275 kg/h) and process water (650 kg/h) by a neutralization mixing pump, and the product fatty alcohol polyoxyethylene ether sodium sulfate is obtained after neutralization.
The product detection data obtained are shown in Table 3:
TABLE 3 detection data
As can be seen from Table 1, table 2 and Table 3, SO is obtained by using the process for producing sodium fatty alcohol-polyoxyethylene ether sulfate provided by the invention 3 The quality of the product fatty alcohol-polyoxyethylene ether sulfuric acid obtained by using the air mixed gas to sulfonate the fatty alcohol-polyoxyethylene ether is the same as that of the original process, but the gas generation process flow related by the invention does not need a silica gel tower drying link, the use equipment cost and the energy consumption are greatly reduced, and the invention relates to a method for preparing the product fatty alcohol-polyoxyethylene ether sulfuric acidCan shorten the start-up and stop time, save the cost and the energy consumption, and is suitable for industrial production.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (10)
1. The production process of the fatty alcohol polyoxyethylene ether sodium sulfate is characterized by comprising the following steps of:
1) Heating and pressurizing outside air after removing impurities, cooling by two cooling mediums, and enabling the obtained cooling air to enter a sulfur burning furnace; simultaneously, liquid sulfur enters a sulfur burning furnace to be in countercurrent contact with cooling air, and is ignited for combustion to generate SO 2 A gas;
2) Diluting the SO in the step 1) 2 The gas enters a conversion tower to be catalytically converted to obtain SO 3 Diluting the gas with cooling air, and diluting the diluted SO 3 After the air mixture is first cooled, fuming sulfuric acid or liquid SO is sprayed in by atomization 3 SO removal 3 Sulfuric acid liquid drops separated out from the air mixed gas;
3) SO after the sulfuric acid liquid drops are removed in the step 2) 3 Filtering the air mixed gas through a secondary cooler and a demister to remove acid mist, and then carrying out sulfonation reaction on the air mixed gas and fatty alcohol polyoxyethylene ether to obtain a reactant sulfate;
4) And (3) removing acid gas from the reactant sulfuric acid ester obtained after the reaction in the step (3), and then carrying out neutralization reaction with process water and liquid alkali to obtain the product fatty alcohol polyoxyethylene ether sodium sulfate after neutralization.
2. The process for producing sodium fatty alcohol-polyoxyethylene ether sulfate according to claim 1, wherein the temperature of the cooling air subjected to the cooling treatment in the step 1) is 4-8 ℃.
3. The production process of the fatty alcohol-polyoxyethylene ether sodium sulfate according to claim 1, wherein the molar ratio of the liquid sulfur to the fatty alcohol-polyoxyethylene ether flow is 1.02-1.12:1.
4. The process for producing sodium fatty alcohol-polyoxyethylene ether sulfate according to claim 1, wherein the SO obtained after combustion in step 1) is 2 The temperature of the gas is 450-700 ℃.
5. The process for producing sodium fatty alcohol-polyoxyethylene ether sulfate according to claim 1, wherein the diluted SO in the step 2) is 3 The temperature of the air mixture is 440-470 ℃.
6. The process for producing sodium fatty alcohol-polyoxyethylene ether sulfate according to claim 1, wherein in the step 2), SO 3 The temperature of the air mixed gas after primary cooling is 270 ℃; atomized spraying oleum or liquid SO 3 The flow rate of the jet liquid drops is 0.1-0.5 per mill of the inlet gas flow rate, and the particle size of the jet liquid drops is controlled to be 20-80 mu m.
7. The process for producing sodium fatty alcohol-polyoxyethylene ether sulfate according to claim 1, wherein in said step 3), SO 3 The temperature of the air mixture after secondary cooling is 45-60 ℃, and SO after secondary cooling 3 In air mixture, SO 3 The gas volume concentration is 3-6%.
8. The process for producing fatty alcohol-polyoxyethylene ether sodium sulfate according to claim 1, wherein the process water flow rate in the step 4) is 15-20% of the sulfate flow rate, and the liquid alkali flow rate is 35-40% of the sulfate flow rate.
9. A production system for the production process of sodium fatty alcohol-polyoxyethylene ether sulfate according to claim 1, wherein the production system comprises an air filter, a Roots blower, an air low-temperature condenser, a sulfur burner, a conversion tower, a primary air cooler, an atomization tank, a secondary air cooler, a demister, a sulfonator, a gas-liquid separator, a neutralization mixing pump and a neutralization mixer which are sequentially connected by pipelines; wherein, the sulfur burning furnace is provided with a liquid sulfur inlet; the primary air cooler is provided with a nicotinic acid outlet; the atomization tank is provided with a nicotinic acid outlet; the secondary air cooler is provided with a nicotinic acid outlet; the demister is provided with a nicotinic acid outlet; the sulfonator is provided with an inlet of fatty alcohol polyoxyethylene ether; the gas-liquid separator is provided with an acid gas outlet; the neutralizing mixer has a gas outlet.
10. The production system for the production process of the sodium fatty alcohol-polyoxyethylene ether sulfate according to claim 9, wherein two cooling medium flow pipelines, a circulating cooling water pipeline and a frozen glycol water solution pipeline are arranged in the air low-temperature condenser; the atomization tank is provided with an atomized nicotinic acid injection port, and receives SO from the primary air cooler 3 Air mixture, the top of which is communicated with a secondary air cooler.
Priority Applications (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB808394A (en) * | 1955-10-28 | 1959-02-04 | Continental Oil Co | Improvements in or relating to process for sulfonation of hydrocarbons |
| CN106563386A (en) * | 2015-10-11 | 2017-04-19 | 宁夏际华环境安全科技有限公司 | Production process for fatty alcohol-polyoxyethylene ether |
| CN111100284A (en) * | 2019-12-27 | 2020-05-05 | 赞宇科技集团股份有限公司 | Production process and device of high-quality fatty alcohol-polyoxyethylene ether sulfate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB808394A (en) * | 1955-10-28 | 1959-02-04 | Continental Oil Co | Improvements in or relating to process for sulfonation of hydrocarbons |
| CN106563386A (en) * | 2015-10-11 | 2017-04-19 | 宁夏际华环境安全科技有限公司 | Production process for fatty alcohol-polyoxyethylene ether |
| CN111100284A (en) * | 2019-12-27 | 2020-05-05 | 赞宇科技集团股份有限公司 | Production process and device of high-quality fatty alcohol-polyoxyethylene ether sulfate |
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