CN111100284A - Production process and device of high-quality fatty alcohol-polyoxyethylene ether sulfate - Google Patents
Production process and device of high-quality fatty alcohol-polyoxyethylene ether sulfate Download PDFInfo
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- CN111100284A CN111100284A CN201911372365.6A CN201911372365A CN111100284A CN 111100284 A CN111100284 A CN 111100284A CN 201911372365 A CN201911372365 A CN 201911372365A CN 111100284 A CN111100284 A CN 111100284A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08G65/30—Post-polymerisation treatment, e.g. recovery, purification, drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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 engineering. Aims to provide a production process of high-quality fatty alcohol-polyoxyethylene ether sulfate with light color and low dioxane residue. The technical scheme is as follows: a production process of high-quality fatty alcohol-polyoxyethylene ether sulfate comprises the following steps: 1) after being mixed with the desorption gas input by the vacuum degassing tank in the Venturi tube, the dry air enters the sulfur burning furnace from a gas phase inlet of the sulfur burning furnace; liquid sulfur enters a sulfur burning furnace from a sulfur burning furnace liquid sulfur inlet, is contacted and burned in the sulfur burning furnace to generate SO2 gas, and is diluted with dry air; 2) converting the diluted SO2 gas by a conversion tower, cooling by a cooler, and allowing the SO2 gas to enter a sulfonator to perform sulfonation reaction with fatty alcohol-polyoxyethylene ether (AEO) input into the sulfonator; 3) and separating the sulfonated product by a gas-liquid separator, treating the sulfonated product by a gas-phase tail gas removal treatment system, discharging the sulfonated product after reaching the standard, and introducing the liquid-phase fatty alcohol-polyoxyethylene ether sulfate into an acid ester degassing system for degassing under vacuum.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a production process for producing sodium fatty alcohol-polyoxyethylene ether sulfate.
Background
The fatty alcohol-polyoxyethylene ether sulfate has excellent wetting, decontaminating, emulsifying and foaming properties, good thickening effect, wide compatibility and good biodegradability, and can be widely applied to liquid detergents, such as meal washes, shampoos, bath lotions and the like, and also used as wetting agents, dyeing assistants, foaming agents, degreasing agents and the like in the industries of textile printing and dyeing, petroleum, leather, building materials and the like.
The fatty alcohol-polyoxyethylene ether sulfate is an anionic surfactant product obtained by sulfonating and neutralizing fatty alcohol-polyoxyethylene ether (AEO). Most of the prior sulfonation processes adopt gas-phase SO3The membrane sulfonation method is mainly used for preparing SO with gas concentration of about 2-6% by combustion conversion of sulfur3And sulfonating the gas with fatty alcohol-polyoxyethylene ether (AEO) and neutralizing with alkalis to obtain the product.
Dioxane is a by-product of the production of fatty alcohol polyoxyethylene ether sulfate, which is designated as a class 2B carcinogen by the international agency for research on cancer (IARC), and its production is inevitable. At the present stage, the neutralized materials are removed mainly by vacuum, so that the residues of the neutralized materials in the product are reduced; according to the state of the art, the dioxane residue in the fatty alcohol-polyoxyethylene ether sulfate product is basically about 10-mg/kg100 mg/kg.
Due to the easy foaming property of the neutralized material, the vacuum removal control difficulty is high; meanwhile, COD in the vacuum removal condensate is high, the vacuum removal condensate contains a large amount of dioxane, and the environmental effect is poor; especially in the process of producing the fatty alcohol polyoxyethylene ether ammonium sulfate, the removal liquid not only contains COD and dioxane, but also contains volatile ammonia, and the wastewater treatment is more difficult.
Disclosure of Invention
The invention aims to overcome the defects in the background art and provide a production process of high-quality fatty alcohol polyoxyethylene ether sulfate with light color and low dioxane residue.
The technical scheme provided by the invention is as follows:
a production process of high-quality fatty alcohol-polyoxyethylene ether sulfate comprises the following steps:
1) after being mixed with the desorption gas input by the vacuum degassing tank in the Venturi tube, the dry air enters the sulfur burning furnace from a gas phase inlet of the sulfur burning furnace; liquid sulfur enters the sulfur burning furnace from a liquid sulfur inlet of the sulfur burning furnace and is contacted and combusted in the sulfur burning furnace to generate SO2Gas and diluting with dry air;
2) diluted SO2Gas is converted by a conversion tower and cooled by a cooler, enters a sulfonator and is subjected to sulfonation reaction with fatty alcohol-polyoxyethylene ether (AEO) input into the sulfonator;
3) separating the sulfonated product by a gas-liquid separator, treating the sulfonated product by a gas-phase tail gas removal treatment system to reach the standard and discharging, introducing the liquid-phase fatty alcohol-polyoxyethylene ether sulfate into an acid ester degassing system for degassing under vacuum, returning the removed gas to the step 1), mixing the removed gas with the air in the drying process, and introducing the mixture into a sulfur furnace;
4) after degassing, the acid ester enters a conventional neutralization system to produce a finished product fatty alcohol-polyoxyethylene ether sulfate;
the flow of the liquid sulfur entering the sulfur furnace in the step 1) is determined according to the productivity; the ratio of the flow rate of the liquid sulfur to the flow rate of the fatty alcohol-polyoxyethylene ether entering the sulfonator is 0.12-0.13.
SO at the outlet of the sulfur burner2The gas temperature is 450-700 ℃.
SO entering the sulfonator in the step 2)3The gas has a volume concentration of 2-6% (determined by controlling the flow of drying air into the sulfur burner) and a temperature of 50-70%.
The acid ester degassing system in the step 3) is a vacuum continuous membrane degassing system (such as a degassing system provided with a falling film evaporator) or a vacuum continuous kettle degassing system (such as a degassing system provided with a reaction kettle evaporator); the removal temperature is 50-80 ℃, and preferably 50-60 ℃; the vacuum degree of the removal is-20 to-99 kPa, preferably-40 to-80 kPa.
The utility model provides a apparatus for producing of high-quality fatty alcohol polyoxyethylene ether sulfate which characterized in that: the device comprises a Venturi tube, a sulfur furnace and an SO which are communicated in sequence by pipelines2Conversion column, SO3A cooler, a sulfonator, a gas-liquid separator, a delivery pump, a vacuum degasser and a vacuum pump;
the sulfonator is provided with a raw material inlet for inputting a fatty alcohol-polyoxyethylene ether raw material; the gas-liquid separator is provided with a tail gas outlet for outputting tail gas;
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 end of the Venturi tube is communicated with a gas phase inlet of the sulfur burning furnace;
the vacuum degasser is provided with a product outlet for outputting fatty alcohol-polyoxyethylene ether sulfate; the gas phase output end of the vacuum degasser is communicated with a vacuum pump.
The vacuum degasser is a conventional falling film evaporator or a conventional reaction kettle evaporator.
The vacuum pump is a roots vacuum pump or a screw vacuum pump.
The invention has the beneficial effects that:
1) the method utilizes a vacuum degassing system to carry out vacuum degassing on the fatty alcohol polyoxyethylene ether sulfate obtained after sulfonation, and can effectively remove the byproduct dioxane in the fatty alcohol polyoxyethylene ether sulfate. The dioxane in the acid ester can be reduced to be within 10mg/kg from the original about 50mg/kg, and the fatty alcohol-polyoxyethylene ether sulfate product with excellent quality can be obtained by direct neutralization. Avoids various defects brought by removing the dioxane from the neutralized product in the prior art. Meanwhile, the process and the equipment are relatively simple, and the investment cost is greatly reduced.
2) The invention utilizes a vacuum degassing system to carry out vacuum degassing on the fatty alcohol-polyoxyethylene ether sulfate obtained after sulfonation, SO that SO in the fatty alcohol-polyoxyethylene ether sulfate can be effectively removed3The content of sulfate in the neutralized product can be reduced from about 0.5 percent of the original process to within 0.3 percent. With SO3To avoid SO in the acid ester3The side reaction caused by the existence of the compound can be further carried out, thereby improving the color of the product and reducing the generation of the dioxane.
3) According to the invention, the tail gas after vacuum removal is mixed with the dry gas, the mixture enters the sulfur burning furnace for combustion, and the dioxane is thoroughly burnt at high temperature by using the sulfur burning furnace, so that adverse effects caused by the fact that the dioxane enters a sewage system after being removed in the subsequent process are avoided. At the same time can remove SO3And returning to the system again to reduce waste.
4) In the original sulfonation process, a large amount of bubbles are carried in the acid ester after simple gas-liquid separation, and the bubbles can cause inaccurate measurement of a flow meter in a subsequent neutralization system, thereby increasing the neutralization control difficulty; in addition, it has been found that the presence of bubbles in the acid ester can also lead to accelerated decomposition of the acid ester. In the acid ester treated by the vacuum degassing system, a large amount of entrained bubbles are reduced; thus, the control of the subsequent neutralization system can be more accurate, and the stability of the acid ester can be improved, thereby further improving the product quality.
Drawings
FIG. 1 is a schematic view of the system structure of the production apparatus of the present invention.
In the figure: 1 is a dry air inlet, 2 is a liquid sulfur inlet, 3 is a raw material inlet, 4 is a Venturi tube, 5 is a sulfur furnace, and 6 is SO2Conversion tower, 7 is SO2A cooler, 8 is a sulfonator, 9 is a gas-liquid separator, 10 is a delivery pump, 11 is a vacuum degasser, 12 is a vacuum pump, 13 is a product outlet, and 14 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 the high-quality fatty alcohol polyoxyethylene ether sulfate shown in the attached drawing comprises a Venturi tube 4, a sulfur burning furnace 5 and SO which are communicated in sequence by pipelines2Conversion tower 6, SO3A cooler 7, a sulfonator 8, a gas-liquid separator 9, a conveying pump 10, a vacuum degasser 11 and a vacuum pump 12.
The sulfonator is provided with a raw material inlet 3 for inputting fatty alcohol-polyoxyethylene ether.
The gas-liquid separator is provided with a tail gas outlet 14 for outputting tail gas;
the inlet end of the Venturi tube is communicated with the dry air inlet 1, and the suction end of the Venturi tube is communicated with the exhaust end of the vacuum pump; the outlet end of the venturi tube is communicated with a gas phase inlet of the sulfur burning furnace.
The vacuum degasser is provided with a product outlet 13 for outputting fatty alcohol polyoxyethylene ether sulfate. The gas phase output end of the vacuum degasser is communicated with a vacuum pump.
Example 1:
3500m3about/h of dry air is mixed with a small amount of gas input by the vacuum degassing tank in a Venturi tube and then enters the sulfur burning furnace; simultaneously, liquid sulfur enters a sulfur burning furnace according to the flow of 300kg/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 3 percent and the temperature of 55 DEG C3The gas enters a falling film type sulfonation reactor; simultaneously, fatty alcohol-polyoxyethylene ether (AEO) enters a falling film sulfonation reactor at a flow rate of 2500kg/h and reacts with SO3Carrying out sulfonation reaction by gas contact;
separating sulfonated product by a gas-liquid separator, outputting gas phase, treating by a tail gas removal treatment system to reach the standard, discharging, conveying liquid-phase fatty alcohol-polyoxyethylene ether sulfate into a falling film evaporator by a pump, and performing vacuum degassing by a screw vacuum pump at 60 ℃ to control the vacuum degree to be-85 kPa;
mixing the gas removed in the falling film evaporator into dry air by using a venturi tube, and completely burning organic matters in the dry air in a sulfur burning furnace; and (4) outputting the degassed acid ester, and then feeding the acid ester into a conventional neutralization system to be neutralized with liquid alkali and water to produce the finished product of the sodium fatty alcohol-polyoxyethylene ether sulfate.
The comparative indices of the final product are as follows:
example 2:
4000m3about/h of dry air is mixed with a small amount of gas input by the vacuum degassing tank in a Venturi tube and then enters the sulfur burning furnace; simultaneously, liquid sulfur enters a sulfur burning furnace according to the flow of 300kg/h, and is contacted and burned in the sulfur burning furnace to generate SO with the temperature of about 520 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 4.0 percent and the temperature of 60 DEG C3The gas enters a falling film type sulfonation reactor; meanwhile, fatty alcohol-polyoxyethylene ether (AEO) enters a sulfonator at the flow rate of 2500kg/h and contacts with SO3 gas to carry out sulfonation reaction.
Separating sulfonated product by a gas-liquid separator, outputting gas phase, treating by a tail gas removal treatment system to reach the standard, discharging, conveying liquid-phase fatty alcohol polyoxyethylene ether sulfate into a falling film evaporator by a pump, performing vacuum degassing by a screw vacuum pump at 60 ℃, and controlling the vacuum degree to be-90 kPa.
Mixing the gas removed in the falling film evaporator into dry air by using a venturi tube, and completely burning organic matters in the dry air in a sulfur burning furnace; and after degassing, the acid ester enters a conventional neutralization system, and is neutralized with liquid alkali and water to produce the finished product of the sodium fatty alcohol polyoxyethylene ether sulfate.
The comparative indices of the final product are as follows:
example 3:
2800m3about/h of dry air is mixed with a small amount of gas input by the vacuum degassing tank in a Venturi tube and then enters the sulfur burning furnace; simultaneously, liquid sulfur enters a sulfur burning furnace according to the flow of 240kg/h, and is combusted in the sulfur burning furnace in a contact way to generate SO2 gas with the temperature of about 600 ℃; 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 3.5 percent and the temperature of 55 DEG C3The gas enters a falling film type sulfonation reactor; simultaneously, fatty alcohol-polyoxyethylene ether (AEO) enters a sulfonator at the flow rate of 2000kg/h and is mixed with SO3The gas contacts to carry out sulfonation reaction.
Separating sulfonated product by a gas-liquid separator, outputting gas phase, treating by a tail gas removing treatment system, discharging, delivering liquid-phase fatty alcohol-polyoxyethylene ether sulfate into a falling film evaporator by a pump, vacuum degassing by a screw vacuum pump at 60 ℃, and controlling the vacuum degree to be-80 kPa.
The degasification in the falling film evaporator is mixed into the dry air by a Venturi tube and enters a sulfur furnace to completely burn the organic matters in the dry air; and after degassing, the acid ester enters a conventional neutralization system, and is neutralized with ammonia water and water to produce the finished product of the fatty alcohol-polyoxyethylene ether ammonium sulfate.
The comparative indices of the final product are as follows:
Claims (9)
1. a production process of high-quality fatty alcohol-polyoxyethylene ether sulfate comprises the following steps:
1) after being mixed with the desorption gas input by the vacuum degassing tank in the Venturi tube, the dry air enters the sulfur burning furnace from a gas phase inlet of the sulfur burning furnace; liquid sulfur enters the sulfur burning furnace from a liquid sulfur inlet of the sulfur burning furnace and is contacted and combusted in the sulfur burning furnace to generate SO2Gas and diluting with dry air;
2) diluted SO2Gas is converted by a conversion tower and cooled by a cooler, and enters a sulfonator to be sulfonated with fatty alcohol-polyoxyethylene ether input into the sulfonator;
3) separating the sulfonated product by a gas-liquid separator, treating the sulfonated product by a gas-phase tail gas removal treatment system to reach the standard and discharging, introducing the liquid-phase fatty alcohol-polyoxyethylene ether sulfate into an acid ester degassing system for degassing under vacuum, returning the removed gas to the step 1), mixing the removed gas with the air in the drying process, and introducing the mixture into a sulfur furnace;
4) and (4) after degassing, enabling the acid ester to enter a conventional neutralization system, and producing to obtain the finished product fatty alcohol-polyoxyethylene ether sulfate.
2. The production process of the high-quality fatty alcohol-polyoxyethylene ether sulfate according to claim 1, characterized in that: the flow rate of the liquid sulfur in the step 1) and the flow rate of the fatty alcohol-polyoxyethylene ether entering the sulfonator are respectively 0.12-0.13.
3. The production process of the high-quality fatty alcohol-polyoxyethylene ether sulfate according to claim 2, characterized in that: SO at the outlet of the sulfur burner2The gas temperature is 450-700 ℃.
4. The production process of the high-quality fatty alcohol-polyoxyethylene ether sulfate according to claim 3, characterized in that: SO entering the sulfonator in the step 2)3The gas has a volume concentration of 2-6% and a temperature of 50-70%.
5. The production process of the high-quality fatty alcohol-polyoxyethylene ether sulfate according to claim 4, characterized in that: the removal temperature of the acid ester degassing system in the step 3) is 50-80 ℃, and the removal vacuum degree is-20 to-99 kPa.
6. The production process of the high-quality fatty alcohol-polyoxyethylene ether sulfate according to claim 5, characterized in that: the acid ester degassing system in the step 3) is a vacuum continuous membrane degassing system or a vacuum continuous kettle degassing system.
7. The utility model provides a apparatus for producing of high-quality fatty alcohol polyoxyethylene ether sulfate which characterized in that: the device comprises a Venturi tube (4), a sulfur furnace (5) and SO which are communicated with each other in sequence through pipelines2Conversion tower (6), SO3A cooler (7), a sulfonator (8), a gas-liquid separator (9), a delivery pump (10), a vacuum degasser (11) and a vacuum pump (12);
the sulfonator is provided with a raw material inlet (3) for inputting a fatty alcohol-polyoxyethylene ether raw material; the gas-liquid separator is provided with a tail gas outlet (14) for outputting tail gas;
the inlet end of the Venturi tube is communicated with a dry air inlet (1), and the suction end of the Venturi tube is communicated with the exhaust end of the vacuum pump; the outlet end of the Venturi tube is communicated with a gas phase inlet of the sulfur burning furnace;
the vacuum degasser is provided with a product outlet (13) for outputting fatty alcohol-polyoxyethylene ether sulfate; the gas phase output end of the vacuum degasser is communicated with a vacuum pump.
8. The production device of the high-quality fatty alcohol-polyoxyethylene ether sulfate according to claim 7, characterized in that: the vacuum degasser is a conventional falling film evaporator or a conventional reaction kettle evaporator.
9. The production device of the high-quality fatty alcohol-polyoxyethylene ether sulfate according to claim 8, characterized in that: the vacuum pump is a roots vacuum pump or a screw vacuum pump.
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| CN201911372365.6A CN111100284A (en) | 2019-12-27 | 2019-12-27 | Production process and device of high-quality fatty alcohol-polyoxyethylene ether sulfate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112795004A (en) * | 2020-12-22 | 2021-05-14 | 赞宇科技集团股份有限公司 | Production process and production system of fatty alcohol-polyoxyethylene ether sodium sulfate |
| CN114288829A (en) * | 2021-12-29 | 2022-04-08 | 赞宇科技集团股份有限公司 | Comprehensive recovery device and recovery process for AES tail gas absorption liquid |
| CN116589385A (en) * | 2023-05-09 | 2023-08-15 | 安徽金桐精细化学有限公司 | Preparation method of low dioxane ethoxylated alkyl sodium sulfate |
| CN116903497A (en) * | 2023-09-11 | 2023-10-20 | 南京为先科技有限责任公司 | Method for preparing sulfonate surfactant by sulfur trioxide film sulfonation |
-
2019
- 2019-12-27 CN CN201911372365.6A patent/CN111100284A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112795004A (en) * | 2020-12-22 | 2021-05-14 | 赞宇科技集团股份有限公司 | Production process and production system of fatty alcohol-polyoxyethylene ether sodium sulfate |
| CN112795004B (en) * | 2020-12-22 | 2023-09-26 | 赞宇科技集团股份有限公司 | Production process and production system of fatty alcohol polyoxyethylene ether sodium sulfate |
| CN114288829A (en) * | 2021-12-29 | 2022-04-08 | 赞宇科技集团股份有限公司 | Comprehensive recovery device and recovery process for AES tail gas absorption liquid |
| CN116589385A (en) * | 2023-05-09 | 2023-08-15 | 安徽金桐精细化学有限公司 | Preparation method of low dioxane ethoxylated alkyl sodium sulfate |
| CN116903497A (en) * | 2023-09-11 | 2023-10-20 | 南京为先科技有限责任公司 | Method for preparing sulfonate surfactant by sulfur trioxide film sulfonation |
| CN116903497B (en) * | 2023-09-11 | 2024-03-29 | 南京为先科技有限责任公司 | Method for preparing sulfonate surfactant by sulfur trioxide film sulfonation |
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Application publication date: 20200505 |