JP2001181255A - Method for producing sulfonated/sulfated product - Google Patents

Abstract

PROBLEM TO BE SOLVED: To separate mist generated in producing sulfonated/sulfated products by a first and a second vapor-liquid separation means as liquid, and to feed the liquid to a sulfur burner. SOLUTION: The mist generated in producing sulfonated/sulfated products is returned to production processes without impairing the quality of products to reduce the quantity of waste products.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for reducing waste (sulfonated mist) of a production process to a process without impairing the quality of the product when producing a sulfonated product / sulfated oxide.

[0002]

2. Description of the Related Art Conventionally, in a process for producing a sulfonated product / sulfur oxide, after a gas-liquid separation of a reaction product of an SO3 gas and an organic raw material, a gas containing a mist is sent to an exhaust gas treatment device to remove the mist. Separated and discharged, mist is
Had been disposed of as waste. The mist contains sulfonic acid / sulfuric acid ester, unreacted organic raw material, unreacted SO3
Gas etc. are included. In recent years, due to environmental protection and energy issues, there has been an increasing tendency to eliminate factory waste, and there is a demand for a sulfonated / sulfurized oxide production method that can reduce mist to the production process without impairing the quality of the product. Was.

[0003]

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide a method for producing a sulfonated product / sulfuric oxide which can reduce the mist to a production step without deteriorating the quality of the product.

[0004]

Means for Solving the Problems and Embodiments of the Invention As a result of intensive research, the present inventors have separated the mist as a liquid by means of gas-liquid separating means and supplied the liquid to a sulfur burner. Found that it is possible to produce sulfonated compounds / sulphated oxides without impairing the quality of the product,
The present invention has been completed. That is, the present invention provides a sulfur burner that generates SO2 gas by burning sulfur and an SO2 gas that converts the SO2 gas into SO3 gas using an oxidation catalyst.
3 converter, and a sulfonation reaction between the SO3 gas and an organic raw material to produce a sulfonic acid / sulfuric acid ester /
A sulfation reactor, first gas-liquid separation means for separating a reaction product in the sulfonation / sulfation reactor into a gas containing a liquid and a mist, and a first gas-liquid separation means for separating the reaction product in the first gas-liquid separation means. Second gas that separates the gas containing the mist into liquid and gas.
A method for producing a sulfonated product / sulfuric oxide, comprising a liquid separating means, and supplying at least a part of the liquid separated by the second gas-liquid separating means to a sulfur burner.

Hereinafter, the present invention will be described in more detail.
In addition,% indication of the blending amount described below means mass%. The outline of the method for producing the sulfonated product / sulfuric oxide of the present invention is shown in FIG. First, the air from which moisture has been removed by the dryer 4 and the molten sulfur are supplied to the sulfur burner 5, and the sulfur is burned to generate SO2 gas. The SO2 gas is introduced into an SO3 converter 6 filled with an oxidation catalyst, where it is converted to SO3 gas.

The SO3 gas and the organic raw material are sulfonated /
It is introduced into the sulfation reactor 7 and reacts to produce sulfonic acid / sulfate. The reaction product contains the sulfonic acid / sulfuric acid ester, unreacted organic raw material, unreacted SO3 gas, air, etc., which are sent to the first gas-liquid separator 8, Separated into a liquid and a gas, the liquid is sent to the next neutralization step (not shown) and becomes a sulfonate / sulfur oxide.

The gas separated by the first gas-liquid separation means 8, that is, the gas containing mist, is supplied to the second gas-liquid separation means 9.
Where the mist is separated as a liquid, and the gas from which the mist has been removed is discharged. Once the separated liquid,
Sulfur burner 5 is stored in storage tank 11 and pumped from here.
Supplied to

[0008] The liquid separated by the second gas-liquid separation means 9 is preferably 0.1 to 5%, especially 0.1 to 5% of sulfur.
It is preferable to supply the sulfur burner at a ratio of 1%. If it exceeds 5%, the quality of the sulfonated product / sulfated oxide may be adversely affected. The separated liquid may be supplied to the sulfur burner alone, or may be supplied by mixing with sulfur or air. Although the separated liquid may be partially supplied to the sulfur burner, it is preferable to supply the whole liquid at the above-mentioned ratio.

The organic raw materials used in the present invention include alkylbenzene, α-olefin, fatty acid alkyl ester,
Higher alcohols and alkylene oxide adducts of higher alcohols.

The sulfonation / sulfation reactor used in the present invention is a falling film reactor, a tube reactor, a tank reactor, etc., and particularly preferably a falling film reactor or a tube reactor.

The first gas-liquid separation means used in the present invention is a cyclone, a flash can, a stirring tank or the like, preferably a cyclone.

The second gas-liquid separation means used in the present invention is an electric precipitator, an absorption tower or the like, and an electric precipitator is preferable.

[0013]

According to the present invention, mist generated during the production of a sulfonated product / sulfuric oxide can be reduced to the production process without deteriorating the quality of the product, and waste can be reduced.

Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.

[0015]

Embodiment 1 FIG. 1 is a flowchart showing an embodiment of the present invention. Sulfur was transferred from the sulfur storage tank 1 to the sulfur burner 5 by piping, and air taken in by the blower 3 from the air intake port 2 was burned by dry air dried by the air dryer 4 to generate SO2 gas.
Next, this SO2 gas is converted into SO3 gas by the converter 6.
It was converted to gas and introduced into the reactor 7. In the reactor 7, linear alkylbenzene was introduced from a raw material tank (not shown) from a raw material introduction section 14, and a sulfonation reaction was performed with SO3 generated by combustion of sulfur to generate a sulfonated product. The generated sulfonate is introduced into the cyclone 8 in a mixed state with unreacted SO3 gas and air at this time. In cyclone 8, liquid and gas are separated,
Linear alkylbenzene sulfonic acid was obtained as a liquid from the lower product outlet 15. On the other hand, the gas portion extracted from the upper part of the cyclone contains air, unreacted SO3, and mist as fine droplets of linear alkylbenzene sulfonic acid, which were collected by the electrostatic precipitator 9 in the subsequent process. The mist collected by the electric dust collector was stored in a mist tank 11. On the other hand, sulfuric acid scrubber 10
After collecting 3 and the like, the air was discharged from the exhaust unit 16 to the atmosphere as clean air. Here, the collected matter (including sulfonated matter, sulfuric acid content, unreacted oil content, etc.) stored in the storage tank 11 is transferred to the transfer pump 1.
2, the sulfur was added to the sulfur burner via the transfer line 13 in an amount of 0.5% based on the amount of sulfur, and the sulfur was burned by the sulfur burner. The color tone of the resulting sulfonated product was 5 points, and the reaction rate and the properties of the exhaust gas were the same as those in the case where the collected material was not added. In addition, since the collected materials were recycled and burned, the amount of waste that was discarded as mist could be reduced.

[0016]

[Comparative Example 1] The same reaction as in the example was carried out, and the reaction was carried out by a conventional method without recycling and burning the mist storage tank waste. As a result, 0.4% of the sulfonic acid product was discarded as mist waste per product weight. Things happened.

[0017]

Comparative Example 2 The same reaction as in the example was carried out, and the reaction was carried out by a conventional method without recycling and burning the mist storage tank waste. The collected mist was directly mixed with a sulfonated product to confirm the properties. As a result, the mist is not discarded, but the color tone of the sulfonic acid is 1 to 2 points.
The color tone was worse than that of, and the product could not be produced. Evaluation criteria of color tone 5 points: equivalent to the conventional method (Comparative Example 1) 4 points: deterioration within 20% compared to the conventional method 3 points: deterioration of 20 to 50% compared to the conventional method 2 points: 50 compared to the conventional method ~ 100% degradation 1 point: 100% or more degradation compared to conventional

[Brief description of the drawings]

FIG. 1 is an embodiment of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Sulfur storage tank 9 Electric dust collector 2 Air intake 10 Sulfuric acid scrubber 3 Blower 11 Mist tank 4 Air dryer 12 Transfer pump 5 Sulfur burner 13 Transfer line 6 Converter 14 Raw material introduction part 7 Reactor 15 Product extraction port 8 Cyclone 16 Exhaust part

Claims (1)

[Claims] 1. A sulfur burner for producing SO2 gas by burning sulfur, and the SO2 gas is converted to SO2 gas by an oxidation catalyst.
SO3 converter for converting into three gases, a sulfonation / sulfation reactor for reacting the SO3 gas with an organic raw material to produce a sulfonated product / sulfated oxide, and a reaction product in the sulfonation / sulfation reactor Gas-liquid separation means for separating the gas into liquid and mist-containing gas, and second gas-liquid separation means for further separating the mist-containing gas separated by the first gas-liquid separation means into liquid and gas. -A method for producing a sulfonated product / sulfur oxide, comprising a liquid separating means, and supplying at least a part of the liquid separated by the second gas-liquid separating means to a sulfur burner.