JP3002779B1 - Method for producing sulfated oxide - Google Patents

Abstract

An object of the present invention is to provide a method for producing a sulfate, which is capable of obtaining a sulfate having a significantly improved hue at a low cost. A compound (hereinafter, referred to as a raw material compound) which reacts with SO ₃ gas to give a sulfate is supplied while flowing down the inner wall of a reaction tube to form a thin film of the raw material compound on the inner wall of the reaction tube. the sO ₃ gas and an inert gas into the reaction tube, a sulfated product manufacturing method of supplying to flow between the thin film and the sO ₃ gas flow of the inert gas starting compound, relative to sO ₃ gas A method for producing a sulfate, wherein an inert gas is supplied so as to have a flow rate ratio of 0.01 to 1.8 and a flow rate ratio of 0.1 to 1.2.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for producing a sulfur oxide useful as a surfactant whose hue is greatly improved.

[0002]

2. Description of the Related Art Sulfation by SO ₃ gas is a highly exothermic reaction, and the reaction product is viscous and lacks fluidity, so that it is liable to excessively react with SO ₃ .
There is a disadvantage that the reactants are often colored or mixed with carbides. Products with poor hue for various commercial purposes may have a reduced commercial value, and thus many methods have been proposed for these hue deteriorations.

In Japanese Patent Publication No. 49-48409, a thin film flow of a reaction solution and SO ₃ are used in a thin film sulfonation apparatus.
Air or inert gas as a cooling gas in the middle of the gas,
SO ₃ about 2-5 times the amount of gas, and by carrying out the sulfonation reaction substantially is introduced with SO ₃ gas stream at the same speed,
A method is disclosed in which the reaction temperature is kept constant to produce a sulfated product having less coloring and by-products. However, in this production method, a large amount of inert gas is required to flow an inert gas for cooling, and as shown in Japanese Patent Publication No. 53-41130 filed later by the applicant of the above publication. It is necessary to take measures such as recycling of exhaust gas, and there is a disadvantage that the load on the equipment is large. Further, although the hue of the sulfate obtained by using such a sulfation reaction method can be improved to some extent, further improvement is required.

[0004]

SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing a sulfate, which can obtain a sulfate having a significantly improved hue at a low cost. In the present invention, “sulfation” means so-called sulfonation or sulfate esterification.

[0005]

According to the present invention, a compound which reacts with SO ₃ gas to give a sulfate (hereinafter referred to as “raw material compound”) is supplied while flowing down the inner wall of the reaction tube, and is supplied onto the inner wall of the reaction tube. A method for producing a thin film of a raw material compound, and supplying an SO ₃ gas and an inert gas into the reaction tube such that the inert gas flows between the thin film of the raw material compound and the SO ₃ gas flow; The present invention also relates to a method for producing a sulfate in which an inert gas is supplied so as to have a flow rate ratio of 0.01 to 1.8 and a flow rate ratio of 0.1 to 1.2 with respect to SO ₃ gas.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION As the starting compounds used in the present invention, alkylaryl hydrocarbons, olefinic hydrocarbons, aliphatic alcohols, alkylphenols, ethoxylates thereof, and other organic compounds capable of being sulfated can be used. . The production method of the present invention is particularly useful for producing a polyoxyethylene alkyl ether sulfate, and the compound is neutralized with a common basic reagent such as an alkali metal hydroxide, an amine or an alkanolamine. Highly effective activator compounds can be prepared.

The flow rate of the raw material compound varies depending on the molecular weight of the raw material compound.
0 kg / mHr or more, and from the viewpoint of preventing excessive reaction due to poor mixing in the liquid film, the immersion side long flow rate 80
It is desirably 0 kg / mHr or less, preferably 600 kg / mHr or less (for example, 50 to 800 kg / mHr, preferably 100 to 600 kg / mHr). Among them, for example, when a reaction tube having an inner diameter of 20 mm or less such as 14 mm is used, the flow rate of the raw material compound is 2.2 kg / Hr or more, preferably 4.4.
kg / Hr or more, preferably 35 kg / Hr
Or less, preferably 26 kg / Hr or less (for example, 2.2 to 35 kg / Hr, preferably 4.4 to 26 kg / Hr).
kg / Hr). When a reaction tube having an inner diameter exceeding 20 mm such as 28 mm is used, the reaction tube is 4.4 kg / Hr or more, preferably 8.8 kg / H.
r, and preferably 70 kg / Hr or less, preferably 53 kg / Hr or less (for example, 4.
4 to 70 kg / Hr, preferably 8.8 to 53 kg / Hr
r) is desirable. The immersion side length flow rate can be obtained by the following equation.

[0008]

(Equation 1)

The temperature of the starting compound may be any temperature above the melting point or cloud point, and from the viewpoint of stable operation,
Before supplying to the reaction tube, it is desirable to adjust the temperature to a constant value by a general means and to supply.

In the reaction tube used in the present invention, a raw material compound is allowed to flow down on the inner wall of the reaction tube to form a thin film of the raw material compound, and SO ₃ gas and an inert gas are used. Any structure may be used as long as it can be supplied so as to flow between the thin film of SO ₃ and the SO ₃ gas flow. For example, a pipe shape is preferable from the viewpoint of manufacturing and availability of equipment.

The dimensions of the reaction tube are, specifically, when the reaction tube has a pipe shape, the inner diameter of the pipe prevents pressure loss,
From the viewpoint of suppressing energy loss, it is desirable that the thickness be 8 mm or more, preferably 12 mm or more. From the viewpoint of shortening the tube length necessary for terminating the reaction and suppressing the equipment cost, it is desirably 80 mm or less, preferably 40 mm or less. In addition, the length of the pipe in that case is preferably 1 m or more, preferably 2 m or more, from the viewpoint of completing the reaction, reducing unreacted raw materials, or efficiently removing heat of reaction heat, From the viewpoint of reducing the apparatus cost by reducing the pressure loss, it is desirable that the distance be 15 m or less, preferably 10 m or less.

The material of the reaction tube is not particularly limited, and examples thereof include stainless steel, glass, fluororesin, titanium, and other alloy materials.

The reaction tube may be installed so that the raw material compound can flow down on the inner wall of the reaction tube, and the arrangement is not limited. For example, it is preferable that the reaction tube is set up vertically to a horizontal plane. .

The SO ₃ gas used in the present invention is generally diluted with air, nitrogen or other inert gas and used at a suitable concentration. In this case, it is generally preferable to use an SO ₃ concentration of 1.0% by volume or more and 10% by volume or less.

The flow rate of only SO ₃ gas at that time varies depending on the inner diameter of the reaction tube.
When a reaction tube having an inner diameter of 20 mm or less such as 1 mm is used, from the viewpoint of performing a good reaction, for example, 1.
8 × 10 ⁻³ Nm ³ / s or more, preferably 2.7 × 10 ⁻³
Nm ³ / s or more is desirable, and from the viewpoint of reducing the apparatus cost by reducing the pressure loss, 9.5 × 10 ^−3.
Nm ³ / s or less, preferably 8.0 × 10 ⁻³ Nm ³ / s
(For example, 1.8 × 10 ^{−3 to} 9.5 × 1)
0 ⁻³ Nm ³ / s, preferably 2.7 × 10 ^{−3 to} 8.0 ×
10 ⁻³ Nm ³ / s). Also, 28
When a reaction tube having an inner diameter exceeding 20 mm, such as 1 mm, is used, it is preferably at least 11 × 10 ⁻³ Nm ³ / s, preferably at least 15 × 10 ⁻³ Nm ³ / s,
57 × 10 ⁻³ Nm ³ / s or less, preferably 48 × 10 ⁻³
Nm ³ / s or less (for example, 11 × 10 ^{−3 to} 5
7 × 10 ⁻³ Nm ³ / s, preferably 15 × 10 ^{−3 to} 48
× 10 ⁻³ Nm ³ / s).

The flow rate of the SO ₃ gas is, for example, 3 from the viewpoint of forming an annular flow in the reaction and obtaining a uniform liquid film.
It is desirably 0 Nm / s or more, preferably 40 Nm / s or more, and from the viewpoint of preventing the liquid film from disturbing and preventing the generation of mist in the reaction, it is desirably 150 Nm / s or less, preferably 125 Nm / s or less.

The flow rate of the SO ₃ gas can be calculated according to the calculation method described in the following embodiment.

In the present invention, the inert gas supplied between the raw material compound and the SO ₃ gas is not particularly limited, and may be, for example, air, dehumidified dry air, sulfur such as nitrogen, or the like.
A gas that does not chemically react with both the O ₃ gas and the raw material compound can be used, and air is preferable in terms of cost, and dehumidified dry air is more preferable in order to reduce by-products such as sodium sulfate. Further, a part of the inert gas used for diluting the SO ₃ gas may be used.

The flow rate at that time is determined by the flow rate inside the reaction tube.
Depending on the diameter, for example, 20 mm like 14 mm
When one reaction tube with an inner diameter of less than 1 mm is used
Is, from the viewpoint of obtaining a sufficient hue improvement effect,
For example, 9.0 × 10^-FiveNm^Three/ S or more, preferably 1.4
× 10^-FourNm^Three/ S or more.
From the viewpoint of promoting and sufficiently reducing unreacted raw materials,
6.3 × 10^-3Nm^Three/ S or less, preferably 5.4 × 1
0^-3Nm^Three/ S or less (for example, 9.0 × 10
^-Five~ 6.3 × 10^-3Nm^Three/ S, preferably 1.4 × 1
0^-Four~ 5.4 × 10^-3Nm^Three/ S)
No. It also has an inner diameter exceeding 20 mm, such as 28 mm.
When one reaction tube is used, 1.1 × 10^-3N
m^Three/ S or more, preferably 1.5 × 10^-3Nm^Three/ S or less
Preferably above 5.7 × 10 ^-2Nm^Three/ S or less
Lower, preferably 4.8 × 10^-2Nm^Three/ S or less
(For example, 1.1 × 10^-3~ 5.7 × 10^-2Nm^Three/
s, preferably 1.5 × 10^-3~ 4.8 × 10^-2Nm^Three
/ S) is desirable.

The flow rate of the inert gas flowing over the raw material compound flowing down the inner wall of the reaction tube depends on the flow rate of the SO ₃ gas flowing through the center of the tube, but from the viewpoint of forming an annular flow and obtaining a uniform liquid film. For example, when one reaction tube having an inner diameter of 20 mm or less such as 14 mm is used, 9 Nm / s
Above, preferably 12 Nm / s or more, and from the viewpoint of prevention of liquid film disturbance and generation of mist,
180 Nm / s or less, preferably 150 Nm / s or less (for example, 9 to 180 Nm / s, preferably 1
2 to 150 Nm / s). Also, 2
When one reaction tube having an inner diameter exceeding 20 mm, such as 8 mm, is used, it is 3 Nm / s or more, preferably 4 Nm / s or more.
Nm / s or more, desirably 120 Nm / s or less, preferably 100 Nm / s or less (for example, 3 to 120 Nm / s, preferably 4 to 100 Nm / s).
s).

Incidentally, the flow rate of the inert gas can be calculated according to a calculation formula described in the following embodiment.

[0022] SO ₃ flow rate of the inert gas to the gas, can not be unconditionally defined by the flow passage area of the SO ₃ gas and an inert gas, the increase in flow area of the inert gas, the inert gas Since an increase in the flow rate is caused, the generation of reaction heat is excessively suppressed and the reaction becomes difficult to proceed, and the reaction is hardly completed in the reaction tube. Therefore, it is not preferable to extremely increase the flow path area. Conversely, a significant decrease in the flow channel area increases the pressure loss in the flow channel, causing a large difference between the liquid film thickness in the inert gas flow channel and the liquid film thickness after the start of the reaction. This is undesirable because it causes disturbance of the reaction and makes it difficult to obtain a reactant efficiently. From these viewpoints, the flow ratio (inert gas / SO ₃ gas) is 0.01 or more, preferably 0.015 or more, and more preferably 0.02 or more, although it varies depending on the inner diameter of the reaction tube. Also, 1.8
Or less, preferably 0.5 or less, more preferably 0.4 or less. Among them, 0.015 to 0.5 is preferable,
0.02 to 0.4 is more preferable.

In particular, when the inner diameter of the reaction tube is 20 mm or less, it is more preferably 0.05 or more, more preferably 0.1 or more, and particularly preferably 0.15 or more. Also, it is preferably 1.8 or less, more preferably 0.5 or less, and particularly preferably 0.4 or less. Among them, 0.0
It is preferably from 5 to 1.8, more preferably from 0.1 to 0.5, and particularly preferably from 0.15 to 0.4.

In particular, when the inner diameter of the reaction tube exceeds 20 mm, it is more preferably at least 0.01, more preferably at least 0.015, particularly preferably at least 0.02.
Further, it is preferably 0.2 or less, more preferably 0.15.
Or less, particularly preferably 0.1 or less. Among them, 0.
01-0.2 is preferable, 0.015-0.15 is more preferable, and 0.02-0.1 is particularly preferable.

The ratio of the flow rate of the inert gas to the SO ₃ gas is 0.1 or more, preferably 0.15 or more, and more preferably 0.2 or more, depending on the inner diameter of the reaction tube. In addition, 1.2 or less, preferably 1.0 or less,
It is more preferably 0.9 or less. Among them, 0.15
1.0 is preferred, and 0.2 to 0.9 is more preferred.

In particular, when the inner diameter of the reaction tube is 20 mm or less, it is more preferably 0.3 or more, more preferably 0.1 mm or more.
It is 4 or more, particularly preferably 0.5 or more. Further, it is preferably 1.2 or less, more preferably 1.0 or less, and particularly preferably 0.9 or less. Among them, 0.3 to 1.2 is preferable, 0.4 to 1.0 is more preferable, and 0.5 to 1.0 is preferable.
0.9 is particularly preferred.

In particular, when the inner diameter of the reaction tube exceeds 20 mm, it is more preferably 0.1 or more, more preferably 0.1 mm or more.
It is 15 or more, particularly preferably 0.2 or more. Further, it is preferably 0.8 or less, more preferably 0.6 or less, and particularly preferably 0.48 or less. Among them, 0.1-0.
8 is preferable, 0.15 to 0.6 is more preferable, and 0.
Particularly preferred is 2 to 0.48.

When the flow rate ratio is outside the above range, the effect of improving the hue of the obtained sulfate may be reduced. In the scope of these flow rate ratio, mixed into an inert gas of SO ₃ gas molecules at the boundary between the SO ₃ gas and the inert gas is suppressed, reaching a rate of the liquid film surface of the starting compound of the SO ₃ molecules It is considered that the rapid reaction in the upper part of the reactor is moderated by the decrease in the temperature, and local heat generation and a rapid rise in the temperature of the reactant are suppressed. In addition, by adjusting to these flow rate ratios, the amount of the inert gas used may be smaller than that of the prior art with respect to the amount of the SO ₃ gas.
Further, an excellent hue improving effect can be obtained without imposing a load on the equipment.

The apparatus used in the present invention is not particularly limited as long as it has a reaction tube having the above-mentioned structure. For example, a sulfation reaction apparatus as shown in FIGS. .

FIG. 1 is a schematic explanatory view of an example of a preferred sulfation reaction apparatus of the present invention. The sulfation reactor 1 is provided with a reaction tube 5 provided with a raw material compound supply port 2, an inert gas supply port 3, and an SO ₃ gas supply port 4, respectively.

The raw material compound, the inert gas and the SO ₃ gas are supplied into the reaction tube 5 from the respective supply ports at the upper part of the reaction tube 5. The raw material compounds react with the SO ₃ gas while flowing down the inner wall of the reaction tube 5. The reaction tube 5 has a structure that can be externally cooled by a cooling device 6, and cooling water is supplied to the cooling device 6. A gas-liquid separator (cyclone) 7 is provided at the end of the reaction tube 5 to separate sulfur oxides and exhaust gas.

FIG. 2 shows the sulfation reaction apparatus 1 shown in FIG.
FIG. 2 is a schematic explanatory view showing the structure of each supply port of a raw material compound, an inert gas, and an SO ₃ gas in FIG.

In carrying out the present invention on an industrial scale, it is preferable to use a multi-tube reactor in which a plurality of reaction tubes are combined. As the reaction tube used in this case, the inside diameter, length, and the like of the above-described reaction tube can be used, and it is preferable that each reaction tube has the same inside diameter, length, and the like.

[0034]

EXAMPLES Examples 1 to 3 As raw material compounds, lauryl alcohol and ethylene oxide were used.
Alkyl ether (molecular weight: 2.5 mol)
295) was used. FIG. 1 shows a reaction apparatus.
One reaction tube (reactor tube inner diameter (D): 14 mmφ,
Reaction tube length: 4m, SO_ThreeInner diameter of gas supply pipe
(D₁): 9 mm, SO_ThreeOuter diameter of gas supply pipe (d _Two):
12 mm).

The raw material compound, SO ₃ gas and inert gas were continuously supplied into the reaction tube from the respective supply ports, and a sulfation reaction was performed in the reaction tube. As for the flow rate of the raw material compound, the immersion length flow rate [= raw material flow rate / (π × reactor tube inner diameter (D))] is 100 kg / m · Hr, and other conditions are shown in Table 1. And a sulfation reaction was performed. The obtained sulfate was neutralized with an aqueous NaOH solution, and the hue (Klett No .; product containing 10% of activator), 10 mm cell, wavelength: 420 nm was measured. Table 1 shows the results.

[Calculation of Inert Gas Flow Rate] As shown in FIG. 2, a donut-shaped portion (reaction tube and S
The flow rate (u _s ) of the inert gas flowing through the gap between the O ₃ gas supply pipe) is obtained by the following formula.

[0037]

(Equation 2)

Here, u _S is the flow rate of the inert gas flowing through the donut-shaped portion [m / s], V _S is the flow rate of the inert gas flowing through the donut-shaped portion [m ³ / s], and D is the inner diameter of the reaction tube [m ], D
₂ indicates the outer diameter [m] of the SO ₃ gas supply pipe, and δ indicates the liquid film thickness [m] of the raw material compound flowing through the donut-shaped portion. Here, the liquid film thickness δ is determined by the following procedure.

First, as a simple model (hereinafter referred to as a cylindrical model), a velocity distribution u of a liquid film flowing on the inner wall of a cylindrical reaction tube in the direction perpendicular to the axial direction of the reaction tube (y-axis direction)
(Y) is expressed as follows from the Navier-Stokes equation.

[0040]

(Equation 3)

(Note that P is a pressure [Pa], u _L is a liquid flow rate [m / s] of the cylindrical model, u _G is an inert gas flow rate [m / s] of the cylindrical model, and u _Li is a gas flow rate of the cylindrical model. Liquid flow velocity at liquid interface [m / s], g is gravitational acceleration [m / s ² ], y
Is the distance [m] in the y-axis direction from the inner wall of the reaction tube, z is the distance [m] in the axial direction of the reaction tube, f is the coefficient of friction between the inert gas and the liquid [-] (calculated by the following formula), ρ _L is the liquid density [kg /
m ^3], [rho _G is the inert gas density [kg / m ^3], mu _L is the viscosity of the liquid [Pa. s], τ _i is the gas-liquid interface shear stress [P
a], δ ′ is the liquid film thickness [m] of the cylindrical model, and Γ ′ is δ ′
Length flow [kg / mH] obtained by calculation based on
r]. Here, the friction coefficient f between the inert gas and the liquid is f
Is obtained by ^{f = 0.0791 · Re -0.25, Re} =
(D · ρ _G · u _G ) / μ _G ; D, ρ _G and u _G are the same as above, and μ _G denotes the inert gas viscosity [Ps · s]. )

Further, the actual immersion side length flow rate [kg / mH]
r] is obtained by Γ = liquid flow rate / (π · D). Here, the liquid film thickness δ ′ is assumed, and the immersion side long flow rate Γ ′ obtained based on this assumption is obtained by Expression (6), and the immersion side long flow rate Γ ′ is obtained.
= Actual immersion side length flow rate Γ (kg / mHr; match up to two decimal places) δ 'is determined. In determining δ ′, the determination is performed assuming the inert gas flow rate u _G.

Next, the liquid thickness δ of the raw material compound flowing through the donut-shaped portion is determined from the obtained liquid thickness δ ′ of the cylindrical model by the following procedure. δ ′ where u _S = u _G is obtained as δ, and u _S is obtained at the same time. That is, if u _S obtained by substituting δ in equation (1) using δ ′ obtained above and u _G assumed in obtaining δ ′ are equal, δ ′ is δ, and at the same time u _S is found. If u _S ≠ u _G , δ and u _S are obtained by changing the assumed value of u _G when obtaining δ ′ and performing the operation after the calculation of δ ′ again and recalculating.

[Calculation of SO ₃ gas flow rate] The flow rate of SO ₃ gas was calculated according to the following formula.

[0045]

(Equation 4)

[0046] Incidentally, u _t is SO ₃ gas flow rate [m / s],
V _G is SO ₃ gas flow rate [m ³ / s], d ₁ denotes the internal diameter [m] of the SO ₃ gas supply pipe.

The inert gas flow rate and SO determined above
_{3 The} gas flow rate [m / s] includes the conditions of temperature and pressure. In order to eliminate the influence, the flow rate shown in Table 1 [Nm
/ S] is calculated using the inert gas flow rate and the SO ₃ gas flow rate converted to [Nm ³ / s].

Comparative Example 1 Example 1 was repeated except that the reaction conditions were adjusted as shown in Table 1.
A sulfation reaction was carried out in the same manner as in the above to obtain a sulfated oxide. Table 1 shows the results.

Examples 4 to 7 As a starting compound, an alkyl ether (molecular weight: 280) was used in which 2 moles of ethylene oxide were added to an alcohol obtained by mixing lauryl alcohol and myristyl alcohol at a ratio of 75:25 (weight ratio) with ethylene oxide in a conventional manner. Also, as a reactor,
48 reaction tubes (reactor tube inner diameter (D): 16 mmφ, SO
₃ the inner diameter of the gas supply pipe (d _1): 11.1mm, an outer diameter of SO ₃ gas supply tube (d _2): 14.1mm, length: 5 m)
Was used.

A raw material compound, SO ₃ gas and an inert gas were continuously supplied to the reactor from the respective supply ports into the reaction tube, and a sulfation reaction was performed in the reaction tube. As for the flow rate of the raw material compound, the immersion length flow rate [= raw material flow rate / (π × reactor tube inner diameter (D))] is 100 kg / m · Hr, and other conditions are shown in Table 1. And a sulfation reaction was performed. The obtained sulfate is Na
After neutralization with an OH aqueous solution, the hue was measured in the same manner as in Example 1. Table 1 shows the results. A product having a hue of 12 or less is regarded as a pass product.

Examples 8 to 10 The same alkyl ethers as in Examples 4 to 7 were used as starting compounds. As a reaction apparatus, one reaction tube as shown in FIG. 1 (reactor tube inner diameter (D): 28 mmφ, reaction tube length: 7 m, SO ₃ gas supply tube inner diameter (d ₁ ): 2)
2 mm, outer diameter of SO ₃ gas supply pipe (d ₂ ): 25 mm)
Was used.

A raw material compound, SO ₃ gas and an inert gas were continuously supplied to the reactor from the respective supply ports into the reaction tube to perform a sulfation reaction in the reaction tube. As for the flow rate of the raw material compound, the immersion length flow rate [= raw material flow rate / (π × reactor tube inner diameter (D))] is 230 kg / m · Hr, and other conditions are shown in Table 1. And a sulfation reaction was performed. The obtained sulfate is Na
After neutralization with an OH aqueous solution, the hue was measured in the same manner as in Example 1. Table 1 shows the results. A product having a hue of 12 or less is regarded as a pass product.

Comparative Examples 2 and 3 Example 4 was repeated except that the reaction conditions were adjusted as shown in Table 1.
A sulfation reaction was carried out in the same manner as described above, and the hue of the obtained neutralized product of the sulfate was measured. Table 1 shows the results.

[0054]

[Table 1]

According to Table 1, the sulfates obtained in Examples 1 to 10 have an inert gas / SO ₃ gas flow ratio and a flow speed ratio in the range of 0.01 to 1.8 and 0.1 to 1. By adjusting to the range of 2, the flow rate ratio, one or both of the flow velocity ratio is significantly improved hue than the sulfate obtained in Comparative Examples 1 to 3 was adjusted out of the above range. Understand.

[0056]

By using the production method of the present invention,
The effect is obtained that a sulfate having significantly improved hue can be obtained at low cost.

[Brief description of the drawings]

FIG. 1 is a schematic explanatory view showing one embodiment of a sulfation reaction apparatus used in the present invention.

FIG. 2 is a schematic explanatory view showing one embodiment of a structure of each supply port of a raw material compound, an inert gas, and an SO ₃ gas in the sulfation reaction apparatus shown in FIG.

[Explanation of symbols]

1 sulfation reactor 2 starting compound feed port 3 inert gas supply port 4 SO ₃ gas feed port 5 reactor 6 cooling device 7 the gas-liquid separator (cyclone)

──────────────────────────────────────────────────続 き Continuation of the front page (51) Int.Cl. ⁷ Identification symbol FI // C11D 1/16 C11D 1/16 (56) References JP-A-49-24915 (JP, A) JP-A-49-70925 (JP, A) JP 51-17538 (JP, B2) (58) Fields investigated (Int. Cl. ⁷ , DB name) C07C 303/06 C07B 45/02 C07C 303/24 C07C 305/04 C07C 305 / 10 C11D 1/16

Claims (1)

(57) [Claims] 1. A compound which reacts with SO ₃ gas to give a sulfur oxide (hereinafter referred to as “raw material compound”) is supplied while flowing down the inner wall of a reaction tube to form a thin film of the raw material compound on the inner wall of the reaction tube. , thin film and SO ₃ in the SO ₃ gas and an inert gas into the reaction tube, an inert gas starting compound
A method for producing a sulfated product supplied to flow between a gas flow and a flow rate ratio of 0.01 to 1.8 to SO ₃ gas and a flow rate ratio of 0.1 to 1.2. To supply an inert gas as described above.