JPS598799A - Production of cationic surfactant powder - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a cationic surfactant, and more particularly, the present invention relates to a method for producing a cationic surfactant, and more specifically, a crystal-stabilized di-long-chain alkyl quaternary ammonium salt and an inorganic surfactant having a particularly remarkable affinity for the crystal-stabilized di-long-chain alkyl quaternary ammonium salt. The present invention relates to a method for producing a powder of a di-long-chain alkyl quaternary ammonium salt by combining it with a compound.

When crushing materials, a large amount of frictional heat is generated.

Substances with low melting points soften and become difficult to crush.

It is widely known that melting and adhesion may occur, eventually resulting in failure to fracture. The case of dichotai alkyl type quaternary ammonium salt is no exception; it causes softening and cracking, and it is difficult to crush it into powder, especially to finely powder it to 200 μm or less. Among the di-long-chain alkyl-type quaternary ammonium salts, di-hydrogenated beef tallow alkyl dimethyl ammonium salt, which is often used as a base material for fabric softeners, is a mixture of long-chain alkyl groups with mainly 16 and 18 carbon atoms (mixed axis). )
Compared to products with a single carbon number of 16 (cibal mityl dimethyl ammonium salt) and products with a single carbon number of 18 (distearyl dimethyl ammonium salt), it has a lower melting point and is easier to soften, making it extremely difficult to pulverize it by crushing. Met.

Methods for crushing di-long chain alkyl type 4#jt having a mixed axis, ammonium salt (hereinafter sometimes abbreviated as mixed axis quaternary ammonium salt) include cooling,
A method of adding inorganic powder is known. However, when cooling, it is necessary to lower the temperature to below 0°C, and in order to obtain a satisfactory yield, the temperature must be lowered even further, which is not only uneconomical but also impractical. . Furthermore, in the case of pulverization of organic compounds, there is a risk of dust explosion, and it is common sense to manufacture under a nitrogen seal, or there is a problem with the amount of cold air.

In the method of adding inorganic powder, the particles of the inorganic compound are embedded in the particles of the mixed shaft 4M ammonium salt using a crushing beam, that is, they become particle nuclei, so that crushing becomes possible. , the crushed particles also soften and adhere 91. It is difficult to expect stable production over a long period of time, and requires extreme cooling or a large amount of inorganic substances to prevent adhesion between particles.
The drawback was that a grade ammonium salt could not be obtained.

Furthermore, since organic compound crystals generally become harder as the water content is lowered, it is believed that extreme dehydration and solvent removal are required, and in practice, manufacturing methods that involve warping have been used. However, under such harsh conditions, the sample deteriorates and
In the case of mixed shaft quaternary ammonium salts, decomposition occurs, resulting in an increase in F),'-amines and deterioration in color tone, which has the disadvantage of seriously deteriorating the quality of the product.

On the other hand, crystals of mixed-axis quaternary ammonium salts produced by conventional methods are generally a mixture of anhydrous hexagonal, orthorhombic, and hydrated hexagonal crystals, but the proportions of the three vary greatly depending on the moisture content. , the proportion of anhydrous hexagonal crystals increases as the temperature approaches absolute dryness. However, this crystal form easily absorbs moisture;
Under normal humidity, it rapidly absorbs water and transforms into a viscous hydrated hexagonal crystal with a low melting point. Therefore, when such bone-dry mixed f14M ammonium salt is crushed, the particles begin to absorb moisture at the same time, and only the particle surface becomes a viscous hydrated hexagonal crystal, causing adhesion phenomenon and significantly reducing the crushing efficiency. let

The present inventors have developed a fine powder of a mixed shaft quaternary ammonium salt that is easily softened and difficult to be pulverized by crushing, and has a particle size of 200 mm.
As a result of intensive studies on a method for stably producing powder with a particle size of less than μ in good yield, we found that crystals of mixed-shaft quaternary ammonium salts are easy to crush within a specific range of water content of 1 to 4 f%.
We also found that there is a region rich in orthorhombic crystals that are stable against moisture. Furthermore, anhydrous sodium sulfate, anhydrous magnesium sulfate, and silica have very good affinity for the mixed-axis quaternary ammonium salt consisting of this crystalline form, and are efficiently and uniformly adsorbed onto the mixed-axis quaternary ammonium salt particle surface. Based on these findings, the present invention was completed.

That is, the cationic surfactant of the present invention has the following (&
) After the cationic surfactant represented by general formula (1) has a moisture content of 1 to 4 Mf%, (b) an inorganic compound selected from anhydrous sodium sulfate, anhydrous magnesium sulfate, and silica. The weight ratio of (a) cationic surfactant and (b) inorganic compound is (a)/(b)=
It is characterized by mixing and crushing within the range of 100/5 to 100/100.

(In the formula, R8 and R2 represent an alkyl group having 14 to 2 carbon atoms;
to the argyl group is within the range of 87/2 to 2/8, and R3 and R4 are an alkyl group having 1 to 4 carbon atoms, a benzyl group, a hydroxyalkyl group having 2 to 4 carbon atoms, or a polyoxyalkylene group and X is halogen; (a) the cationic surfactant used in the present invention, i.e., the di-long chain alkyl type quaternary ammonium salt having mixed chains, is
The moisture content is 1 to 4 mm%, preferably 1 to 3 mm%. When the water content is less than 1ml/t%, the proportion of mixed chain quaternary ammonium crystals is anhydrous hexagonal,
Adhesion occurs during crushing, or in some cases, fusion occurs, making it impossible to crush. The crystal hardness of the mixed chain quaternary ammonium salt also depends on the content of lower alcohols such as methanol, ethanol, and impropatol used as an electric medium during production. is preferable. Furthermore, the mixed chain quaternary ammonium salt of the present invention may contain an unreacted amine, a by-produced heptanoalkyl quaternary ammonium salt, or a long chain alcohol, which may improve crystal stability and Since it has an adverse effect on softness, it is usually less than 1011%, preferably less than 6% by weight.

Representative examples of the cationic surfactants of the present invention include:
Enjoy dihydrogenated beef tallow alkyldimethylammonium salt, dihydrogenated beef tallow alkylbenzylmethylammonium salt,
In addition, examples of counter ions include chloride and bromide.

(b) The inorganic compound used in the present invention is (a,
) The cationic surfactant, ie, the mixed-chain quaternary ammonium salt, must be able to prevent moisture absorption, have particularly strong affinity, and be able to be coated uniformly with a small amount. Specifically, it is a powder of an inorganic compound selected from anhydrous sulfuric acid, anhydrous magnesium sulfate, and silica, and from the viewpoint of uniform coating, one having an average particle size of 100 μm or less is preferable.

In the present invention, (b) the inorganic compound is 5 to 100% sodium bicarbonate, preferably 10% to the cationic surfactant (b).
~60 weight is attacked. If this value is less than 5 weight %, sufficient crushing cannot be carried out, and if it exceeds 100 weight %, the content of cationic surfactant in the obtained powder becomes small, which is not practical.

The crushing of the present invention can be carried out using a conventional crusher under conventional conditions. Further, fine powder having a predetermined particle size can be obtained by air classification.

As explained above, according to the present invention, the water content of the mixed chain quaternary ammonium salt is adjusted to improve the stability against moisture, and the quaternary salt is coated with an inorganic compound having high affinity for the salt. It is easily crushed by 200
It is possible to stably obtain a powder with a particle size of less than μ in a high yield, and the physical properties of the obtained powder are also good. In addition, the amount of air required for wind classification and cooling is small, which promises to reduce costs during powder production.

Example 1 Dimethyldihydrogenated beef tallow alkyldimethylammonium chloride (Alucard 2HT) produced by a conventional method was deelectrified under reduced pressure at 110°C to reduce the water content and lower alcohols to 14% as shown in Table 1. Thereafter, it was cooled to room temperature and crystallized. Next, this was coarsely crushed to an average particle size of 1+m, and then an inorganic compound was added thereto at the ratio shown in the first coating, and the mixture was crushed under the following conditions. The yields of the obtained powders of 100μ or less were compared, and the results are shown in the first coating.

Crusher: Fine Victory Mill FVP-I type (manufactured by Micron) K Lid: 'In? / Cooling lice temperature: 28°C Air classification: Average particle size: 100μ (Left below) As is clear from Table 1, Experiment 1i 1 according to the present invention
, 2 , and 3 , 1 with high yields exceeding 90%
Powder with a particle size of 00μ or less was stably obtained.

Moreover, the powder physical properties were also good.

Example 2 ACM pulperizer (fine micron casing) as a crusher
A powder was produced in exactly the same manner as in Example 1, except that the following was used, and the results are shown in Table 2.

(The following is a blank space) As is clear from Table 2, Experiments A8 and 9 according to the present invention
．． 100μ with flattening yield of over 90% only in the case of 10
The following powder was stably obtained. Moreover, the powder physical properties were also good.

Claims (1)

[Scope of Claims] 1. (a) General formula (I) (in the formula, s R1 and D represent an alkyl group having 14 to 20 carbon atoms, and k is an alkyl group having a prime number of 16 and a carbon number of 18
and the alkyl group is within the range of 8/2 to 2/8,
R3 and R4 represent an alkyl group having 1 to 4 carbon atoms, a benzyl group, a hydroxyalkyl group having 2 to 4 carbon atoms, or a polyoxyalkylene group, and X is halogen, CH,
SO4, C, H, SO4 or CHji◇)so. ) Adjust the moisture content of the cationic surfactant represented by 1 to 4% by weight, (b) anhydrous sulfur, (b) anhydrous sulfur, and (b) anhydrous sulfur.
Glaze or two or more branches, (,) cationic surfactant and fb
) The weight ratio of the inorganic compound is (al/(b)=100/
A method for producing a cationic surfactant powder comprising mixing and crushing within a range of 5 to IQO/100.