JPS5930897A - Manufacture of granular cation surfactant - 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 cationic surfactant particles.

When washing clothes at home to make them softer,
Normally, after washing with detergent, the detergent components are rinsed off with a large amount of water, and then a fabric softener mainly composed of a cationic surfactant such as a quaternary ammonium salt is added for treatment. . However, performing washing and softening separately requires extra time and effort, and therefore there is a need for a detergent that combines washing and softening.

Di-long-chain alkyl type quaternary ammonium salts that are poorly water-soluble have excellent softening effects, but it has been difficult to obtain sufficient effects when used with detergents. Household detergents generally have anionic surfactants or nonionic surfactants as their main ingredients, and the quaternary ammonium salts added during washing are attacked by the detergent component surfactants before being adsorbed onto the fabric being washed. The ionicity may be lost or the dispersion may be stabilized, making it difficult to be adsorbed onto the cloth to be washed, and as a result, a sufficient softening effect cannot be exhibited.

Therefore, in order to add flexibility to clothing by adding quaternary ammonium salts during washing, quaternary ammonium salts are granulated or coated with inorganic salts or organic dispersants, and quaternary ammonium salts are added during washing. Methods for controlling dispersion have been proposed (Japanese Patent Publication No. 36-8927, U.S. Patent No. 4,073,7315, Japanese Patent Application Laid-open No. 153-41).
312, JP-A-49-98403). However, although these methods are somewhat effective when washing conditions such as water temperature and washing time are constant,
In reality, the washing conditions are often different each time, such as the water temperature being different in summer and winter, and the quaternary ammonium salt may be dispersed too quickly or, conversely, may not be sufficiently effective. Often there isn't.

The present inventors have conducted extensive research on the adsorption mechanism of quaternary ammonium salts on clothing when laundered with detergents and softeners, and have found that quaternary ammonium salts of di-long chain alkyls are There are two types of crystals: vertical crystals that grow in the direction of the molecular chain and horizontal crystals that grow in the direction of the molecular chain. They discovered that the water content of quaternary ammonium salts is specifically and uniformly adsorbed to the surface of clothing fibers. Furthermore, as a result of repeated research on a method to efficiently produce oblong crystals, they found that the water content in quaternary ammonium salts was It was discovered that there was no significant influence on the shape, and based on this knowledge, the present invention was completed.

That is, in the method for producing a particulate cationic surfactant of the present invention, a solid cationic surfactant represented by the general formula (I) and having a moisture content of 1.0% by weight is pulverized while removing moisture. It is characterized in that the content is adjusted to i,o~5.0% by weight and granulated.

(In the formula, R8 and R1 represent an alkyl group having 14 to 20 carbon atoms, and R1 and R4 are an alkyl group having 1 to 4 carbon atoms, a benzyl group, a human tetraxyalkyl group having 2 to 4 carbon atoms, or a polyoxyalkylene group. , and X represents halogen, CH@S 04 t C! 1) Distearyldimethylammonium salt (2)
Distearylbenzylmethylammonium salt (3) Distearylmethylhydroxyethylammonium salt (4) Distearyldihydroxyethylammonium salt (5) Hydrogenated beef tallow alkyldimethylammonium salt (6) Shisui /#-mualkyldimethylammonium salt Counter ions include chloride, butemide, etc. O NG Quaternary ammonium salt has a water content of 1.0 before crushing.
OL, which must be less than 0% by weight
If it is more than that, the desired crystal form cannot be obtained.

The crushing is performed so that the water content in the granulated material after crushing is 1.0 to 5.0% by weight. If this value is less than 1.0% by weight, unstable vertically elongated crystals will result, and a sufficient softening effect will not be obtained. Moreover, if it exceeds 5.0% by weight, it becomes a hydrated gel and is easily dispersed and solubilized by anionic or nonionic surfactants in detergents, making it impossible to obtain a sufficient softening effect.

The crushing can be carried out using a normal crusher, and for efficient crushing, it is preferable that the environmental temperature is as low as possible, for example, 20C or lower. Since it is necessary to absorb moisture at the same time as crushing, it is necessary to carry out the process in an atmosphere with some degree of humidity. It is sufficient to perform this under atmospheric conditions, and the humidity in the atmosphere is at a normal level, e.g. 40-70%R.
H, and there is no need to use special humidification or dry air. The particle size of the crushed material is 1 from the viewpoint of use in combination with detergent.
A value of about mm or less is appropriate.

According to the method of the present invention, oblong crystals of a di-long-chain alkyl quaternary ammonium salt are obtained. Di-long chain quaternary ammonium salt has a dissociable quaternary nitrogen as a polar group, two of the four groups bonded to this are hydrophobic groups with a long chain alkyl structure, and the molecular shape is elongated. It is asymmetrical. Therefore, it forms molecular crystals similar to general surfactants or fats and oils such as triglycerides. Crystals of these substances grow in the direction of their molecular chains and in the direction in which the molecular chains are arranged in parallel.

In the X-ray diffraction pattern of such a crystal, diffraction lines originating from repeating units in the molecular chain direction are obtained in the long surface region, and diffraction lines originating from repeating units in the cross section of the molecular chain are obtained in the short surface region.

The same goes for di-long chain quaternary ammonium salts; by specifying the degree of crystal growth in the direction of the molecular chain and the degree of crystal growth in the cross-sectional direction of the molecular chain, quaternary ammonium salt particles with excellent flexibility imparting effects can be obtained. It will be done. The degree of directionality of this crystal growth is measured by xm diffraction, and the ratio (4)/(B ), and those whose long chain alkyl group mainly has 18 carbon atoms are (A) / (B
) ratio is 2.0 or less, preferably 1.3 or less, and 1. A mixture of alkyl groups with 16 and 18 carbon atoms, such as C
16/C48=l/9~9/1 (5)/(B
) ratio is 1.5 or less, preferably 1.1 or less. According to the method of the present invention as described above, such a crystalline quaternary ammonium salt can be obtained.

EXAMPLE Distearyldimethylammonium chloride (Cxa
/exe = 97/3) 110-120c
After dehydration under reduced pressure in a molten state, the mixture was left to cool to room temperature under reduced pressure and solidified. Moisture content was measured immediately after cooling and solidification.

The solid material was cooled in the atmosphere to near OC using dry ice, crushed using a mallet, and then sieved to obtain particles with a particle size of 250 μm or less.

Grinding time: 2-3 minutes Grinding temperature: Approximately oC (temperature 22-24C) Grinding humidity: 50
~60%RH Moisture content and (A)/03) ratio after crushing and sieving were measured.

(1) Measurement method for (A) / (B) Width: 35g, height: 50mm, thickness 1.7mm from the top of the glass plate.
A double-sided tape of 20 ya x 15 mm was pasted underneath with a gap of 5 m, and the dialkyl ammonium salt particles were uniformly dropped onto the double-sided tape to adhere to the entire surface of the double-sided tape.

Using this, an X-ray diffraction spectrum was obtained under the following conditions.

X-ray: CuK (1 ray (λ = 1.5418X) filter: Nl slit; 1st; 1°

3rd; 1'X20 hegemonic tube voltage and current j30KV, 1 (lfflA time constant: 1 second angular velocity: 2.0°/min From the spectrum (4) and (B) (A+2.6°, B
! The peak at 18.8') was read as the peak height from the baseline, and this ratio was defined as (4)/(B).

Table 1

Claims (1)

[Claims] 1. General formula (1) (wherein R8 and R2 represent an alkyl group having 14 to 20 carbon atoms, and R and D represent an alkyl group having 1 to 4 carbon atoms,
(represents a ndyl group, a human tetraxyalkyl group having 2 to 4 carbon atoms, or a dilyoxyalkylene group, and X is halogen, CH, 80,, C, H, 80, or CH, -Q-S
O, is shown. ), and the water content is less than 1.0% by weight. While grinding, the water content is reduced to 1.0 to 5
．． A method for producing a powdery cationic surfactant, which comprises adjusting the weight to 0 weight and granulating it.