JPS6257639A - Production of grain of cationic surface active agent - Google Patents

Abstract

PURPOSE:To lend substantial resilience to a cotton fabric by adding and mixing the chloride of an alkalimetal or alkaline earth metal at 1-20 pts.wt. to 100 pts.wt. long-chain di-alkyl quaternary ammonium salt. CONSTITUTION:The chloride of the alkalimetal or alkaline earth metal is added at 1-20 pts.wt. and 20-80 pts.wt. to 100 pts.wt. powder of long-chain di-alkyl quaternary ammonium salt and thereafter the mixture is grnaulated by a rotary drum, etc. The embodiment of the quaternary ammonium salt includes a di- stearyl dimethyl ammonium salt, etc. which have perferably <=105mum average primary grain size. NaCl, KCl, MgCl, etc. are adequate as the chloride of the alkalimetal or alkaline earth metal. A nonionic surface active agent, polyhydric alcohol, etc. are used as a binder.

Description

[Detailed description of the invention] skill set The present invention relates to a method for granulating a cationic surfactant.

Cationic surfactants have the effect of imparting flexibility to fibers such as clothing, and among them, di-long-chain alkyl quaternary ammonium salts are widely used.

In consideration of prevention of dust generation, ease of handling, powder blending into granular detergents, etc., di-long chain alkyl quaternary ammonium salts are granulated using a binder.

JP-A-59-8800 and JP-A-59-216
Publication No. 619 proposes a method in which a di-long-chain alkyl quaternary ammonium salt is granulated with silica powder using a nonionic surfactant, and zeolite or calcium carbonate powder is further added and granulated. This prevents moisture absorption and assimilation, making it possible to obtain granules with excellent water dispersibility.

However, if this granule is added during rinsing, it can effectively impart flexibility, but if it is blended in advance into an anionic detergent or added to a washing liquid together with a detergent, When used in the presence of a synthetic detergent, the softening effect deteriorates, and this is particularly noticeable in the case of cotton fabrics.

The present invention provides a method for producing di-long-chain alkyl quaternary ammonium salt granules that can impart sufficient flexibility to cotton fabric even when used in the presence of an anionic detergent. It is something to do.

In the method for producing cationic surfactant granules of the present invention, when di-long chain alkyl quaternary ammonium salt powder is granulated using a binder, chlorination of an alkali metal or alkaline earth metal is carried out. di-long-chain alkyl quaternary ammonium salt 10
It is characterized by adding 1 to 20 parts by weight relative to 0 parts by weight.

The present invention will be explained in more detail below.

Representative examples of di-long chain alkyl ammonium salts used in the present invention include the following.

(In the formula, R,, R,, R,, R4, and X are as follows.

R1,R,: Alkyl group of C2-C2G R,,R,
: C□-C4 alkyl group, benzyl group, 02-C4
hydroxyalkyl group or polyoxyalkylene group x: halogen, CH, So, , C, H, SO, or C
H,<Esu)-3o, ) Specific examples of the di-long chain alkyl quaternary ammonium salt represented by the above general formula (I) include (1) distearyl dimethyl ammonium salt (2) dihydrogenated beef tallow alkyl dimethyl Ammonium salt (3) Dihydrogenated tallow alkylmethylbenzylammonium salt (4) Distearylmethylbenzylammonium salt (5) Distearylmethylhydroxyethylammonium salt (6) Distearylmethylhydroxypropylammonium salt (7) Distearyldihydroxyethyl Examples include ammonium salts, and counter ions include chloride and bromide.

In the present invention, when such a di-long-chain alkyl quaternary ammonium salt is granulated using a binder, an alkali metal or alkaline earth metal chloride is added. As the alkali metal or alkaline earth metal chloride, those with high water solubility are preferable, such as N a C1.

Examples include K Cl , M g C1, and Ca C1□.

These chlorides are dilong-chain alkyl quaternary ammonium salts 1
1 to 20 parts by weight, or 1 to 1 part by weight
0 parts by weight is added. If the amount added is less than 1 part by weight, the flexibility improvement effect will not be sufficient, while if it exceeds 20 parts by weight, hygroscopicity will increase.

It solidifies easily during storage.

The chloride may be added as a powder or dissolved in a binder or water. When added as a powder, it is preferably added to the quaternary ammonium salt before adding the binder. Furthermore, it can also be added by using as a raw material a quaternary ammonium salt that already contains the necessary amount of chloride.

A nonionic surfactant is used as a binder.

Polyhydric alcohol etc. are used.

The nonionic surfactant is preferably one that has high solubility in water, that is, one that is easily soluble. Examples of such nonionic surfactants include the average number of added moles of ethylene oxide (hereinafter referred to as ethylene oxide).

Polyoxyethylene alkyl phenyl ether (expressed as EOp) with 4 to 30 moles of polyoxyethylene alkylphenyl ether (expressed as EOp)
18), polyoxyethylene alkyl ether (number of carbon atoms in alkyl group: lO~24), or EO macro=2
~15, average number of added moles of polyoxypropylene (PO
i5) polyoxyethylene polyoxypropylene alkylphenyl ether having 2 to 15 (carbon number of alkyl group = 6 to 18), EO75 = 2 to 15. POp=2～
There are 15 polyoxyethylene polyoxypropylene alkyl ethers (carbon number of alkyl group: 10 to 24). Specific examples include polyoxyethylene ([:0i5=8) dodecyl ether, polyoxyethylene (EOp=10) dodecyl ether, and polyoxyethylene (EOp=28) nonylphenyl ether.

Polyoxyethylene (EO macro = 10) nonylphenyl ether, polyoxyethylene (EO75 = 20) palmityl ether, polyoxyethylene ([EOi5 =
4) Polyoxypropylene (POi5=6) Dodecyl ethyl, polyoxyethylene (EOp=8) Polyoxypropylene (POβ=10) Tetradecyl ether, polyoxyethylene (EOi5=5) Polyoxypropylene (POi5=5) Examples include nonylphenyl ether.

The polyhydric alcohol is preferably trivalent or higher, and specific examples include glycerin, sorbitol, diglycerin ((C)I20)ICIIOHCH,)zO), polyglycerin (dehydrated glycerin), mannitol,
Examples include water-soluble alcohols such as glucose.

Granulation can be carried out by adding chloride and a binder to quaternary ammonium salt powder and granulating it with a rotating drum or the like. The quaternary ammonium salt powder preferably has an average dimensional diameter of 150 μl or less. As the particle size increases, the amount of deposits on cloth after washing and rinsing tends to increase.

Binder is di-long chain alkyl quaternary ammonium salt 10
0 parts by weight, 20 to 80 parts by weight, preferably 30 parts by weight
~70 parts by weight is added. If the amount added is less than 20 parts by weight, granulation properties will deteriorate, while if it exceeds 80 parts by weight, the particles will become sticky and solidify easily.

Although the chloride and the binder can be used as an aqueous solution, it is preferable that the amount of water brought in by them is 25 parts by weight or less based on 100 parts by weight of the di-long-chain alkyl quaternary ammonium salt. If the water content becomes too large, the melting point of the quaternary ammonium salt will decrease, leading to deterioration of moisture absorption and solidification properties when used in powder blend with an anionic powdery detergent.

Note that water brought in as crystal water or bound water by an inorganic substance such as zeolite does not affect the melting point of the quaternary ammonium salt, and is therefore excluded from the above calculation of the amount of water.

During granulation, it is preferable to add an inorganic powder to further improve properties such as moisture absorption and solidification properties.
Fine silica powder, zeolite powder, and calcium carbonate powder shown in Japanese Patent No. 9-216619 are preferred.

The fine silica powder preferably has an average dimensional diameter of 0.1 μm or less so that it can be uniformly coated on the quaternary ammonium salt. The silica fine powder is preferably added in an amount of 10 to 30 parts by weight per 100 parts by weight of the quaternary ammonium salt. If the amount added is less than 10 parts by weight, coverage of the quaternary ammonium salt will be insufficient.

The appropriate zeolite powder has an average dimensional diameter of 0.1 to 10 μm or less so that it can adsorb moisture under high humidity and rapidly release moisture under low humidity. It is preferable to add 30 to 150 parts by weight of the zeolite powder and calcium carbonate powder to 100 parts by weight of the quaternary ammonium salt. If the amount added is less than 30 parts by weight, the solidification property will not be improved sufficiently.

It is desirable that these inorganic powders be granulated by adding and mixing fine silica powder to quaternary ammonium salt, then adding the binder of the present invention, and then re-granulating by adding zeolite powder or calcium carbonate powder. .

Examples of inorganic substances other than those mentioned above include water-insoluble inorganic substances such as alumina and titanium dioxide, and water-soluble inorganic salts such as sodium sulfate, sodium sulfite, magnesium sulfate, sodium carbonate, and sodium hydrogen carbonate.

The di-long-chain alkyl quaternary ammonium salt of the present invention is granulated to a size of about 100 to 1000 μm, although it depends on the form in which it is used.

The obtained di-long chain alkyl quaternary ammonium salted granules are as follows:
It can be used by pre-blending it into an anionic detergent, or it can be added separately during cleaning to impart flexibility.

According to the present invention, when granulating di-long-chain alkyl quaternary ammonium salt powder with a binder, by adding an alkali metal or alkaline earth metal chloride,
It is possible to obtain di-long chain alkyl quaternary ammonium salt granules that exhibit an excellent softening effect on cotton fabrics even when used in the presence of an anionic detergent.

100 parts by weight of dihydrogenated beef tallow alkyldimethylammonium chloride powder with an average primary particle size of 80 μm or less was placed in a rotating drum, and 20 parts by weight of fine silica powder with an average primary particle size of 0.2 μm was added. After mixing, the binder shown in Table 2 below is added and granulated. At this time, chloride is added according to the method below, and 70 parts by weight of zeolite with an average primary particle size of 2 μm is added to form a 4th grade zeolite. Ammonium salted granules were obtained. In addition, sample NQ13 in Table 1-2 had no chloride added, and sample Na14 had Na25o added instead of chloride.

Chloride A: After adding the binder, a 25% aqueous solution (40°C) of each chloride was added.

B: 5 parts by weight of chloride was added to the quaternary ammonium salt as a powder by the method of A, and the amount exceeding 5 parts by weight was added to the quaternary ammonium salt as a powder prior to the addition of silica powder.

C: Added after being dissolved in a sorbitol aqueous solution.

D = total amount was added to the quaternary ammonium salt as a powder prior to addition of silica powder.

E: A quaternary ammonium salt containing chloride was used in advance.

Using the granulated product, the flexibility to cotton cloth was determined by the following method, and the results are shown in Table 2 below.

Softness test for cotton fabric Method J (1) Cleaning method ■ Add the above granules to 40 g of anionic granular detergent having the composition shown below, and add di-long chain alkyl quaternary ammonium salt.
Add 0 g and mix well to make a mixed detergent.

(Left below) Table 1: Anionic granules “J group” Straight-chain alkylbenzenesulfonate sodium 18wt%
Zeolite 15wt%
Sodium silicate 10wt%
Soda carbonate 585% moisture 5wt% Glauber's salt Balance■ Pour 30 fl of 25°C water into a washing machine, add the above detergent mixture, and stir for 30 seconds.

■ Place 1.0 kg of cotton towel in the above washing bath and wash for 10 minutes.

■ After washing, dehydrate for 1 minute.

■ Repeat 3 minutes of rinsing and 1 minute of dehydration twice.

■ Repeat the operations from ■ to ■ above two more times for the same towel.

■ Air dry and use as a wiping cloth.

(2) The above operation is performed using an anionic detergent to which the di-long-chain alkyl quaternary ammonium salt granules are not added, and a blank is obtained.

(2) Judgment method: When di-long chain alkyl quaternary ammonium salt is added;
A pairwise comparison was made for the case without (blank), and scores were given according to the following criteria.

Obviously soft 2 points Slightly soft
Equivalent to 1 point blank
0 points This was done for 10 panelists, and the total score was taken as the flexibility for cotton fabric.

(Margin below)

Claims (1)

[Claims] 1. When granulating di-long-chain alkyl quaternary ammonium salt powder using a binder, add 1 part by weight of alkali metal or alkaline earth metal chloride to 100 parts by weight of di-long-chain alkyl quaternary ammonium salt. A method for producing a cationic surfactant granule, characterized in that ~20 parts by weight is added.