JPS598800A - Granulation of cationic 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 granulating powder of di-long chain alkyl quaternary ammonium salt (hereinafter referred to as dialkyl quaternary salt). This invention relates to a method for producing a granulated product with good dispersibility.

Dialkyl quaternary salts are usually produced in liquid form, but powder form is often more convenient depending on the application. For example, when using it as a fabric softener, it is possible to obtain the same effect as a commercially available liquid fabric softener by adding just a small amount of Sial/Vru quaternary salt powder to the washing and rinsing bath. However, they are rarely manufactured because they generate dust or are inconvenient to handle.

Therefore, re-granulation may be considered, but the conventional granulation method using a nonionic surfactant has the disadvantage that water dispersibility after storage becomes poor. This is because dialkyl quaternary salts are sensitive to humidity, and under high humidity conditions, they absorb a large amount of water and their transition point drops rapidly, but when the humidity drops again, they quickly dehumidify. It is based. That is, the particles of the dialkyl quaternary salt absorb moisture under high humidity and high humidity conditions, and as the transition point lowers, the molten dialkyl quaternary salt particles coalesce and solidify as they dehydrate.

Generally, in order to granulate such a hygroscopic substance, there is a method of mixing it with an inorganic powder that can adsorb water as crystal water, such as anhydrous sulfuric acid, anhydrous magnesium sulfate, etc. The amount of water that can be retained as water is limited, and once taken in, it will never be released again at room temperature, so storage cannot prevent particles from coalescing without losing their waterproofing effect.

Furthermore, when stored under high temperature and high humidity conditions, water condensed between granulated particles causes interparticle adhesion. Water-soluble inorganic substances partially dissolve in condensed water, recrystallize as the condensed water evaporates,
It also has the disadvantage that it causes bonds between particles and promotes solidification.

Even in the method of mixing water and Is-soluble inorganic powder, substances such as calcium carbonate and aluminum hydroxide have a strong affinity for water, so water easily penetrates, and substances such as bentonite prevent moisture absorption. The pores between particles became larger, making it easier for water to pass through, resulting in poor water dispersibility after storage and also making it difficult to prevent assimilation.

As a result of intensive investigation into a method for granulating dialkyl quaternary salt powder that has good dispersibility in water and does not cause moisture absorption and solidification even during storage, the present inventors have found that silica powder with an average primary particle size of 0.1 μm or less has a particularly high affinity for dialkyl quaternary salts.
．． ．． Furthermore, since the particles are fine particles, they are layered uniformly and densely, and it has been found that it is possible to prevent the dialkyl quaternary salt particles from coming into contact with each other in the granulated particles during dinner.

In addition, since the above-mentioned silica absorbs moisture and hardly changes its shape even after layering, the gaps between the silica particles do not become too thick due to moisture adsorption, and the swelling and softening caused by the absorption of moisture by dialkyl quaternary salts is suppressed. I discovered that the effect was clearly large.

Furthermore, in addition to the effects of this silica powder, a nonionic surfactant or a nonionic surfactant aqueous solution is added to fill the gaps between silica particles, and at the same time prevents the dialkyl quaternary salt particles from absorbing moisture. Zeolite powder with an average particle size of 01 to 10μ is adsorbed around the granulated particles to prevent shielding between the granulated particles, increase the water absorption capacity under high humidity, and improve water absorption under low humidity. It has been found that the above objects of the present invention can be achieved by facilitating moistening.

That is, the cationic surfactant granulation method of the present invention is as follows:
This was achieved by skillfully combining the above series of findings, and for 100 parts of di-long chain alkyl quaternary anthonium salt powder with an average particle size of 150μ or less, the average primary particle size was 0
．． Mixing 10 to 30 parts of fine silica powder of 1μ or less,
Next, 20 to 80 parts by weight of a nonionic surfactant or a nonionic surfactant aqueous solution is added to granulate the particles, and 30 to 80 parts by weight of zeolite powder with an average primary particle size of 0.1 to 10 μm is added to the granulated particles. It is characterized in that it is granulated by adding a certain amount.

The dialkyl quaternary salt powder used in the present invention has an average particle size of 150 μm or less. In addition, as a representative example of dialkyl quaternary salt, the following general formula (1
) is expressed.

(In the formula, RI r R2 represents a C3, to C16 argyl group, g, l R4 represents a C, -C2 alkyl group, benzyl group, C2 to C4 hydroxyalkyl group, or polyoxyalkylene group, represents halogen, CH, So, , C2H, So4 or cu8-@)-so. ) Specific examples of dialkyl quaternary salts represented by the above general formula (I) include (1) distearyldimethylammonium salt (2)
Dihydrogenated beef tallow alkyldimethylammonium bungalow (3)
Dihydrogenated beef tallow alkylbenzylmethylammonium salt (4
) Distearylmethylbenzylammonium salt (5
) Distearylmethylhydroxyethylammonium salt (6) Distearylmethylhydroxypropylammonium salt (7) Distearyldihydroxyethylammonium salt, etc. can be exemplified, and counter ions include chloride and bromide.

In the present invention, the fine silica powder added to and mixed with the dialkyl quaternary salt is selected from the viewpoint that it can uniformly and densely cover the particle optical surface of the dialkyl quaternary salt in a small amount.
Those having an average primary particle size of 0.1 μm or less are used, preferably 0.05 μm or less. The silica is added in an amount of 10 to 30 parts by weight, preferably 15 to 30 M, per 100 parts of the dialkyl quaternary salt, and mixed well.

If the number of Usuka lids is less than 10 times, the coating will not be sufficient, and the dialkyl quaternary salt will aggregate and coalesce, resulting in poor water dispersibility. In addition, if the amount added exceeds 30 portions,
Not only is the effect of improving water dispersibility saturated and no further improvement can be expected, but the content of dialkyl quaternary salt in the finished product decreases, making it undesirable as a commercial product.

The nonionic surfactant used in the present invention is preferably one that has a high solubility in water, that is, one that is easily soluble. Examples of such nonionic surfactants include polyoxyyenalene alkylphenyl ethers (with 2 carbon atoms in the argyl group) having an ethylene oxide average addition mole of 4 to 30 moles, Q/number (expressed as 6~lS)
, polyoxyethylene alkyl ether (number of carbon atoms in the alkyl group: 10 to 24), or polyoxyethylene polyoxypropylene alkyl phenyl ether (number of carbon atoms in the alkyl group = 6 to 18), polyoxyethylene polyoxypropylene alkyl ether ( Carbon % number of alkyl group: 1o to 24). Further, specific examples include polyoxyethylene (p=8) dodecyl ether, polyoxyethylene (i21O) dodecyl ether, polyoxyethylene (p=28) nonylphenyl ether, polyoxyethylene (p= 10) Nonylphenyl ether, polyoxene ethylene (ili=20)
Halumithyl ether, polyoxyethylene (p=4) polyoxypropylene (p=6) dotesyl ether, polyoxyethylene (p=8) polyoxypropylene ('
1i=10 ) tetradecyl ether, polyoxyethylene (p=5) polyoxypropylene (p=5) nonylphenyl ether, and the like. In addition, the nonionic surfactant may be used as an aqueous solution, but in this case, in order not to lower the melting point of the dialkyl quaternary salt, the amount of water is 30 parts by weight per 10 parts by weight of the nonionic surfactant. The following is preferable. The nonionic surfactant or its aqueous solution is added in an amount of 26 to 80 parts by weight, preferably 30 to 70 parts by weight, per 1 oz part of dialkyl quaternary salt. The nonionic surfactant or its aqueous solution acts as a binder, and if the amount of the surfactant is less than 20 parts by weight, the granulation properties will deteriorate.

Moreover, if it exceeds 80 layers, the granulated particles become sticky and tend to solidify. The nonionic surfactant used in the present invention exhibits liquid to fluid-solid properties under granulation conditions, and in the case of a liquid to fluid, it can be used as it is or as an aqueous solution, and in the case of a solid, it can be used as it is or as an aqueous solution. is preferably used in the presence of moisture within the above range.

The zeolite conveniently used in the present invention has an average primary particle size of 0.1 to 10 μm, preferably 0.1 μm, so that it can adsorb moisture under high humidity and quickly release moisture under low humidity. A powder of 5 to 5 microns is used. The amount of zeolite added is 30 to 1 part per 100N parts of dialkyl quaternary salt.
The amount is 50"fL parts, preferably 50 to 120 parts. If this amount is less than 30 parts, the improvement in solidification of the particles is not sufficient, while on the other hand, even if it exceeds 150 parts, there is no effect on improving assimilation. Not only can no more be expected, but the concentration of dialkyl quaternary salt in the granulated product becomes low, making it undesirable as a commercial product.

According to the method of the present invention, dialkyl 4M salt and silica are uniformly mixed, a nonionic surfactant is added to partially granulate the mixture, and then zeolite is added to further granulate the particles into larger particles. The dialkyl quaternary salt is 25 to 6
A granulated product containing 0% M% can be obtained. Moreover, the average particle diameter of the obtained granules is preferably 300 to SOOμ, more preferably 400 to 600μ.

The granulation of the present invention can be carried out using a conventional granulator under conventional conditions.

As described in detail above, according to the present invention, a shell efficiently coated with silica having high affinity for dialkyl quaternary salts,
By granulating a nonionic surfactant with a similar high affinity as a binder, the dialkyl quaternary salt is shielded from water, and even if it absorbs to some extent and swells and flows, its high affinity allows it to remain close to the exposed surface. Furthermore, adsorption of the above-mentioned compound occurs, preventing aggregation and coalescence of the swollen particles, and improving water dispersibility.

In addition, zeolite prevents granulated particles from sticking together and suppresses solidification.

As is clear from the above theory ψJ and the later examples,
According to the present invention, the following effects are mainly obtained.

(1) Moisture absorption and assimilation of the dialkyl quaternary salt is prevented, and the water dispersibility after storage is also good.

(2) Due to the high concentration of dialkyl quaternary salt in the granules and proper dispersion into primary particles in water, it is possible to obtain excellent cationic surfactants such as surfactants, softeners, and antistatic agents. It will be done.

(3) Assimilation after storage can be prevented even if it is blended into granular detergents containing other surfactants as main ingredients.

EXAMPLE A 100-weight portion of powder of dialkyl (hard heifer J11t) dimethylanthonium chloride (A) with an average particle size of 80 μm was placed in a rotating drum, and a predetermined tht (parts by weight) of the inorganic substance tB) shown in Table 1 was added. and mixed. Then, similarly, a nonionic surfactant or a nonionic surfactant water bath solution (C
') was added for granulation, and then an inorganic substance (D) was added to complete the granulation. The granulated product thus obtained was heated at 20°
C-60%RH (15 hours) and 45℃-80φRH (9
Stored under recycling conditions (hours). After storage, the water dispersibility and moisture absorption solidification properties were measured as shown below, and the results were shown to the first person.

(1) 10 g of a water-dispersible sample was added to tap water 5009 at 15°C, stirred for 10 minutes, and the remaining liquid was passed through the surface of 24 meshes. Furthermore, after washing by passing tap water in step 11, drying the sieve,
Increase in weight of the sieve before and after the test Particle residue on the sieve (chi)
was determined and evaluated using the following criteria.

○: Sieve residue 5 or less △: Decorative residue 5-15% ×: Sieve residue 15 or more (2) Moisture absorption and assimilation evaluation criteria ○: No solidification ×: Solidification As is clear from Table 1 , Experiment 1 according to the present invention
, 2 had satisfactory water dispersibility and moisture absorption solidification before and after storage.

In addition, the detailed contents of the compounds in Table 1 and the abbreviation Kurami are listed after the table.

Liponox NCH; polyoxyethylene nonylphenol ether (EOi=8) Liponox NCG; polyoxyethylene nonylphenol ether (EOi=7) Liponox NCI; polyoxyethylene nonylphenol ether (EO=9) pga12oo; polyethylene glycol (average molecule i200) PEG $400; Polyethylene glycol (average molecular 1i400) Silica; Tokuyama Soda Tokusil N, average primary particle size 0.02μ Zeolite; Mizusawa Kagaku Zilton B, average primary particle size 0.8μ Calcium carbonate: Average particle size: 20μ Glauber's salt: Average particle size: 60μ

Claims (1)

[Claims] 1. lθ~30 parts by weight of fine silica powder with an average primary particle size of 0.1 μ or less is mixed with 10 weight parts of di-long chain alkyl quaternary ammonium salt powder with an average particle size of 150 μ or less, and then Add 20 to 80 parts of a nonionic surfactant or an aqueous solution of a nonionic surfactant to granulate the particles, and then add 30 to 150 parts of zeolite powder with an average primary particle size of 0.1 to 10 μm to the granulated particles. A method for granulating a cationic surfactant with good water dispersibility, which is characterized by granulating it in water.