JPS6058938A - Aluminum behenate and production thereof - Google Patents

Abstract

NEW MATERIAL:The aluminum behenate having the diffraction peaks at the d- value of 4.15, 4.70, 3.86 and 3.71 by X ray diffraction analysis and absorption peaks of carboxylic acid at 1,580cm<-1> by infrared spectrophotometry. USE:Useful as a lubricant, especially for plastics, etc. PREPARATION:An emulsion of behenic acid is produced at >=80 deg.C in the presence of an electrolyte such as sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, etc. The amount of the behenic acid is preferably to give a concentration of <=10wt%. The emulsion is added with an alkali metal hydroxide, e.g. sodium hydroxide, etc., and then with a soluble aluminum salt, and the product is filtered and dried to obtain the objective compound. The bulk density of the titled compound is 0.4-2.0g/cm<3>.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to aluminum behenate, a novel compound useful as a lubricant, particularly as a lubricant for plastics, and a method for producing the same.

This new compound aluminum behenate has a d value of 415.470 in X-ray diffraction analysis, a diffraction peak at filtration 86 and loa 1, and a diffraction peak of 1580 cm' in infrared spectroscopy analysis.
It has an absorption peak of carboxylic acid salt.

Regarding the method for producing aluminum behenate of the present invention, in the presence of an electrolyte substance such as sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, etc.
Produced by forming an emulsion of behenic acid at C or above, adding an alkali metal hydroxide, such as sodium hydroxide, potassium hydroxide, then adding a soluble aluminum salt, and filtering and drying the product. can do.

It is preferable that the electrolyte be added to the hot water in an amount of 1 to 60% by weight based on the amount of behenic acid. Generally, if this is below the lower limit, the product becomes lumpy when the emulsion of behenic acid is reacted with the 11 alkali gold hydroxides described below, making it impossible to carry out a uniform and sufficient reaction. If it exceeds a little less than 21, the electrolyte substance remains in the final product, aluminum behenate, and the purity of the product decreases, which is undesirable.

However, the reason for using an electrolyte is that, as mentioned above, in the absence of an electrolyte, when an emulsion of behenic acid is reacted with an alkali metal hydroxide, the product becomes lumpy and cannot be produced evenly and sufficiently. Due to the inability to carry out the reaction.

Therefore, the addition of electrolyte material is extremely important in the present invention.

In addition, electrolyte substances are not only added to cold water in advance, but also
It may be used by adding it to hot water.

Next, the aqueous solution in which the electrolyte substance has been decomposed is heated to 80°C or higher.
At temperatures below 0°C, the amount of alkali metal behenic acid salt produced by the reaction between behenic acid and an alkali metal hydroxide decreases and precipitates, and the emulsion itself becomes unstable and hydroxide The reaction with the compound does not proceed and a mixture of behenic acid and alkali metal behenic acid is formed, which inhibits the next reaction with a soluble aluminum salt, resulting in a significant decrease in the reaction rate of a/reminium behenic acid.

Now, behenic acid is then added to the heated water and stirred to form an emulsion. It should be noted that adding an emulsifier at this time is not preferable as it reduces the purity of aluminum behenate, but depending on the intended use of aluminum behenate,
This does not preclude adding an emulsifier.

It is preferable to add behenic acid at a concentration of 10% or less to form an emulsion.

That is, when the concentration exceeds IO@%, it is difficult to uniformly react with the alkali metal hydroxide, which results in a problem of lowering the yield of aluminum behenate.

After forming an emulsion by sufficient stirring, an alkali metal hydroxide such as sodium hydroxide or potassium hydroxide is added. The proportion of sodium hydroxide or potassium hydroxide used must be stoichiometrically equivalent or more than that of behenic acid, but the proportion of alkali metal hydroxide that greatly exceeds the equivalent Addition is not preferable because the Pal of the solution increases too much. It is generally desirable to have an excess of about 2% over the chemical equivalent to behenic acid.

During this time, what about the reaction solution? Of course, the relationship is maintained at 80° or more.

When behenic acid and thorium hydroxide or potassium hydroxide react sufficiently, the emulsion collapses and becomes a homogeneous solution.

Next, a soluble aluminum salt is added as a powder or as an aqueous solution, but it is generally preferable to use the aqueous solution in order to conduct a homogeneous reaction.

Soluble aluminum salts include aluminum sulfate,
Examples include aluminum chloride, aluminum nitrate, basic aluminum sulfate, basic aluminum chloride, etc.
Among these, aluminum sulfate is preferably used.

The ratio of soluble aluminum salt used is behenic acid/
The ratio of A/', On of soluble aluminum salt is 30 (
molar ratio) is suitable.

That is, if it deviates from this range, it will not be possible to produce aluminum behenate at the desired reaction rate, and especially if it falls below this stoichiometric ratio, hydroxides of soluble aluminum salts will be produced, resulting in the formation of behenic acid. This is not preferable because the purity of aluminum decreases.

The aluminum behenate obtained after a sufficient reaction between the alkali metal salt of behenic acid and the soluble aluminum salt is water-inert and has tE! It is obtained as a suspension of fine and homogeneous particles. This is filtered and dried using any drying means such as spray drying, vacuum drying, and freeze drying.
The drying temperature is preferably 100°C or less.

The thus obtained aluminum behenic acid powder is a fine and homogeneous katsura powder, and in its X-ray diffraction analysis, it has a d value of 415.470, a characteristic diffraction peak at 86 and 71, and I 580 in infrared spectroscopy
It has an absorption peak of carboxylate at cm'.

Moreover, the bulk specific gravity is in the range of 04 to 0.297 cd, and this compound is a novel compound useful as a lubricant, especially as a lubricant for plastics and the like.

Now, to further explain the physical properties and manufacturing method of aluminum behenate of the present invention, specific examples will be given.

Specific Example 1 5y of l-IJium chloride was dissolved in 101 of water, and after the solution was heated to 82°C, flaky behenic acid (manufactured by Shin Nihon Rika) 4002 was added and vigorously stirred.
By maintaining the liquid temperature at 82°C without continuing vigorous stirring, the behenic acid melts and forms an emulsion. While stirring and heating were continued, a 48% aqueous sodium hydride solution was gradually added, and a total of 989 g of the solution was added.

Subsequently, aluminum chloride solution (2% as A40+)
After slightly slowing down the stirring, 2000 f of the mixture (containing) was gradually added. At this time, the solution gradually becomes cloudy. The pH of the solution after the addition of aluminum chloride was 68.

The product was filtered and washed and left to dry at 100°C to obtain aluminum behenate powder. The bulk specific gravity of this material was 0.31 y/at, and its X-ray diffraction analysis results are shown in FIG. 1, and the infrared spectroscopy results are shown in FIG.

For comparison, the results of X-ray diffraction and infrared spectroscopy of behenic acid are shown in FIGS. 2 and 4, respectively.

To explain the present invention in more detail, the terms X-ray diffraction, infrared spectroscopy, and bulk density used in the present invention will be explained.

1) X-ray diffraction The X-ray diffractometer used was a Rigaku +11.1'IIR Geiger Flex RAD-Engineering A model. The measurement was carried out by a powder method, and nickel was used for the X-ray source and CuKn ray filter.

Note that the sample may be used as is, but the diffraction peak may become broad depending on the manufacturing conditions, so in such cases, use a sample that has been melted at 160°C and gradually cooled. This makes it possible to obtain relatively sharp diffraction peaks.

2) Infrared spectroscopic analysis The infrared spectroscopic analyzer was manufactured by JASCO Corporation (Yoseikaku R-810).
The measurements were carried out using the KBr tablet method.

2) Weigh 1 oy of the sample in a glass test tube with bulk specific gravity inner diameter 0 bleaching, volume 10 ome, and test tube with J1 sled and fall height 10 500 on the same evening. After pinging, measure the volume of the sample. The bulk specific gravity was determined by the following formula.

Now, as is clear from Figure 1, aluminum behenate has a d value of 415.470.386 in the X-ray diffraction peak.
It has a diffraction peak at 371, especially at 4.70 ('2θ=1
89°), and a completely new peak at 86 (29=23.0°). In contrast, the X-ray diffraction peak of behenic acid (Figure 2) does not have this peak.

The infrared spectroscopic analysis peaks of aluminum matabehenate and behenic acid are shown in Figures 6 and 4, respectively, and as can be seen from these figures, the +700 Cnl observed in behenic acid
-' carboxylic acid peak is rarely seen in aluminum behenate, instead +5800711-
”, a carboxylate peak is seen. This also indicates that the product is an aluminum behenate compound.

The reaction rate of behenic acid to aluminum behenate, that is, the yield of aluminum behenate, is approximately 90% or higher, but the method for measuring this is to extract the reactant with a mixed solvent of benzele water, Measured by removing reaction aluminum gel, etc. Furthermore, since other impurities can be removed by this method, it can also be applied to purification of aluminum behenate.

What about aluminum nabehenate like this? It can be used not only as a lubricant for fJII, especially Glastysox, but also as an additive for paints, greases, cosmetics, waterproofing agents, and the like.

In addition, depending on these uses, this behenine aluminum may be further pulverized and used.

The present invention will be further explained below with reference to Examples.

Example 1 Thorium sulfate (anhydrous) 258F was dissolved in water+02, and after the solution was heated to 90°C, flaky behenic acid (New Japan Rika iM) 9502 was added and vigorously stirred. By maintaining the liquid temperature at 90°C and continuing vigorous stirring, it was confirmed that behenic acid was in an emulsion state, and 1565 of 10% potassium hydroxide solution was added.
y was added gradually. After the addition of the potassium hydroxide solution, continue with the aluminum sulfate solution (5% as A40+).
1,900y of (containing) was gradually added.

At this time, the solution gradually becomes cloudy. After filtering and washing the product, it was vacuum dried.

For comparison, 10 J of water was crystallized at 90"C, then flakes of behenic acid 9502 were added, followed by vigorous stirring. No electrolyte was added at this time. The liquid temperature was raised to 90°C. Confirm that the behenic acid has become an emulsion, and add 10% potassium hydroxide solution.
When 565f was gradually added, the solution became a sticky, non-uniform white mass. Subsequently, 1900y of aluminum sulfate solution (AI!, containing 5% as 0+) was gradually added. As the addition progressed, the viscosity of the solution decreased slightly, but it became quite heterogeneous.

The product was filtered and dried in the same manner as above to obtain a white powder.

Table 1 shows the analysis results of the above-mentioned products of the present invention and comparative products.

Example 2 Water 5/? Dissolve 113y of sulfur chloride in the mixture, heat the solution to 85°C, and then dissolve the flaky behenic acid.
Add 507 and mix vigorously until 17.

The liquid temperature was maintained at 85° C., and after confirming that behenic acid had become an emulsion-like rα, 540y of 10% thorium hydroxide solution was gradually added.

Subsequently, aluminum sulfate solution i (A/!, 8 as 0.
563y (containing 0%) was added to obtain a white fli0 product.

This was filtered and washed, and then left to dry at 100°C.

Also, for comparison, chloride in water 51) IJum 11
After dissolving 6y and heating the liquid temperature to 85°C, flaky behenic acid 10 (109) was added and vigorously stirred.The liquid temperature was maintained at 85°C until the behenic acid was in an emulsion state. After confirming that the solution had become toned, 10% thorium hydroxide solution (12OL12) was added to the solution, but the solution became highly viscous and became non-uniformly cloudy.Subsequently, aluminum sulfate solution (Al to 1250 g of white 1iKf product (containing 80% as r) was added. After filtering and washing this, leave it at +00'C and dry it! I did this.

Table 2 shows the analysis results of the above-mentioned products of the present invention and comparative products.

Table 2 Example 6 Water 10 J Add 50 y of behenic acid in the form of flakes, heat to liquid temperature of 82°C, and then chloride) IJum 0
．． Added 5y. After the behenic acid became a dissolved layer and became an emulsion, 10% thorium hydroxide solution 59y was gradually added. Subsequently, aluminum chloride solution (AZ
962y (containing 52% as +O+) was added to obtain a white product.

After washing it thoroughly, use a spray dryer (inlet temperature 250℃,
Drying was carried out at an outlet temperature of +05'C).

Dry Me was pulverized using a Lamicron mill (manufactured by Honkawa Micron Co., Ltd.). The bulk specific gravity of this product was 022-te, and the yield of aluminum behenate was 9q4%.

[Brief explanation of the drawing]

Figure 1 is an X-ray diffraction diagram of aluminum behenate;
The figure shows an X-ray diffraction diagram of behenic acid, Figure 3 shows an infrared spectroscopic analysis of aluminum habehenate, and Figure 4 shows an infrared spectroscopic analysis of behenic acid. Ya3@CIl! −“ ′ outside IZ

Claims (1)

[Claims] (1) In X-ray diffraction analysis, the d value is 415.470.38.
Aluminum behenate has a diffraction peak at 6.371 and an absorption peak of carboxylate at +580 cm-' in infrared spectroscopy. (2) Aluminum behenate according to claim 1141, having a bulk specific gravity of 04 to 0.2117 cd. (3) A behenic acid emulsion consisting of forming an emulsion of behenic acid at 80° C. or above in the presence of a 1M delyte, adding an alkali metal hydroxide, and then adding a soluble aluminum salt. Method for producing aluminum acid. +4+ Emulsion concentration of behenic acid 10% by weight
A manufacturing method according to claim 6 below. (5) The manufacturing method according to claim 6, characterized in that the electrolyte substance is previously present in the warm water in a range of 1 to 30% by weight based on the amount of behenic acid.