JPS6042219B2 - Aluminum behenate and its manufacturing method - Google Patents

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.

In X-ray diffraction analysis, this new compound aluminum behenate has d values of 4.15, 4.70), 3.8(), 3.
It has a diffraction peak at 71 and 15 in infrared spectroscopy.
It has a carboxylic acid salt absorption peak at 80 cm-1.

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 a temperature above °C, adding an alkali metal hydroxide, such as sodium hydroxide, potassium hydroxide, then adding a soluble aluminum salt, filtering and drying the product. be able to.

It is preferable that the electrolyte be added to the hot water in an amount of 1 to 3% by weight based on the amount of behenic acid.

Generally, if the value is below the lower limit, the product becomes lumpy when the behenic acid emulsion is reacted with the alkali metal hydroxide described below, making it impossible to carry out a uniform and sufficient reaction. Moreover, when the upper limit is exceeded, the electrolyte substance remains in the final product, aluminum behenate, and the purity of the product decreases, which is not preferable. 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 a uniform and sufficient reaction cannot be achieved. due to inability to do so. Therefore, adding electrolyte material is extremely important in the present invention.

Further, the electrolyte substance may be used not only by adding it to cold water in advance, but also by adding it to hot water.

Next, the aqueous solution in which the electrolyte substance is dissolved is heated to 80'C or higher.The reason for heating the solution to 80'C or higher is that the water temperature is
At temperatures below 0C, the amount of alkali metal behenic acid salt produced by the reaction between behenic acid and an alkali metal hydroxide, dissolved in water, decreases and precipitates, and the emulsion itself becomes unstable, causing a reaction with the hydroxide. does not proceed, resulting in a mixture of behenic acid and alkali metal behenate, and the subsequent reaction with soluble aluminum salt is also inhibited, resulting in a significant decrease in the reaction rate of aluminum behenate. Now,
Behenic acid is then added to the warm water and stirred to form an emulsion. At this time, addition of an emulsifier is not preferable because it reduces the purity of aluminum behenate, but this does not prevent the addition of an emulsifier depending on the intended use of aluminum behenate. It is preferable to add behenic acid at a concentration of 1% by volume or less to form an emulsion.

That is, when the concentration exceeds 10% by weight, 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 the equivalent to behenic acid, but the addition of alkali metal hydroxide that greatly exceeds the equivalent is not preferable because the [·H of the solution increases too much. It is generally desirable to have an excess of about 2% over the chemical equivalent to behenic acid. It goes without saying that during this time the temperature of the reaction solution is maintained at 80'C or higher.

When behenic acid and sodium 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/
A suitable ratio of Al2O3 in the soluble aluminum salt is 3.0 (molar ratio).

That is, if it deviates from this range, it will not be possible to obtain aluminum behenate at the desired reaction rate, and especially if it falls below this stoichiometric ratio, hydroxide of soluble aluminum salt will be produced, and the purity of aluminum behenate will decrease. This is less preferable than a decrease in

Aluminum behenate obtained after sufficiently reacting an alkali metal salt of behenic acid with a soluble aluminum salt is water-insoluble and is obtained as a suspension of fine and homogeneous particles.

This is filtered and dried using any drying method such as spray drying, vacuum drying, and freeze drying. Drying temperature is product temperature 100
'C or less is preferable. The aluminum behenate thus obtained is a fine and homogeneous powder, and its X-ray diffraction analysis shows that the d values are 4.15, 4.70, 3.86,
It has a unique diffraction peak at 3.71, and an absorption peak of the carbocepta salt at 1580α-1 in infrared spectroscopy.

Moreover, its bulk specific gravity is in the range of 0.4 to 0.2 y/Cd, and it is a novel compound useful as a lubricant, especially as a lubricant for plastics and the like.

Now, to further explain the substance contained in aluminum behenate of the present invention and the manufacturing method, specific examples will be given. -Specific Example 1 5 g of sodium chloride was dissolved in 10 g of water, and after the solution was heated to 28° C., 400 g of flaky behenic acid (manufactured by Shin Nihon Rika) was added and vigorously stirred.

By maintaining the liquid temperature at 82° C. while continuing vigorous stirring, behenic acid melts and forms an emulsion. While stirring and heating were continued, 48% sodium hydroxide solution was gradually added, totaling 98 q. Subsequently, 2000 y of aluminum chloride solution (containing 2% Al2O3) was gradually added after the stirring was slightly relaxed. At this time, the solution gradually becomes cloudy. The pH of the solution after the addition of aluminum chloride was 6.8. The product was filter washed and left to dry at 100°C to obtain aluminum behenate powder. The bulk specific gravity of this material is 0.31 y/d, and the results of X-ray diffraction analysis of this material are
In addition, the results of infrared spectroscopic analysis 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.

1X-ray Diffraction The X-ray diffraction apparatus used was Geigerflex RAD-1A manufactured by Rigaku Denki Co., Ltd.

The measurement was carried out by the powder method, and nickel was used for the X-ray source and the CLlKα 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, it is better to use a sample that has been melted at 130°C and gradually cooled. ,
A relatively sharp diffraction peak can be obtained.

2 Infrared spectroscopic analysis The infrared spectroscopic analyzer is 1R-81 manufactured by JASCO Corporation.
The measurement was carried out by the KBr tablet method using 0.

3 Bulk specific gravity Weigh 10 d of sample into a glass test tube with internal diameter 30 ordinal diameter and volume 10 mt, tap it 500 times at a drop height of 10 wr1, measure the volume of the sample, and measure bulk specific gravity using the following formula. did.

- - Oshina? ■■α1 Bulk specific gravity (y/・I) full, A, sample.

Volume (.,) Now, as is clear from Figure 1, aluminum behenate has a d value of 4.15, 4.15 in the X-ray diffraction peak.
It has diffraction peaks at 7013.86 and 3.71, especially at 4
．． 70 (2θ=18.93), 3.86 (20=23.
0), a completely new peak can be seen. In contrast, the X-ray diffraction peak of behenic acid (Figure 2) does not have this peak. In addition, the infrared spectroscopic analysis peaks of aluminum behenate and behenic acid are shown in Figures 3 and 4, respectively.
As you can see from these figures, 170 found in behenic acid
The carboxylic acid peak at 0 cm-1 is hardly seen in aluminum behenate, but instead at 1580 cm-1.
The peak of carphonate can be seen at 1. This also indicates that the product is an aluminum behenate compound. Reaction rate of aluminum behenate of behenic acid,
That is, the yield of aluminum behenate is approximately 90%.
Although obtained above, the measurement method is to extract the reactant with a mixed solvent of benzene water and remove residual aluminum gel and the like.

Furthermore, since other impurities can be removed by this method, it can also be applied to purification of aluminum behenate. Such aluminum behenate is not only used as a lubricant, especially for plastics, but also
Some can also be used as additives in paints, greases, cosmetics, waterproofing agents, etc.

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

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

Example 1 238V of sodium sulfate (anhydrous) was dissolved in 10e of water, the temperature of the solution was heated to 90°C, and then flakes of behenic acid (
950 Da (manufactured by Shin Nippon Rika) 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 1565y, a 10% potassium hydroxide solution, was gradually added. After the addition of potassium hydroxide solution, 19% of aluminum sulfate solution (containing 5% Al2O3) was added.
00q was added gradually. At this time, the solution gradually becomes cloudy. After washing the product, it was vacuum dried.
For comparison, 10f of water was heated to 90'C, then 950y of flaky behenic acid was added and vigorously stirred. No electrolyte material was added at this time. Set the liquid temperature to 90
After confirming that behenic acid has become an emulsion, add 1565y of 10% potassium hydroxide solution.
was gradually added, and the solution turned into a sticky, non-uniform white mass. Subsequently, aluminum sulfate solution (Al
1900q of 5% (as 2O3) was gradually added. With each addition, the viscosity of the solution decreased slightly, but it became quite heterogeneous. Product as above? The mixture was filtered and dried 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 Dissolve 113y of sodium chloride in 5f of water and raise the liquid temperature to 85.
After warming to 0.degree. C., 450 y of flaky behenic acid was added and vigorously stirred.

The liquid temperature was maintained at 85° C., and after confirming that behenic acid was in an emulsion state, 10% sodium hydroxide solution 540y was gradually added. Subsequently, 563 da of aluminum sulfate solution (Al containing 8.0% as O3) was added to obtain a cloudy product. After washing it at 100℃
It was allowed to stand and dry. For comparison, 113y of sodium chloride was dissolved in 5' of water, and after the solution was heated to 85°C, 1000y of flaky behenic acid was added and vigorously stirred. The liquid temperature was maintained at 85°C, and after confirming that behenic acid was in an emulsion state, 1200 y of 10% sodium hydroxide solution was gradually added, but the solution became highly viscous and became non-uniform and cloudy. Ta. Subsequently, aluminum sulfate solution (8.0% as Al2O3
1250y of (containing) was added to obtain a cloudy white product. this? After excessive washing, it was allowed to stand and dry at 100°C. Table 2 shows the analysis results of the above-mentioned products of the present invention and comparative products.

Example 3 50 f of flaky behenic acid was added to 10 e of water, and after the liquid temperature was heated to 87 C, 0.5 da of sodium chloride was added.

After behenic acid melts and becomes an emulsion, 10
59V of % sodium hydroxide solution was added slowly. Subsequently, aluminum chloride solution (5.2% as Al2O3)
96.2y of (containing) was added to obtain a white product. After this was washed, it was dried in a spray dryer (inlet temperature: 250°C, outlet temperature: 105°C).

The dried product was pulverized using a micron mill (manufactured by Hosokawa Micron Co., Ltd.). The bulk specific gravity of this product was 0.22y/Clt, and the yield of aluminum behenate was 99.4%.

[Brief explanation of the drawing]

Figure 1 is an X-ray diffraction diagram of aluminum behenate;
The figure is an X-ray diffraction diagram of behenic acid, and Figure 3 is an infrared spectroscopy diagram of aluminum behenate. Figure 4 is an infrared spectroscopy diagram of behenic acid.

Claims (1)

[Claims] 1. In X-ray diffraction analysis, d values of 4.15, 4.70, 3
．． Aluminum behenate has a diffraction peak at 86, 3.71 and an absorption peak of carboxylate at 1580 cm^-^1 in infrared spectroscopy. 2. Aluminum behenate according to claim 1, which has a bulk specific gravity of 0.4 to 0.2 g/cm^2. 3. A method for producing aluminum behenate, which comprises forming an emulsion of behenic acid at 80° C. or higher in the presence of an electrolyte, adding an alkali metal hydroxide, and then adding a soluble aluminum salt. 4. The manufacturing method according to claim 3, wherein the emulsion concentration of behenic acid is 10% by weight or less. 5 1 to 30% by weight of electrolyte substance based on the amount of behenic acid
3. The manufacturing method according to claim 3, characterized in that the above-mentioned amount is preliminarily present in hot water.