JPS60169436A - Quickly soluble furamic acid composition - Google Patents

Abstract

PURPOSE:To provide the titled composition soluble rapidly in water without causing the clouding of the solution, miscible with pefumery without emitting ill odor, and utilizable as a component of detergent, deodorizer, bath liquid, etc. for home use, by coating the surface of fumaric acid with a specific water-soluble polymeric compound. CONSTITUTION:Fumaric acid is coated with a water-soluble polymeric compound consisting of the homopolymer or copolymer of the monomer of formula I (R1 and R2 are H or COOX2 provided that both R1 and R2 are not COOX2 at the same time; R3 is H or methyl; X1 and X2 are alkali metal) and/or formula II(A1 is H or methyl; A2 is acid ester group of COOY; Y is 1-8C alkyl or 2-5C monohydroxyalkyl). The composition is preferably incorporated further with a condensed phosphoric acid salt (e.g. sodium tripolyphosphate) to prevent the generation of ill odor and stabilize the perfumery. The amount of the salt is 0.01- 2wt% in terms of phosphorus based on the fumaric acid composition.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to fumaric acid compositions that dissolve rapidly without causing cloudiness. To be more specific, the present invention provides that by coating the surface of 7-maric acid with a specific water-soluble polymer compound, it can be dissolved quickly without causing cloudiness, and even when mixed with fragrances, etc., there is almost no occurrence of off-odor. The present invention relates to fast-dissolving fumaric acid compositions that do not contain any of the following.

Fumaric acid is an inexpensive organic carboxylic acid that is expected to be used as an ingredient in household detergents, deodorizers, bath salts, and other products. However, compared to other organic carboxylic acids such as cono-phosphoric acid, malic acid, citric acid, and tartaric acid, which have similar properties, fumaric acid is hydrophobic, so its dissolution rate in water is extremely low, and it may cause problems. Due to its low apparent density, it floats on the water surface, which is an inconvenience in actual use.

Therefore, various attempts have been made to improve these drawbacks of fumaric acid. A method has been proposed for coating a maltotextrin containing . However, fatty acid esters have various drawbacks, such as a tendency to foam when dissolved in water, a decrease in solubility due to oral changes, the generation of precipitates and floating substances, and furthermore, when mixed with fragrances, they emit a strange odor. On the other hand, the maltofuxtrin compositions that have been proposed to solve these drawbacks are not sufficient in terms of providing rapid solubility. When the surface of fumaric acid particles is coated with saccharides, the compound itself is hydrophobic, and in order to increase the surface area of the fumaric acid particles, it is necessary to reduce the particle size as much as possible. However, if the particle size is small, fumaric acid tends to float, making the dissolution operation difficult.

The present invention provides a composition for improving these drawbacks. That is, the present invention can be specified as follows.

(1) Fumaric acid with an average molecular weight of 300 to 50,00
The following general formula CI) and/or (I
Fast-soluble fumaric acid group +21, characterized in that it is coated with a water-soluble polymer compound such as a homopolymer or copolymer of the monomer represented by t). Convert to phosphorus and get 0.
1. A fast-dissolving fumaric acid composition comprising: 01-2% by weight.

The present invention will be explained in more detail. The 7-maric acid used in the present invention has a particle size of 30 to 200 mesh, which is obtained by the usual method for producing 7-maric acid. Also, the water-soluble polymer compound used in the present invention.

It is preferable that the average molecular weight is in the range of 300 to so, ooo, preferably 500 to 30,000, and that has high wetting power and dispersing power. Alkali metal salts of saturated carboxylic acids, more specifically alkali metal salts of polymers or copolymers of acrylic acid, methacrylic acid, maleic acid, fumaric acid, especially sodium salts and potassium salts and/or the above-mentioned El) Monomers such as methyl, ethyl, butyl, and 2-ethylhexyl esters of acrylic acid and 2-hydroxyethyl and 2-ethyl acrylic acids and methacrylic acids.
Examples include polymers or copolymers of hydroxypropyl esters.

These water-soluble polymer compounds are coated on the fumaric acid composition in an amount of 0.1 to 50 weight percent, preferably 1 to 30 weight percent.

In addition, examples of condensed phosphates suitably used in the present invention include sodium tripolyphosphate and sodium tetrapolyphosphate, which have low hygroscopicity, but sodium tripolyphosphate is usually used, and is It is coated in a range of 0.0, 1 to 2% by weight, giving good results.

Coating with condensed phosphates is important because when fast-dissolving fumaric acid compositions are used in household detergents, deodorizers, bath salts, etc., they are often mixed with fragrances, in which case the fragrances often contain off-flavors. This is because it has been found to have a remarkable effect on preventing the occurrence of odors and stabilizing fragrances. The amount of condensed phosphate added to the fumaric acid composition is within the above range as phosphorus, but if it is less than 0.01%, the effect of the addition will be weak, and it is also necessary to maintain the stability of the fragrance. The following coating is sufficient; however, increasing the amount added is not desirable as it may cause contamination of wastewater when used in household detergents, deodorizers, bath additives, etc.

Furthermore, it goes without saying that the condensed phosphate salt does not need to be added for applications that do not use fragrances.

The coating method of the fumaric acid composition according to the present invention may be either a spraying method or a dipping method, and a spraying method is preferably used.Specific examples are as follows:〇Jacketed kneader
Alternatively, charge fumaric acid in the range of 30 to 200 mesh into a V-type mixer, and while stirring and mixing while heating at 50 to 130°C, mix the above-mentioned specific water-soluble polymer compound 5 to
A method is used in which a mixed aqueous solution of 40% by weight and sodium tripolyphosphate of 0.1-10% by weight is sprayed to uniformly coat the surface while evaporating water. The spray nozzle used in the present invention may be either a pressurized type or a two-fluid type,
Preferably, a two-fluid nozzle using air is suitably used. In addition, in order to uniformly coat the surface of the fumaric acid particles, the relationship between the spray speed and the rate of water evaporation from the coated fumaric acid surface is important. Due to the viscosity of the polymeric compound, agglomeration occurs between the fumaric acid particles, and if the rate of water evaporation becomes rapid, the particle surface will not become smooth and a uniformly coated product cannot be obtained. Therefore, in order to have a smooth and uniform coating on the surface of the finished product and to have a uniform particle size distribution, the fumaric acid surface temperature should be kept in the range of 50 to 130°C, preferably 60 to 130°C.
It is important to keep the surface moist during coating at a temperature of 10°C.

In order to remove the 7-malic acid composition thus prepared, it was pulverized and classified, and its performance was evaluated by the solubility test as described below.

300 m/ of 40°C water in a 300 m/beaker! 0.51 of the fumaric acid composition is added to water that is stirred at 25 Or, p, m in a star 2-, and the time until complete dissolution is measured. In addition, by observing the hydrophilicity to water and judging the appearance, those that dissolve immediately were rated as ◎, those that partially floated and dissolved in water while being dispersed were rated as 0, and those where most of the particles floated as X.

Examples and comparative examples are shown below.

Example 1 An inverted conical blender with a maximum diameter of 1.000 m and a height of 1,100 m and equipped with a jacket and a screw type stirrer had a particle size in the range of 60 to 200 mesh, a ratio of 95, and a bulk density of 0.
5+ was added to fumaric acid 60 of 71f/Cc, and while heating the fumaric acid surface temperature to 90 to 100°C by passing water vapor at 5 h/cm2 into the jacket, the average was sprayed from the top of the blender using a pneumatic two-fluid spray nozzle. Molecular weight 4,
An aqueous solution containing 30% by weight of sodium polyacrylate and 1.0% by weight of sodium tripolyphosphate of 61%
The fumaric acid composition crystals were coated by spraying at a rate of 1 hour for 5 hours, and then heated and dried for 1 hour to obtain fumaric acid composition crystals with a moisture content of 0.5 weight coefficient and a particle size ranging from 10 to 32 meshes of 85 qb1 and a force density of 0.78 r/cc. Got 9 for 69.5. The crystals were crushed and classified, and a 32-mesh pass product was subjected to a solubility test. In addition, sodium polyacrylate in the crystals was analyzed by gel permeation chromatography, and the phosphorus content was determined by JIS K01.
It was determined by the 01 method. The results are shown in Table 1.

Example 2 A ribbon-type kneader with a jacketed internal volume of 3 tons was equipped with 60
~200 mesh range is 95%, bulk density 0.71
A pneumatic two-fluid spray nozzle was applied to the upper part of the kneader while heating the fumaric acid surface temperature to 85 to 90°C by passing 2 Ky/cm'' of water vapor into the jacket. using, average molecular weight s, oo
It was coated with an aqueous solution containing 30% sodium polyacrylate by weight at a rate of 35g1/hr for 8 hours, and then heated and dried for 2 hours to obtain a water content of 0.2% by weight and a particle size of 20~
The range of 100 mesh is 90, the bulk density is 0.75f/
CL fumaric acid composition crystals of 1.08 Ko were obtained.

The crystals were crushed and classified, and a solubility test was conducted on a 48-menshu bath product. In addition, sodium polyacrylate in the crystals was analyzed by gel permeation chromatography, and the phosphorus content was determined by J
It was quantified by IS K 0101 method. The results are shown in Table 1.

Example 3 The same procedure as in Example 2 was carried out except that an aqueous solution containing 30 parts by weight of sodium polyacrylate and 3 parts by weight of sodium tripolyphosphate with an average molecular weight of 500 was used as the water-soluble polymer compound. The results are shown in Table 1.

Examples 4 to 7 As water-soluble polymer compounds, polysodium methacrylate (average molecular weight 13.000), acrylic WR/maleic acid (mole ratio 70:30) copolymer sodium salt (average molecular weight 3.0 G O) , acrylic acid/2-hydroxyethyl acrylate (molar ratio g4:14) copolymer)
The same procedure as in Example 3 was conducted except that IJium salt (average molecular weight: i15.o00) and sodium polymaleate (average molecular weight: 700) were used. The results are shown in Table 1.

Comparative Example l A jacketed ribbon-type kneader with an internal volume of 3 tons was charged with 200 kg of fumaric acid pulverized by pulverization class, and mixed with separately prepared monoester-containing [90% sucrose stearate]. While stirring and mixing 4.69 g of the ethanol solution in Section 10, the mixture was sprayed from the upper part of the kneader using a pneumatic two-fluid spray nozzle.
Ethanol was evaporated to dryness at 5°C, and the dried product was crushed and classified to obtain a 200-mesh pass product. The loading rate of sucrose ester was 0.4 qb. The results of the solubility test are shown in Table 1.

Comparative Example 2 Into a jacketed ribbon m kneader with an inner volume of 3 tons, 300 mesh bath of fumaric acid iKo, which had been granulated by crushing and classification, and 5 of maltodextrin were charged and mixed by stirring. Next, 1,500 ta of water was added and immersion treatment was carried out at room temperature under stirring. Then filter, dry, crush, and classify 30
I got 0 mesh pass items.

The compatibility of maltodextrin was 5 parts by weight.The results of the solubility test are shown in Table 1.

Claims (1)

[Scope of Claims] (I) Fumaric acid having an average molecular weight of 300 to
1. A rapidly soluble hexamaric acid composition coated with a water-soluble polymer compound such as a homopolymer or copolymer of the monomer shown below. f21 A fast-dissolving fumaric acid composition, characterized in that it contains a condensed phosphate in the composition according to claim 111 in an amount of 0.01 to 2 weight percent in terms of phosphorus.