KR100436171B1 - Tablet detergent composition and method for preparing the same - Google Patents

Abstract

The present invention relates to a tablet laundry detergent composition and a method for producing the same, and more particularly, to a tablet laundry detergent composition and a method for producing the same, which disintegrate in a short time and have excellent solubility of particles after the disintegration.

The present invention for this purpose, in a tablet laundry detergent composition, a) 10 to 50 parts by weight of an alkali builder; b) an acid precursor material-containing liquid surfactant having a weight mixing ratio of 1: 5 to 5: 1; And ii) 5 to 40 parts by weight of a mixture of powdered surfactant; c) 3 to 10 parts by weight of nonionic surfactant; d) 5 to 30 parts by weight of surface modifier; e) 0.1 to 10 parts by weight of inorganic dissolution accelerator; f) 1 to 10 parts by weight of disintegrant; And g) a tablet laundry detergent composition comprising 3 to 20 parts by weight of a disintegration aid, and a method for preparing such a tablet laundry detergent.

The tablet-type laundry detergent of the present invention has a disintegration in the wash water within a short time, excellent in the solubility of the particles after the disintegration, the washing time is short, it is suitable for the washing conditions of our country using low-temperature wash water.

Description

Tablet type detergent composition and its manufacturing method {TABLET DETERGENT COMPOSITION AND METHOD FOR PREPARING THE SAME}

The present invention relates to a tablet laundry detergent composition and a method for producing the same, and more particularly, to a tablet laundry detergent composition and a method for producing the same, which disintegrate in a short time and have excellent solubility of particles after the disintegration.

Conventional laundry detergents are mainly in powder form, and dust is generated when they are used, and they are not easy to be hygienic because they are easy to get on hands, and there is an inconvenience of using a measuring container. In order to solve this problem, a method of preparing a tablet of a predetermined amount of laundry detergent powder has been developed. Such tablet-type laundry detergent is easy to handle, does not generate dust when used, does not get on the hands, there is an advantage that can prevent excessive use.

Such tablet-type laundry detergents have to dissolve quickly when they are put into the wash water to have an effect, and are prepared by tableting at a considerable pressure to prevent the tablets from breaking when transported and stored. However, if the pressure is excessive during tableting, the manufactured tablets are not easily collapsed. If the tablets are compressed at low pressure in order to facilitate the collapse of the tablets, they may be damaged during transportation and storage, resulting in a problem of lowering the value of the product.

In fact, British Patent Publication No. 2318575 A discloses a sodium acetate-trihydrate (sodiumacetate · 3H ₂ O) and sodium citrate dihydrate (sodium citrate · 3H ₂ O) in order to make the best degradable 7-50% by weight And a technique for producing a particle size of sodium acetate of 0.3 mm or more while containing 2 to 20% by weight of a water soluble binder. In addition, British Patent Publication No. 2320254 A uses a liquid phase having a viscosity of 1000 cps or less at room temperature in order to improve the disintegration force, so that the proportion of pores is 5% by weight or more, and sodium carbonate as a water-soluble binder. ), Sodium citrate and the like using 15 to 85% by weight.

However, the above production methods are low in surfactant content, suitable for washing conditions in Europe, containing bleach, and also suitable for washing machines in drum type in Europe. Low washing conditions have a problem that the manufactured tablet laundry detergent does not melt well.

On the other hand, Japanese Patent Application Laid-Open No. 9-87696 is a nonionic surfactant having 10 to 35% by weight of an alkyl ether (AE) having a melting point of 40 ° C. or less and a HLB of 9 to 16 and an oil absorption of 30 to 70 ml / 100g. A tablet nonionic detergent containing 3 to 10% by weight of montmorillonite, active bentonite in the form is disclosed. This detergent is characterized by minimizing the dissolution of non-ion, but due to the phenomenon that the non-ion is fused with the builder (builder) during compression, there is a problem that does not collapse when the tablet detergent is added to the water.

Therefore, it is necessary to develop a tablet-type detergent having excellent solubility of particles after disintegration and rapid disintegration in washing water.

Disclosure of Invention It is an object of the present invention to provide a tablet-type laundry detergent composition and a method for preparing the same, in which disintegration occurs in a wash water within a short time and excellent in solubility of particles after the disintegration in view of the problems of the prior art.

The present invention, in order to achieve the above object, in the laundry detergent composition,

a) 10 to 50 parts by weight of alkali builders;

b) the weight mixing ratio is from 1: 5 to 5: 1

Iii) a liquid surfactant containing an acid precursor material; And

Ii) powdered surfactants

5 to 40 parts by weight of a mixture of;

c) 3 to 10 parts by weight of nonionic surfactant;

d) 5 to 30 parts by weight of surface modifier;

e) 0.1 to 10 parts by weight of inorganic dissolution accelerator;

f) 1 to 10 parts by weight of disintegrant; And

g) 3 to 20 parts by weight of disintegration aids, if necessary

It provides a tablet laundry detergent composition comprising a.

In addition, the present invention provides a method for producing a tablet laundry detergent,

a) on the mixer

Iii) 10 to 50 parts by weight of a powdered alkali builder;

Ii) the weight mixing ratio is from 1: 5 to 5: 1

A) liquid precursor containing acid precursor material; And

B) powdered surfactants

5 to 40 parts by weight of a mixture of;

Iii) 3 to 10 parts by weight of nonionic surfactant;

Iii) 5 to 30 parts by weight of surface modifier; And

Iii) 0.1 to 10 parts by weight of inorganic dissolution accelerator

Injecting, mixing and assembling to prepare detergent particles; And

b) to a tablet press

In the detergent particles prepared in step a)

Iii) 1 to 10 parts by weight of disintegrant; And

Iii) 3 to 20 parts by weight of disintegration aids, if necessary

After adding by mixing, tableting to prepare a tablet detergent

It provides a method for producing a tablet-type laundry detergent comprising a.

Hereinafter, the present invention will be described in detail.

The inventors of the present invention mix and assemble a detergent composition comprising a liquid surfactant having a precursor and a powdered surfactant as in the above composition to prepare a tablet detergent, to prepare detergent particles, and then mix and tablet the disintegrant and tablet When the type laundry detergent was prepared, disintegration occurred in the wash water within a short time, and it was found that the dissolution of the particles after the disintegration was excellent and the present invention was completed.

The term "collapse" refers to a phenomenon in which a tablet of a laundry detergent is absorbed and broken in water, and the term "dissolve" means a phenomenon in which detergent particles disintegrated in water are easily dissolved and dissolved in water.

To this end, the present invention is to first put 10 to 50 parts by weight of a powdered alkali builder (mixer), such as a high speed rotary mixer (schugi mixer, or lodige mixer) and at the same time a liquid surfactant and an alpha olefin having an acid precursor 5 to 40 parts by weight of a powdery surfactant, such as a salt, is added at a weight ratio of 1/5 to 5/1. At the same time, 3 to 10 parts by weight of the nonionic surfactant, 5 to 30 parts by weight of the surface modifier, and 0.1 to 10 parts by weight of the inorganic dissolution accelerator are added to assemble the detergent particles.

When the ratio of the acid precursor and the alpha olefin exceeds 1/5, the content of the powdered surfactant is increased, so the fine powder is greatly increased and the fluidity is lowered. Since the amount of liquid is increased, the powder is sticky, so that the tableting is difficult to prepare, making it difficult to prepare a detergent.

When the nonionic surfactant is added in less than 3 parts by weight, the particles are not formed well, and when the nonionic surfactant is added in excess of 10 parts by weight, the powder becomes sticky.

In addition, when the surface modifier is used in less than 5 parts by weight of the fluidity of the particles is lowered, the powder becomes sticky and tableting is not good, and when used over 30 parts by weight, the powder content is increased, the fine powder is increased, the tableting is not good.

In addition, the inorganic dissolution accelerator is less than 0.1 parts by weight of the detergent particles are not dissolved well after the collapse of the tablet, when used over 10 parts by weight of the detergent particles are not formed well.

The detergent particles thus prepared exhibit an optimum particle size for preparing tablets when particles of 12 to 80 mesh size are produced in 80% by weight or more.

The alkali builder is used to enhance the washing power in addition to the surfactant, carbonates such as sodium carbonate, calcium carbonate, or sodium hydrogen carbonate; Silicates such as layered crystalline α-sodium silicate (Na ₂ SiO ₃ ), or β-sodium silicate (Na ₂ SiO ₃ ); Phosphates such as orthophosphoric acid, pyrophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid, or salts thereof; Phosphonates such as diethylenetriaminepentamethylenephosphonate, aminotrimethylenephosphonate, 1-hydroxyethylene, or 1-diphosphonate; Nitrilotriacetic acid or salts thereof; Ethylenediaminetetraacetic acid or salts thereof; Carboxymethyl cellulose, polyethylene glycol; Polyvinyl alcohol; Polyvinylpolydon; Polyacrylic acid or salts thereof; And maleic acid-vinyl ether copolymers, salts thereof, or sulfate salts thereof.

In addition, the liquid surfactant having the acid precursor may be selected from the group consisting of a linear alkylbenzene sulfonic acid represented by the following formula (1), and a fatty acid represented by the following formula (2).

[Formula 1]

In the formula (1), R is alkyl having 10 to 14 carbon atoms.

[Formula 2]

In the formula (2), R is alkyl having 14 to 16 carbon atoms.

In addition, the powdered surfactant may be selected from the group consisting of an alpha olefin sulfonate represented by the following formula (3), and an alkyl sulfonate represented by the following formula (4).

[Formula 3]

In the formula (3),

R is alkyl having 12 to 18 carbon atoms and n is an integer of 9 to 15.

[Formula 4]

In the formula (4), R is alkyl having 11 to 18 carbon atoms.

In addition, the nonionic surfactant may be used by selecting one or more from the group consisting of alkyl ethoxylate represented by the following formula (5), oxo alcohol polyethylene glycol ether represented by the following formula (6), and fatty acid alkanolamide represented by the following formula (7). .

[Formula 5]

In Formula 5, n is an integer of 3 to 15.

[Formula 6]

In the formula (6),

R and R 'are alkyl having 11 to 18 carbon atoms,

n is an integer of 3-15.

[Formula 7]

In the formula (7),

R is alkyl having 11 to 17 carbon atoms,

n is 1 or 2 and m is 0 or 1.

In addition, the surface modifier may be selected from one or more selected from the group consisting of powder zeolites and silicas.

The inorganic dissolution accelerator is a swelling inorganic material in water, preferably at least one selected from the group consisting of bentonite, smectite clay, and clay.

After the preparation of the powder detergent as described above, 1 to 10 parts by weight of one or more disintegrating agents, 3 to 20 parts by weight of one or more disintegrating aids, if necessary, is mixed into a tabletting machine to prepare a final tablet laundry detergent. .

It is preferable in terms of productivity that the tableting machine performs the tableting while rotating the tableting punch by a mechanical structure, and in the present invention, a self-produced rotary tableting machine was used.

The disintegrant is polyvinylpyrrolidone (PVP), Ca-carboxymethylcellulose (Ca-CMC), Na-carboxymethylcellulose (Na-CMC), crosslinked Na-carboxylmethylcellulose (NA-CMC), hydroxyethylcellulose (HEC). , Starch, sodium gluconate, polysodium acrylate, and cellulose derivatives may be used. Such disintegrant may be mixed with 1 to 10 parts by weight of the prepared powder detergent, and less than 1 part by weight is not easily collapsed, when used over 10 parts by weight is not well tableted.

Disintegration aids are sodium acetate, trihydrate (sodium acetate, 3H ₂ O), sodium acetate, anhydrous, sodium chloride (NaCl), potassium chloride (KCl), sodium succinate, and sodium benzoate ( sodium benzoate) by selecting one or more from the group consisting of 3 to 20 parts by weight can be mixed in the prepared powder detergent, the use of less than 3 parts by weight relatively low disintegration effect, when used over 20 parts by weight well tableting It doesn't work. Particularly, when NaCl is used, strength is strong after tableting, and the prepared tablet detergent is preferable because of its long-term stability.

In addition to the above components, the tablet detergent composition of the present invention may be a fluorescent brightener such as stilbene, biphenyl, pyrazoline, fumarin, or quinoline; Enzymes such as proteases, amylases, lipases, or cellulases; And 0.1 to 5 parts by weight of at least one additive selected from the group consisting of bubble control agents such as fatty acids, silicones, or paraffin waxes to prepare detergent particles and final tablet detergents. If the content of such an additive is less than 0.5 parts by weight, the performance of the additive cannot be exhibited, and if it is used more than 5 parts by weight, it is uneconomical.

The present invention will be described in more detail with reference to the following examples. However, an Example is for illustrating this invention and is not limited only to these.

EXAMPLE

Examples 1-4, Comparative Examples 1-4

(Production of Detergent Particles)

Each of the compositions shown in Table 1 below was added to a schugi mixer, mixed, and granulated to prepare detergent particles. The unit is parts by weight.

First, soda ash and LAS were added to the mixer at the same time to neutralize, followed by the addition of the remaining ingredients to prepare detergent particles.

division Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Acid precursor containing liquid surfactant Linear alkylbenzenesulfonic acid 10 12 15 20 3 4 25 25 fatty acid 2 2 2 2 2 2 2 2 Powdered surfactant 13 10 8 7 30 32 3 4 Nonionic surfactant 5 5 5 5 5 5 5 5 Surface modifier 20 20 20 20 20 20 20 20 Dissolution accelerator 4 5 6 7 0.5 0.5 11 11 Alkaline builder (soda ash) 35 35 35 35 35 35 30 30 sulphate of soda 10.5 10.5 8.5 3.5 4 One 3.5 2.5 Fluorescent dyes 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5

In Table 1, the linear alkylbenzene sulfonic acid (C _{10 ~} C ₁₄ ) is LAS (Linear Alkyl benzensulfonic Acid; LG Household Products)

The powdered surfactant is sodium alpha olefin sulfonate having 12 to 18 carbon atoms,

Nonionic surfactant is Korea Polyol AE-7 (Formula 5),

Surface modifiers are Cosmo industry manufactured powder zeolites,

The dissolution accelerator is Bentonite (trade name: Vasagel) manufactured by Ciba Specialty Chem, and the fluorescent dye is a non-phenyl (Bi-Phenyl) -based (or Stylben-based fluorescent dye) manufactured by Ciba Specialty Chem.

(Particle size and solubility of detergent particles)

The particle size of each of the detergent particles prepared above was measured, and the distribution of 12 to 80 mesh sizes is shown in Table 2 below.

In addition, the dissolution time was filled with 1000 ml of water at 4 ° C. in a 1 L beaker, 10 g of each detergent particle was added thereto, and stirred in a magnetic bar for 10 minutes, followed by blending (60 wt% polyethylene, and cotton). 40% by weight of the black cloth (filtering) and the remaining amount was naturally dried at a temperature of 25 ℃ to evaluate the solubility in the amount of the detergent remaining in Table 2 below. At this time, if the amount is large, the solubility of the detergent was evaluated as low.

division Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 12 to 80 mesh particle size distribution (% by weight) 80 to 85 80 to 85 85-90 80 to 85 30-40 30-40 20-25 20-25 Solubility (g) One One 0.5 0.5 4 4 One One

Examples 5-12, Comparative Examples 1-4

(Preparation of Tablet Detergent)

As shown in Table 3, the detergent particles of Examples 1, 2, and Comparative Examples 1, 2, 3, and 4 were mixed with disintegrants, disintegration aids, and enzymes, and tableted using a tableting punch. A mold detergent was prepared. At this time, the tableting punch was compressed into a detergent composition while rotating by a mechanical structure. The unit is parts by weight.

division Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 Example 11 Example 12 Comparative Example 5 Comparative Example 6 Comparative Example 7 Comparative Example 8 Example 1 Detergent Particles 94.5 93.5 92.5 91.5 - - - - - - - - Example 2 Detergent Particles - - - - 86.5 84.5 82.5 80.5 - - - - Comparative Example 1 Detergent Particles - - - - - - - - 99 - - - Comparative Example 2 Detergent Particles - - - - - - - - - 98.9 - - Comparative Example 3 Detergent Particles - - - - - - - - - - 98.8 - Comparative Example 4 Detergent Particles - - - - - - - - - - - 98.7 Disintegrant 5 6 7 8 5 6 7 8 0.5 0.6 0.7 0.8 Collapse Aid - - - - 8 9 10 11 - - - - enzyme 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 system 100 100 100 100 100 100 100 100 100 100 100 100

In Table 3, the disintegrating agent is a cellulose derivative (Nyline, manufactured by FMC), the disintegrating aid is NaCl (manufactured by Handuk Co., Ltd., edible), and the enzyme is Savinase, manufactured by Novo.

(Decay time and strength of tablet detergent)

Each prepared above is shown in Table 4 to determine the disintegration time and strength of the tablet detergent.

The disintegration time was set to the disintegration time by filling a 1 L beaker with water at 20 ° C., installing a trivet, placing a wire mesh on the top, placing a tablet detergent on the tablet, and measuring the time when the tablet completely disintegrated. The disintegration time below is the initial disintegration time after manufacture, and the disintegration time after one month is the disintegration time after one month of storage.

In addition, the strength was measured after the tablet-type detergent, the initial strength and the compressive fracture strength after 3 days.

division Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 Example 11 Example 12 Comparative Example 5 Comparative Example 6 Comparative Example 7 Comparative Example 8 Disintegration time (seconds) 25 22 14 15 11 10 9 8 200 180 220 230 Disintegration time after one month (seconds) 46 45 55 53 15 15 18 19 - - - - Initial strength (kg / ㎠) 4 5 6 7 6 6 7 7 - - - - Strength after 3 days (kg / ㎠) 4 5 6 7 8 8 9 9 - - - -

The tablet-type laundry detergent of the present invention has a disintegration in the wash water within a short time, excellent in the solubility of the particles after the disintegration, the washing time is short, it is suitable for the washing conditions of our country using low-temperature wash water.

Claims (12)

In the tablet laundry detergent composition, a) 10 to 50 parts by weight of alkali builders; b) 5 to 40 parts by weight of a mixture of an acid precursor material-containing liquid surfactant and a powdered surfactant in a weight ratio of 1: 5 to 5: 1; c) 3 to 10 parts by weight of nonionic surfactant; d) 5 to 30 parts by weight of surface modifier; e) 0.1 to 10 parts by weight of inorganic dissolution accelerator; And f) 1 to 10 parts by weight of disintegrant Including; i) The acid precursor-containing liquid surfactant is at least one selected from the group consisting of a linear alkylbenzene sulfonic acid represented by the following formula (1), and a fatty acid represented by the formula (2), ii) The powdered surfactant is one or more selected from the group consisting of alpha olefin sulfonates represented by the following formula (3), and alkyl sulfonates represented by the following formula (4) Tablet laundry detergent composition, characterized in that. [Formula 1] In the formula (1), R is alkyl having 10 to 14 carbon atoms, [Formula 2] In the formula (2), R is alkyl having 14 to 16 carbon atoms. [Formula 3] In the formula (3), R is alkyl having 12 to 18 carbon atoms, n is an integer from 9 to 15, [Formula 4] In the formula (4), R is alkyl having 11 to 18 carbon atoms. The method of claim 1, g) 3 to 20 parts by weight of disintegration aids Tablet type laundry detergent composition further comprising. The method of claim 1, The alkali builder of a) is a carbonate of sodium carbonate, calcium carbonate, or sodium bicarbonate; Silicates of α-sodium silicate (Na ₂ SiO ₃ ) of layered crystalline, or β-sodium silicate (Na ₂ SiO ₃ ); Phosphates of orthophosphoric acid, pyrophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid, or salts thereof; Phosphonates of diethylenetriaminepentamethylenephosphonate, aminotrimethylenephosphonate, 1-hydroxyethylene, or 1-diphosphonate; Nitrilotriacetic acid or salts thereof; Ethylenediaminetetraacetic acid or salts thereof; Carboxymethyl cellulose; Polyethylene glycol; Polyvinyl alcohol; Polyvinylpolydon; Polyacrylic acid or salts thereof; And a maleic acid-vinyl ether copolymer, a salt thereof, or a sulfate salt thereof. delete delete The method of claim 1, Tablets selected from the group consisting of alkyl ethoxylate represented by the following formula (5), oxo alcohol polyethylene glycol ether represented by the following formula (6), and fatty acid alkanolamide represented by the following formula (7) Type Detergent Detergent Composition: [Formula 5] In the formula (5), n is an integer of 3 to 15, [Formula 6] In the formula (6), R and R 'are alkyl having 11 to 18 carbon atoms, n is an integer from 3 to 15, [Formula 7] In the formula (7), R is alkyl having 11 to 17 carbon atoms, n is 1 or 2 and m is 0 or 1. The method of claim 1, The tablet detergent composition of claim 1, wherein the surface modifier of d) is selected from the group consisting of powder zeolites and silicas. The method of claim 1, Wherein the inorganic dissolution accelerator of e) is selected from the group consisting of bentonite, smectite clay, and clay, laundry detergent composition. The method of claim 1, The disintegrating agent of f) is polyvinylpyrrolidone (PVP), Ca-carboxymethylcellulose (Ca-CMC), Na-carboxymethylcellulose (Na-CMC), crosslinked Na-carboxylmethylcellulose (CMC), HEC ( A tablet laundry detergent composition selected from the group consisting of hydroxyethylcellulose, starch, sodium gluconate, polysodium acrylate, and cellulose derivatives. The method of claim 2, The disintegration aid of g) is sodium acetate, trihydrate (sodium acetate, 3H ₂ O), sodium acetate, anhydrous, sodium chloride (NaCl), potassium chloride (KCl), sodium succinate, and A tablet laundry detergent composition selected from the group consisting of sodium benzoate. In the manufacturing method of a tablet laundry detergent, a) on the mixer Iii) 10 to 50 parts by weight of a powdered alkali builder; Ii) the weight mixing ratio is from 1: 5 to 5: 1 A) liquid precursor containing acid precursor material; And B) powdered surfactants 5 to 40 parts by weight of a mixture of; Iii) 3 to 10 parts by weight of nonionic surfactant; Iii) 5 to 30 parts by weight of surface modifier; And Iii) 0.1 to 10 parts by weight of inorganic dissolution accelerator Injecting, mixing and assembling to prepare detergent particles; And b) to a tablet press In the detergent particles prepared in step a) Iii) 1 to 10 parts by weight of disintegrant After adding by mixing, tableting to prepare a tablet detergent Method for producing a tablet-type laundry detergent comprising a. The method of claim 11, The mixing of step b) iii) 3 to 20 parts by weight of the disintegration aid is added to the method for producing a laundry detergent.