KR100203738B1 - Process for preparing powder detergent of high density - Google Patents

Abstract

The present invention has an agitating shaft perpendicular to a vertical mixing tank and agitating vanes on the shaft to inject a powdered alkali builder into a mixer for mixing the powder, and at the same time, anionic and nonionic surfactants and liquid silicic acid. A method for producing a high density powder detergent, characterized in that the granules are first granulated by neutralizing by high-speed rotation while spraying soda, and the final particles are granulated by a high-speed rotating granulator by adding a powder anionic surfactant and surface modifier. will be. The method of the present invention can produce a powder detergent having a higher apparent density and better solubility and fluidity than the detergent produced by the conventional countercurrent spray drying apparatus, and it does not cost fuel compared to the conventional countercurrent drying apparatus, and it is possible to prevent fire and explosion. Risks are completely eliminated and environmental pollution can be minimized.

Description

Manufacturing method of high density powder detergent

The present invention relates to a method for producing a high density powder detergent. More specifically, the present invention has a mixer that has a vertical stirring shaft inside the vertical mixing tank by a method of making a detergent without using a conventional countercurrent spray drying apparatus, and mixing the powder by installing a stirring blade on the shaft ( At the same time, the powder-type alkali builder is added to the mixer, and at least one liquid surfactant component and an appropriate amount of liquid sodium silicate are neutralized by spraying to form particles first, and then a powdery surfactant and a surface modifier are added. It relates to a method for producing a high-density powder detergent characterized in that the granulated final particles in a high speed rotary granulator. According to the present invention, it is possible to prepare a powder detergent having a good fluidity and solubility compared to the detergent made through the conventional countercurrent spray drying apparatus.

In order to increase the density of detergents by the conventional method of manufacturing high-density powder detergent, dry particles dried by countercurrent spray drying apparatus are put into a high speed mixer or Lodige mixer, pulverized, and then sprayed with a liquid material. Forming a contact point on the pulverized dry particles and then applied with a water-insoluble material such as zeolite, talc has been proposed a method of making a high-density detergent with good fluidity, but this method has a disadvantage in poor solubility through the drying process. Methods for densifying the powder detergent produced by the countercurrent spray drying apparatus include Japanese Patent Laid-Open Nos. 61-69900, 61-69898, 78-43710, and 4-5080 Described in the heading. However, the methods described in the above-mentioned patent documents have a poor solubility due to the drying process, complicated processes such as neutralization-blend-drying-concentration, high production cost for production, excessive production cost, and high energy consumption. There are disadvantages such as low efficiency. In addition, methods for making detergents by neutralizing alkylbenzenesulfonic acid directly in a mixer are described in EP-390251 and EP-544365, etc., but these methods are used to prepare the detergent by granulating the surface with a surface modifier after the production of alkylbenzenesulfonate. There was a limit to high concentrations. In general, in order to prepare a laundry detergent containing 10 to 60% by weight of a surfactant without drying process, a process of converting alkylbenzenesulfonic acid to alkylbenzenesulfonic acid salt by an alkaline substance is necessary, and in this process, soda ash (Na ₂ CO ₃ ) If alkylbenzenesulfonic acid is added directly to the solution, neutralization does not occur. Also, if a liquid nonionic surfactant is used for concentration, it is impossible to use it by sticky, and the content of the surfactant is low because it does not increase the content of the surfactant. In Europe, the above method has been used.

An object of the present invention to solve the problems of the prior art described above is to provide a method for producing a high-density powder detergent having excellent fluidity and solubility, high concentration and simple manufacturing facilities.

The present invention has a stirring shaft perpendicular to the inside of the vertical mixing tank, the stirring blade is installed on the shaft 10 to 50% by weight of the powder type alkali bilter at the same time at least one liquid anionic surfactant 12 to 25% by weight of components, 3 to 20% by weight of one or more nonionic surfactants, and 1 to 10% by weight of liquid sodium silicate are neutralized by high-speed rotation to be granulated first, followed by powdered anionic surfactants 1 to 1. It relates to a high-density powder detergent manufacturing method characterized in that the final particles are granulated in a high speed rotary granulator by adding 10% by weight and 5 to 30% by weight surface modifier.

The method according to the present invention is carried out in two stages, and granulation is carried out, and the binder and the surface modifier are separately added at each stage, and powdered surfactants are used to reduce the stickiness of the particles and commercialize them.

The powdered alkali builder used in the method of the present invention may be selected from Na ₂ CO ₃ or K ₂ CO ₃ , and the surface modifier may be aluminosilicate (zeolite) used as a remover of Ca ions, having a thickness of 10 μm or less. Preferred are inorganic nonpowders such as bentonite, clay, talc and the like. The amount of the surface modifier used in the method of the present invention is preferably 5 to 30% by weight of the total weight. If the surface modifier is used in less than 5% by weight it is difficult to obtain a good fluidity powder, when used in excess of 30% by weight may lower the fluidity and fine powder may cause a feeling of use.

The apparent specific gravity of the high density detergent produced by the method of the present invention is preferably 0.6 to 1.0 g / cm 3. If the apparent specific gravity exceeds 1.0 g / cm 3, the solubility becomes poor.

In the present invention, as the main component of the detergent raw material and the liquid surfactant added to the primary granulation step, a linear alkylbenzene sulfonate (R- -SO ₃ Na: R = C ₁₀ -C ₁₄ alkyl), Fatty acid salt (R-CH ₂ -COONa: R = C ₁₄ -C ₁₆ alkyl), Alkanesulfonate (R ₁ = CH-SO ₃ Na: R ₁ = C ₁₁ -C ₁₈ alkyl) and alpha olepinsulfonate (R-CH = CH- (CH ₂ ) _n -SO ₃ Na, n = an integer of 9-15, R = C ₁₂ -C ₁₈ alkyl) One or more selected may be mentioned. Moreover, as a nonionic surfactant, alpha sulfo fatty acid methyl ester ( : R = C ₁₄ -C ₁₈ alkyl), oxo alcohol polyethylene glycol ether (alcohol ethoxylate, AE)

Fatty acid alkanolamides

Etc. can be used, and as an amphoteric surfactant Etc. can be used.

On the other hand, in order to enhance the cleaning power of the above-mentioned surfactants, carbonates (eg, sodium carbonate (Na ₂ CO ₃ ) or sodium bicarbonate (NaHCO ₃ )), silicates (eg, layered crystalline α) -Na ₂ SiO ₃ or β-Na ₂ SiO ₃ ), phosphates (eg orthophosphoric acid, pyrophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid or salts thereof), phosphonates (eg, Diethylenetriaminepentamethylenephosphonate, aminotrimethylenephosphonate, 1-hydroxyethylene-1, 1-diphosphonate), nitrilotraacetic acid or salts thereof, ethylenediaminetetraacetic acid or salts thereof, carboxymethyl Cellulose, polyethylene glycol, polyvinyl alcohol, polyvinylpolydon, polyacrylic acid or its salts, copolymers of maleic acid and vinyl ether or salts thereof or sulfates thereof can be used.

In the method of the present invention, it is preferable to use 1 to 10% by weight in the case of sodium silicate, which is a liquid component introduced into the mixer. If less than 1% by weight of sodium silicate is used, the particles do not form in the mixer and the particles become sticky. If the amount is more than 10% by weight, the particles become large and the solubility is lowered, making it difficult to commercialize. In the case of the liquid sodium silicate, the ratio of Na ₂ O: SiO ₂ is most preferably 1: 1.5 to 1: 3. When the ratio is 1: 3 or more, insoluble SiO ₂ is precipitated and the solubility becomes poor.

In the method of the present invention, it is preferable that the powdered anionic surfactant use 1 to 10% by weight of sodium alpha olefin sulfonate or sodium lauryl sulfate. In particular, it is preferable to use those having an apparent density of 0.4 to 1.5 g / cm 3, an average particle size distribution of 250 to 700 μm, and a particle size distribution of 25 wt% or less. If the anionic surfactant is used at less than 1% by weight, it may cause deterioration of cleaning power. If the anionic surfactant is used at less than 10% by weight, it may cause deterioration of productivity and deterioration of product properties, resulting in problems such as caking. do.

As the surface modifier, it is preferable to use at least one selected from powder zeolite, talc, clay and silica, and it is preferable to contain 50 wt% or more of particles having a particle diameter of 10 μm or less.

Meanwhile, the detergent composition of the present invention prepared by the method described in detail above may further include a fluorescent brightener (for example, stilbene-based biphenyls, piazoline-based, fumarine-based or quinolone-based) enzymes in addition to the above-mentioned components. (E.g., protease, alkylase, lipiase, or cellulase), foam control agents (e.g., Chibaan, silicone, paraffin wax) and the like can be prepared.

The manufacturing process of the high-density powder detergent according to the present invention basically consists of two steps, which will be described in more detail in each step as follows.

1) Neutralization and 1st Assembly Process (Granulation Step)

Alkylbenzenesulfonic acid, fatty acid, liquid sodium silicate, and alkyl ethoxylate are added to the mixer in which powder is mixed into a mixer which has a stirring shaft perpendicular to the inside of a vertical mixing tank and a stirring blade is installed on the shaft to mix the powder. It is a step of assembling primary particles by spraying at high speed by spraying. In this step, the liquid sodium silicate is used in an amount of 1 to 10% by weight, and the mixer uses a granulator in the form of a hand mixer made by a handman.

2) Second Assembly Process (Surface Modification Step)

In the concentrated state after the first granulation, alpha olefin sulfonate powder, sodium lauryl sulfate powder and surface modifier are added and stirred using a high speed mixer (lodige mixer) to prepare a detergent having excellent fluidity and solubility. Manufacture.

The production method according to the present invention can simplify the existing neutralization slurry production → blend slurry production → drying → concentration process into a process leading to granulation → surface modification to simplify the process equipment can minimize the manufacturing cost. In addition, there is no fuel cost for the existing reflux drying equipment, and the risk of fire or explosion is completely eliminated, thereby minimizing environmental pollution.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, these examples are only for illustrating the present invention, and the scope of the present invention in any sense is not limited by these examples.

[Example: Comparative Example 1 and Examples 1 to 4]

Comparative Example 1

A powder slurry was prepared by spraying a detergent slurry (solid content: 60% by weight) containing a detergent composition having the ingredients and contents shown in Table 1 from the top of the countercurrent spray drying tower.

* Fluorescent dye biphenyl: Tinopal CBS-X (disodium 4,4'-bis (2-sulphostyryl) biphenyl)

[Examples 1 to 4]

Powder detergents were prepared using the method of the present invention without the use of countercurrent spray drying towers with the components and contents shown in Table 2 below.

* 5: AE-7 (manufactured by Korea Polyol Co., Ltd.) (the average number of moles of ethylene oxide (EO) added as alcohol ethoxylate is 7)

* 6: sodium alpha olefin sulfonate (C ₁₂ -C ₁₈ )

* 8: fragrance, bubble regulator, enzyme, water, etc.

Experimental Example 1

Physical property test of powder detergent according to the present invention

The detergent and the fluidity of the powder detergent prepared according to Comparative Example 1 and Examples 1 to 4 were evaluated under the following conditions.

1) Detergency Test

Washing Machine: Terg-O-Tometer

Cleaning temperature: 25 ℃

Washing water: Hardness 80ppm Ca ⁺⁺ , 20ppm Mg ⁺⁺

Bath ratio: 3.5g contaminated cloth / ℓ

Pollution mark: EMPA Art No.102 (olive oil, carbon black / blend (polyester / cotton)

Detergent Concentration: 0.67g / ℓ

Evaluation: Converting the cleaning power with Comparative Example 1 as 100

2) liquidity evaluation

The fluidity of each powder detergent was compared by measuring the time it took for 100 cc of powder to pass through a funnel of diameter 10 cm in the KS-2709 specific gravity hopper. The smaller the time, the better the fluidity.

3) Solubility Evaluation

Solubility was measured by dissolving 5 g of powder detergent in 1 liter of water at 25 ° C., stirring for 5 minutes with a magenetic stirrer, and filtering the resultant with a Buchner funnel on a black cloth. It is evaluated that solubility is bad when there is much residual amount.

Test results for detergency and rheology are shown in Table 3 below along with the apparent density and surfactant content of the powder detergent.

As can be seen from the results of Table 2, the powder detergent (Examples 1 to 3) according to the present invention is superior in washing power and fluidity as compared to the conventional powder detergent, and apparent density is higher compared to the detergent produced by the conventional method It can be seen that the product has excellent quality. However, as shown in Example 4, when the content of the liquid sodium silicate exceeds 10% by weight, it can be seen that the particles are very sticky and poor in fluidity.

Claims (7)

10 to 50% by weight of a powdered alkali builder is added to a mixer which has a stirring shaft perpendicular to the inside of the vertical mixing tank, and a stirring blade is installed on the shaft to mix the powder. 12 to 25% by weight, 3 to 20% by weight of a nonionic surfactant, and 1 to 10% by weight of liquid sodium silicate are neutralized by high-speed rotation to give first granulation, followed by 1 to 10% by weight of powdered anionic surfactant. And adding 5 to 30% by weight of the surface modifier to granulate the final particles with a high-speed rotary granulator. The method of claim 1 wherein the powdered alkali builder is Na ₂ CO ₃ or K ₂ CO ₃ and the surface modifier is powder zeolite, talc, clay and silica. The method of claim 1, wherein the liquid sodium silicate has a SiO ₂ : Na ₂ O of 1: 1.5 to 1: 3. The method according to claim 1, wherein the powdered anionic surfactant is sodium alpha olefin sulfonate or sodium lauryl sulfate, and the nonionic surfactant is alpha sulfo fatty acid methyl ester, oxo alcohol polyethylene glycol ether or fatty acid alkanolamide. The method according to claim 4, wherein the powdery anionic surfactant has an apparent density of 0.4 to 1.5 g / cm 3, an average particle size of 250 to 700 μm, and a particle size distribution of 25 wt% or less. The method of claim 1 wherein the countercurrent drying apparatus is not used by neutralizing directly with a powdered alkali builder. A high density powder detergent prepared by the method of claim 1.