KR960008670B1 - Method of powder detergent - Google Patents

Abstract

The method includes the steps of ; (a) manufacturing dry powder detergent by spraying detergent slurry from the top of counter-current spray dryer; (b) crushing in high-speed rotary granulating machine; (c) spraying 0.5-5 wt% polymer such as acrylic acid polymer, acrylic acid-malein acid anhydride copolymer or acrylic acid-malein acid anhydride-methylvinyleter copolymer on it; (d) applying 2-30 wt% insoluble inorganics to it.

Description

Manufacturing method of high density powder detergent

The present invention relates to a method for producing a high-density powder detergent, and more specifically, to a conventional powder by densifying the beads powder obtained by a counter-current spray drying apparatus using a high molecular material The present invention relates to a method for producing a high density powder detergent having a higher apparent density than the detergent obtained under unconditional conditions and excellent fluidity.

In general, there are a number of methods for preparing a laundry powder detergent, but the method using a countercurrent spray drying tower that is easy to mass produce and has good uniformity of particles is most widely used. However, since the detergent produced by this method has an apparent density of about 0.3 g / cm ² and its weight is small compared to its volume, it requires a lot of space and transportation costs when the product is stored, and the product is sufficiently displayed on a limited shelf in the distribution process. Since there is a problem that can not be solved, a study on the densification of powder detergent has been steadily progressed as a solution.

In order to improve the low apparent density, which is a disadvantage of the powder detergent produced by the countercurrent spray drying apparatus, to increase the density, first, the dry particles first prepared by the countercurrent spray drying apparatus are put into a high speed rotary granulator and pulverized. Contact is formed between the dry particles pulverized by spraying a liquid material on the. Subsequently, a porous, water-insoluble inorganic material such as zeolite is applied to the particles on which the contacts are formed, thereby densifying the detergent particles. However, it should be borne in mind that densification of the first dried detergent particles is to select an appropriate liquid binder capable of forming aggregates between the detergent particles crushed on the high-speed rotary granulator. That is, in order to increase the density of the bead-like powder detergent dried by the countercurrent spray drying apparatus, an appropriate liquid binder is sprayed on the dry powder detergent powder to form agglomerates between the powders, and then a water-insoluble inorganic material is applied to the fluidity. The high density detergent should be prepared, but when the binding force of the liquid binder sprayed is low, agglomerates cannot be formed between the crushed detergent particles, and thus a detergent having a apparent density of 0.6 g / cm ² or more, which is the standard apparent density of a general high density detergent, is prepared. It's hard to do.

Techniques for densifying the powder detergent produced by the countercurrent spray drying apparatus are described in Japanese Patent Application Laid-Open Nos. 78-43710, Japanese Patent No. 86-69897, and Japanese Patent Application No. 89-20297. Patent Publication No. 78-43710 discloses a method of densifying using a nonionic surfactant as a liquid binder when grinding and assembling the first dried powder detergent. However, since nonionic surfactants have a weak binding force to form aggregates between the pulverized detergent particles, this method makes it difficult to increase the apparent density of the powder detergent to 0.6 g / cm ³ or more, as well as detergents prepared in this manner. The problem was that liquidity was low.

In addition, Japanese Patent Laid-Open Publication Nos. 86-69897 and 89-20297 disclose a method of using water to densify the first dried powder detergent, which also does not provide sufficient binding force. Therefore, there is a problem that it is difficult to increase the density of the detergent and the fluidity is not preferable because the binding force to agglomerate the crushed detergent particles is weak.

In general, in order to increase the density of the powder detergent containing 10 to 60% by weight of the surfactant, a process of pulverizing these detergents is first required, and the first crushed detergent has an apparent density compared to the powder detergents prepared in the countercurrent spray drying apparatus. However, the detergent pulverized in this state has high dust generation and low fluidity, and thus deteriorates its value as a product. Therefore, in order to commercialize the powder detergent, by forming a contact between the crushed detergent particles and then coated with a porous, water-insoluble inorganic material, etc. to prepare a high-density powder detergent having excellent fluidity. At this time, if the appropriate liquid binder is not used, no contact is formed between the crushed detergent particles, making it difficult to increase the density and lowering the fluidity of the final product.

Accordingly, an object of the present invention is to select a liquid binder suitable for bonding the pulverized detergent particles and to add it to the pulverized detergent particles in order to solve the problems of the above-described method for producing a high-density powder detergent improved fluidity To provide.

Hereinafter, the present invention will be described in detail.

The present invention provides a high-density powder detergent by spraying a binder or a coating agent onto the beads powder detergent particles obtained by spraying the detergent slurry downward from the top of the countercurrent spray drying tower, the polymer material 0.5 to 5 It is a method for producing a high density powder detergent, characterized in that the coating by weight% and water insoluble inorganic material 2 to 30% by weight.

Referring to the present invention in more detail as follows.

, 아크릴산/무수말레이인산 공중합체

및 무수말레인산/메틸비닐에테르 공중합체

중에서 선택된 1종 이상의 고분자물질(분자량 1,000 내지 300,000) 0.5 내지 5중량%를 분무하여 분쇄된 세제분말간에 접점을 형성시켜 응집체를 형성시킨다. 이어서, 도포제로서 제올라이트, 탈크 클레이 및 실리카 등에서 선택된 1종 이상의 수 불용성 무기물질 2 내지 30중량%를 상기 응집체에 도포시키게 되면 유동성이 우수하고 겉보기 밀도가 0.6g/cm³이상인 고밀도 분말세제가 제조되게 된다.The present invention first blends 10 to 60% by weight of one or more surfactants and 20 to 90% by weight of one or more inorganic builders and organic builders into water and sprays downward from the top of the countercurrent spray drying tower, while 200 to 400 ° C.) to make beads of dry detergent powder, and then 60 to 95 wt% of the dry powder is added to a vertical type high speed mixer (Fukae, Japan, or Lodige mixer, Lodige, Germany). To grind. Acrylic acid homopolymer as binder in this pulverized dry powder

Acrylic acid / maleic anhydride copolymer

And maleic anhydride / methylvinyl ether copolymer

0.5 to 5% by weight of at least one polymer material (molecular weight 1,000 to 300,000) selected from among sprayed to form a contact between the pulverized detergent powder to form an aggregate. Subsequently, when 2 to 30% by weight of one or more water-insoluble inorganic materials selected from zeolite, talc clay, silica and the like are applied to the aggregate, a high-density powder detergent having excellent fluidity and an apparent density of 0.6 g / cm ³ or more is prepared. do.

At this time, if the content of the polymer material of the liquid binder is less than 0.5% by weight, it is difficult to increase the dry powder because it is not possible to form a contact between the crushed detergent dry powder, while if the content exceeds 5% by weight the final product There is a problem in that agglomeration of is severe and fluidity is significantly reduced.

In addition, when the amount of the water-insoluble inorganic material is less than 2% by weight, the apparent density is lowered. When the amount of the water-insoluble inorganic material is more than 30% by weight, the excessive amount of the water-insoluble inorganic material remaining after coating is present in the form of dust. Such water-insoluble inorganic material is preferably contained in the 50 to 99% by weight of the particle size of 10㎛ or less, if the particle size exceeds 10㎛ in excess of 50% by weight, they are the fiberol of the laundry even after washing It remains in between.

R₁+R₂=C₁₁~C₁₇), 알레올레핀술폰산염[(CH₃-(CH₂)_m-CH=CH-(CH₂)_n-SO₃Na)와

(CH₂)_X-SO₃Na)의 혼합물 ; m+n=9~15, R=C₇~C₁₃), 알파술포지방산메틸에스테르

R=C₁₄~C₁₅), 지방알코올술페이트(R-CH₂-O-SO₃Na ; R=C₁₁~₁₇), 알칼에테르술페이트(R-CH-CH₂-O-(CH₂CH₂-O)_n-SO₃Na; R'=H, R=C₁₀~₁₂또는 R+R'=C₁₁~C₁₃, R'=H, C₁또는 C₂, n=1~4) 등의 음이온성 계면활성제, 지방알코올 폴리에틸렌글리콜에테르(R-CH₂-CH₂-O)_nH ; R=C₅~C₁₅, n=3~15), 옥소알코올폴리에틸렌글리콜에테르

; R+R'=C₁₁~C₁₃, R'=H, C₁또는 C₂, n=3~15), 알킬페놀폴리에틸렌글리콜에테르(R-C₆H₄-O-(CH₂-CH₂-O)nH ; R=C₈~C₁₂, n=5~10), 지방산 알칸올 아미드

; R=C_11~17, n=1 또는 2, m=0 또는 1)등의 비이온성계면활성제 또는 알킬베타인

; R=C₁₂~C₁₈), 알킬술포베타인

등의 양쪽성계면활성제가 이용될 수 또한, 계면활성제의 세척력을 증강시키는 성분으로는 탄산염계(Na₂CO₃, NaHCO₃, Na₂CO₃·2H₂O), 규산염계(Na₂O : SiO₂=1 : 1.9 내지 3.5), 델타 또는 베타형 층상결정형규산염계(δ-Na₂Si₂O₅또는 β-Na₂Si₂O₅), 인산염계(오르토인산, 피로인산, 트리폴리포스포릭 에시드, 테트라폴리포스포릭에시드 또는 이들의 염), 포스폰산염계(디에틸렌트리아민 펜타메틸렌포스포네이트, 아미노트리메틸렌포스포네이트, 1-히드록시에틸렌-1,1-디포스포네이트, 에틸렌디아민테트라 메틸렌포스포네이트, 헥사메틸디아민테트라 메틸렌포스포네이트), 니트릴로트리아세트산 또는 그의 염, 에틸렌디아민테트라아세트산 또는 그의 염, 구연산 또는 그의 염, 오르토카르복시메틸타르로닉산 또는 그의 염, 카르복시메틸옥시숙신산 또는 그의 염, 카르복시메틸셀룰로오즈, 폴리에틸렌글리콜, 폴리비닐알코올, 폴리비닐피롤리돈, 폴리아크릴산 또는 그의 염, 폴리아크릴산의 아릴알코올의 공중합체 또는 그의 염, 폴리아크릴산과 말레인상의 공중합체 또는 그의 염, 말레인산과 비닐에테르의 공중합체 또는 그의 염, 보렉스(Borax), 황산염 또는 제올라이트(A형) 등을 사용할 수 있으며, 첨가제로는 형광증백제(스틸벤계, 비페닐스틸벤계, 피라졸린계, 쿠마린계, 퀴놀론계), 효소제(프로테아제, 아밀라아제, 리파아제, 셀룰라아제), 기포조절제(지방산계, 실리콘계, 파라핀왁스계) 등을 사용할 수 있다.As a detergent raw material used in the present invention, the main cleaning component is a linear alkylbenzenesulfonate (RC ₅ H ₄ -SO ₃ Na; R = C ₁₀ ~ C ₁₃ ), a fatty acid salt (R-CH ₂ -COONa). R = C ₁₀ -C ₁₅ ), alkyl sulfonates

R ₁ + R ₂ = C ₁₁ -C ₁₇ ), alleleolefinsulfonate [(CH _3- (CH ₂ ) _m -CH = CH- (CH ₂ ) _n -SO ₃ Na) and

A mixture of (CH ₂ ) _X -SO ₃ Na); m + n = 9 ~ 15, R = C 7 ~ C 13), alpha-sulfo fatty acid methyl ester

_{R = C 14 ~ C 15)} , fatty alcohol sulfate _{(R-CH 2 -O-SO} 3 Na; R = C 11 ~ 17), alkali ether sulfate _{(R-CH-CH 2 -O-} (CH 2 _{CH 2 -O) n -SO 3 Na} ; R '= H, R = C 10 ~ 12 or _{R + R' = C 11 ~} C 13, R '= H, C 1 or C _2, n = 1 ~ 4 Anionic surfactants such as), fatty alcohol polyethylene glycol ether (R-CH ₂ -CH ₂ -O) _n H; R = C ₅ to C ₁₅ , n = 3 to 15), oxo alcohol polyethylene glycol ether

; R + R '= C ₁₁ -C ₁₃ , R' = H, C ₁ or C ₂ , n = 3-15), Alkylphenol polyethylene glycol ether (RC ₆ H ₄ -O- (CH ₂ -CH ₂ -O nH; R = C ₈ ~ C ₁₂ , n = 5-10), fatty acid alkanol amide

; Nonionic surfactant or alkylbetaine such as R = C _11-17 , n = 1 or 2, m = 0 or 1)

; R = C ₁₂ ~ C ₁₈ ), alkylsulfobetaine

Amphoteric surfactants such as may be used. Further, components that enhance the washing power of the surfactant include carbonates (Na ₂ CO ₃ , NaHCO ₃ , Na ₂ CO ₃ · 2H ₂ O), silicates (Na ₂ O: SiO ₂ = 1: 1.9 to 3.5), delta or beta layered crystalline silicate type (δ-Na ₂ Si ₂ O ₅ or β-Na ₂ Si ₂ O ₅ ), phosphate type (orthophosphoric acid, pyrophosphoric acid, tripolyphosphoric Acid, tetrapolyphosphoric acid or salt thereof), phosphonate type (diethylenetriamine pentamethylenephosphonate, aminotrimethylenephosphonate, 1-hydroxyethylene-1,1-diphosphonate, ethylene Diaminetetra methylenephosphonate, hexamethyldiaminetetra methylenephosphonate), nitrilotriacetic acid or salts thereof, ethylenediaminetetraacetic acid or salts thereof, citric acid or salts thereof, orthocarboxymethyltaronic acid or salts thereof, carboxymethyloxy Succinic acid or its Salts, carboxymethylcellulose, polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, polyacrylic acid or salts thereof, copolymers of aryl alcohols of polyacrylic acid or salts thereof, polyacrylic acid and maleic copolymers or salts thereof, maleic acid And a copolymer of vinyl ether or a salt thereof, Borax, sulfate or zeolite (type A), and the like, and as an additive, a fluorescent brightener (stilbene type, biphenylstilbene type, pyrazoline type, coumarin type) , Quinolones), enzymes (protease, amylase, lipase, cellulase), bubble control agents (fatty acid, silicone, paraffin wax) and the like can be used.

Hereinafter, the present invention will be described in more detail with reference to Examples.

[Examples 1 to 4 (Comparative Examples 1 to 4)]

: Densification and physical property change by liquid binder

Next, the detergent slurry (solid content: 60% by weight) containing the detergent composition as shown in Table 1 was sprayed downward from the top of the countercurrent spray drying tower, and hot air (temperature: 220 ° C., discharge temperature: 100) from the bottom of the spray drying tower. C) was flowed upward to prepare a powdered powdery detergent (apparent density 0.31 g / cm ³ ). This was put into a high speed rotary granulator (Lodige Mixer: German Lodige Co., Ltd.) with stirring blades and grinding blades and ground for 5 minutes (stirring blades: 100 to 200 rpm, grinding blades: 1000 to 2000 rpm), followed by the following Table 2 The liquid binder was sprayed and stirred for 3 minutes to form a contact point between the detergent particles. Next, a water-insoluble inorganic material according to the following Table 2 was applied to the particles and stirred for 2 minutes to prepare a high density detergent. The results are shown in Table 2 below.

* Distyryl biphenyl series: Tinopal CBS-X from Ciba-Geigy

* 1: Beads detergent prepared by spraying the composition of Table 1 from the top of the countercurrent spray drying tower

* 2: liquid binder

①: Soaptanol-90 (Japan catalytic chemical industry)

②: Polyacrylate (Taechang Products)

* 3: coating agent

* 4: High density powder detergent

③: time taken for 100cc of powder to pass through a funnel having a diameter of 10cm

As shown in Table 2 above, as a result of investigating the densification and physical properties according to the type of the liquid binder, it is preferable to use the other acrylic polymer in the present invention than the case of using water or a nonionic surfactant as the binder. Was excellent.

[Examples 5 to 10 (Comparative Examples 3 and 4)]

: Densification and physical property change according to the content of acrylic polymer

The same detergent slurry as in Table 1 was sprayed downward from the top of the countercurrent spray drying tower to prepare a bead-like powder detergent, which was then fed to a high speed rotary granulator (Lodige Mixer: German Lodige) equipped with stirring blades and grinding blades. After grinding for 5 minutes (stirring blade: 100 to 200rpm, grinding blade: 1000 to 2000rpm), sprayed the liquid binder (acrylic polymer) according to the following Table 3 and stirred for 3 minutes to contact the detergent particles between Was formed. Then, a water-insoluble inorganic material (zeolite) according to the following Table 3 was applied and stirred for 2 minutes to prepare a high density detergent. The results are shown in Table 3 below.

As shown in Table 3 above, when the amount of the liquid binder (acrylic polymer) was maintained at an appropriate line at 0.5 to 5% by weight (Examples 5 to 10), the apparent density and fluidity of the finished product detergent, etc. were preferred. In case of less than 0.5% by weight (Comparative Example 3), it was difficult to achieve high density due to insufficient contact between the dry powder detergents, and when the content exceeded 5% by weight (Comparative Example 4), the fluid content was too high to reduce fluidity. .

Claims (2)

In the densification of the powder detergent produced by the countercurrent spray drying apparatus, the detergent slurry is sprayed downward from the top of the countercurrent spray drying apparatus to prepare a bead-like detergent dry powder, and the dry powder is put into a high speed rotary granulator and pulverized. Then, after spraying 0.5 to 5% by weight of the polymer material with respect to the total weight of the detergent composition to the pulverized dry powder, and then to 2 to 30% by weight of the water-insoluble inorganic material to the total weight of the detergent composition Method for producing a high density powder detergent. The method of claim 1, wherein the polymer material is at least one selected from the group consisting of a homopolymer of acrylic acid, a copolymer of acrylic acid and maleic anhydride, and a copolymer of maleic anhydride and methylvinyl ether, and has a molecular weight of 1,000 to 300,000. How to.