JPS60262895A - Manufacture of granular detergent - Google Patents

Manufacture of granular detergent

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Publication number
JPS60262895A
JPS60262895A JP11834684A JP11834684A JPS60262895A JP S60262895 A JPS60262895 A JP S60262895A JP 11834684 A JP11834684 A JP 11834684A JP 11834684 A JP11834684 A JP 11834684A JP S60262895 A JPS60262895 A JP S60262895A
Authority
JP
Japan
Prior art keywords
granular detergent
detergent
calcium carbonate
weight
alkali metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP11834684A
Other languages
Japanese (ja)
Other versions
JPH0550558B2 (en
Inventor
誠治 阿部
信一 福留
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lion Corp
Original Assignee
Lion Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lion Corp filed Critical Lion Corp
Priority to JP11834684A priority Critical patent/JPS60262895A/en
Publication of JPS60262895A publication Critical patent/JPS60262895A/en
Publication of JPH0550558B2 publication Critical patent/JPH0550558B2/ja
Granted legal-status Critical Current

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Abstract

(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。
(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 産」ししΦ重重り年回□ 本発明は粒状洗剤の粉体物性、特に無リン洗剤の吸湿時
の加圧固化性を改善する粒状洗剤の製造方法に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a granular detergent that improves the powder properties of a granular detergent, particularly the pressurized solidification property of a phosphorus-free detergent upon moisture absorption.

従速10丸肴 リン酸系ビルダーは優れた無機質ビルダーであり、従来
は汎く粒状洗剤に配合されていた。
Phosphate-based builders are excellent inorganic builders and have conventionally been widely incorporated into granular detergents.

しかし、湖沼、内湾などの富栄養化への配慮から、無リ
ン化への努力が払われている。リン酸系ビルダーに代る
ものとしては、珪酸アルカリ塩、炭酸アルカリ塩、重炭
酸アルカリ塩などが用いられ、また、近年ゼオライトが
注目されている。
However, in consideration of eutrophication in lakes, marshes, inner bays, etc., efforts are being made to eliminate phosphorus. Alkali silicate salts, alkali carbonate salts, alkali bicarbonate salts, etc. are used as substitutes for phosphoric acid builders, and zeolites have recently attracted attention.

しかしながら、これら代替ビルダーは洗浄力の向上に対
する効果は認められるものの、粉体特性の改質効果は不
十分であった。
However, although these alternative builders were recognized to be effective in improving detergency, the effect of modifying powder properties was insufficient.

本出願人はこのような無リン粒状洗剤の吸湿に基因する
固化性を改善するため、粒状化した洗剤の外面に非吸湿
性のビルダー、金属石けんあるいはアルミノシリケート
を層として被覆し、洗剤粒子表面の性質を改質すること
を提案した(特開昭49−38906号、特開昭50−
51508号、特開昭50−24305号)。
In order to improve the solidifying properties of such phosphorus-free granular detergents due to moisture absorption, the applicant coated the outer surface of the granulated detergent with a layer of non-hygroscopic builder, metal soap, or aluminosilicate, and added a layer to the surface of the detergent particles. proposed to modify the properties of
No. 51508, JP-A-50-24305).

また、水不溶性ないし水難溶性の粉体を粒状洗剤に付着
させることにより、粒状洗剤の粉体物性を改善しうろこ
とを見出し、このような粉体として平均粒径1.5μm
以下の酸化マグネシウム、水酸化アルミニウム、重質炭
酸カルシウム、ホワイトカーボン、酸化チタン(特開昭
53−114807号公報)あるいは平均粒径2〜5μ
mの炭酸カルシウム(特開昭54−103406号公報
)を提案した。
In addition, we have found that by attaching water-insoluble or poorly water-soluble powder to granular detergent, the physical properties of the granular detergent can be improved.
The following magnesium oxide, aluminum hydroxide, heavy calcium carbonate, white carbon, titanium oxide (Japanese Unexamined Patent Publication No. 114807/1983) or average particle size 2 to 5μ
proposed calcium carbonate (Japanese Unexamined Patent Publication No. 103406/1983).

明が ′ しようとする。 点 しかし、特開昭50−24305号等に開示した洗剤粒
子を膜層で被覆する方法は、当初の吸湿番コよる固化の
防止という点では効果があるものの、工程の煩雑さ、均
質品の取得の困難さ等の点で問題があるばかりでなく、
洗剤の溶解性、長期保存時の吸湿固化性等にも難があり
、必ずしも満足すべきものではなかった。
Ming tries to ′. However, although the method of coating detergent particles with a film layer disclosed in JP-A No. 50-24305 is effective in preventing solidification due to the initial moisture absorption rate, it is complicated in the process and disadvantageous in the production of homogeneous products. Not only is there a problem in terms of difficulty in obtaining it, but
There were also problems with detergent solubility, moisture absorption and solidification properties during long-term storage, and the results were not necessarily satisfactory.

また、特開昭53−’114807号公報等に記載され
たような粉体を付着させて被覆する方法は、製造操作は
簡便であるものの、十分に付着しにくいため、洗浄力を
維持しつつ十分な粉体特性の改質効果を得るという点で
さらに改善がまたれていた。
In addition, the method of coating by adhering powder as described in JP-A-53-'114807 etc., although the manufacturing operation is simple, does not adhere well, so it is difficult to adhere to the powder while maintaining cleaning power. Further improvements were made in terms of obtaining sufficient powder property modification effects.

皿蟇(解法1泰り表例王殺一 本発明は、洗浄力を損なうことなく粉体物性を改善する
ことのできる粒状洗剤の製造方法を提供することを目的
とする。
An object of the present invention is to provide a method for producing a granular detergent that can improve powder physical properties without impairing detergency.

すなわち、本発明の粒状洗剤の製造fJ法は、少なくと
も1種のアニオン界面活性剤と、アルカリ金属珪酸塩と
、アルカリ金属炭酸塩とを含有する粒状洗剤の粒子表面
に、−次粒子径が0.1〜1.5μmのサイコロ状の微
細沈降炭酸カルシウムを、該粒状洗剤100重量部当り
0.5〜3重硼部付着することに特徴とする。
That is, the fJ method for producing a granular detergent of the present invention has a particle surface of a granular detergent containing at least one kind of anionic surfactant, an alkali metal silicate, and an alkali metal carbonate having a -order particle size of 0. It is characterized in that 0.5 to 3 parts of finely precipitated calcium carbonate in the form of dice of 1 to 1.5 μm are deposited per 100 parts by weight of the granular detergent.

本発明の粒状洗剤で用いられるアニオン界面活性剤とし
ては、 アルキル基の炭素数が8〜15のアルキルベンゼンスル
ホン酸塩、 アルキル基の炭素数が8〜]8のアルキル硫酸塩、 アルキル基の炭素数が8〜18のアルコールに酸化エチ
レンを平均1〜8付加させたアルキルエーテル硫酸塩、 炭素数12〜22のα−オレフィンスルホン酸塩(α−
オレフィンのスルホン化物でアルケンスルホン酸塩、ヒ
ドロキシアルカンスルホン酸塩などの混合物)、 炭素数12〜22のパラフィンから得られるアルカンス
ルホン酸塩、 高級脂肪酸塩、 高級脂肪酸とタウリンとの縮合物の塩(N−アシルアミ
ノエタンスルホン酸塩)、スルホコハク酸ジアルキルエ
ステルの塩などが例示される。これらはアルカリ金属塩
か適当で、スルホン酸やサルフェート型アニオン活性剤
の場合はマグネシウム塩も適している。
The anionic surfactants used in the granular detergent of the present invention include alkylbenzene sulfonates whose alkyl group has 8 to 15 carbon atoms, alkyl sulfates whose alkyl group has 8 to 8 carbon atoms, and alkyl sulfates whose alkyl group has 8 to 8 carbon atoms. Alkyl ether sulfate, which is made by adding 1 to 8 ethylene oxides on average to an alcohol with 8 to 18 carbon atoms, α-olefin sulfonate having 12 to 22 carbon atoms (α-
olefin sulfonates (mixtures of alkenesulfonates, hydroxyalkanesulfonates, etc.), alkanesulfonates obtained from paraffins having 12 to 22 carbon atoms, higher fatty acid salts, and salts of condensates of higher fatty acids and taurine ( N-acylaminoethanesulfonate), salts of dialkyl sulfosuccinates, and the like. These are suitably alkali metal salts, and in the case of sulfonic acid or sulfate type anion activators, magnesium salts are also suitable.

アニオン活性剤は粒状洗剤中に10〜40重量%配合す
るのが適当であり、このましくは15〜30重量%であ
る。
The anionic activator is suitably blended in the granular detergent in an amount of 10 to 40% by weight, preferably 15 to 30% by weight.

本発明の粒状洗剤は、また、無機ビルダーとしてアルカ
リ金属珪酸塩およびアルカリ金属炭酸塩を含有し、ナト
リウム塩、カリウム塩が好適である。 アルカリ金属珪
酸塩としては、M2O・n5jO□(M :アルカリ金
属)でモル比nが2゜0〜3.6のものが好ましい、ア
ルカリ金属珪酸塩は洗剤中に4〜20wt%配合するの
が適当であり、好ましくは8〜+5iyt%である。
The granular detergent of the present invention also contains alkali metal silicates and alkali metal carbonates as inorganic builders, with sodium salts and potassium salts being preferred. The alkali metal silicate is preferably M2O・n5jO□ (M: alkali metal) with a molar ratio n of 2°0 to 3.6. It is preferable that the alkali metal silicate be blended in the detergent in an amount of 4 to 20 wt%. Suitable, preferably 8 to +5 iyt%.

アルカリ金属炭酸塩は洗剤中に2〜40νt%配合する
のか適当であり、好ましくは5〜3(ht%である。
The alkali metal carbonate is suitably blended into the detergent in an amount of 2 to 40 vt%, preferably 5 to 3 (ht%).

1−記各成分を含む洗剤は、噴霧乾燥法などにより造粒
されて、通りハ粒径300〜600μmの粒状洗剤とさ
れる。
1- The detergent containing each component is granulated by a spray drying method or the like to form a granular detergent having a particle size of 300 to 600 μm.

この粒状洗剤の粒子表面に、−次粒子径が0.1−1.
5μm、好ましくは(1,33−1pの沈降炭酸カルシ
ウムが付着される。この粉体による被覆は回転混合機、
振動混合機などの混合機により行うことができ、また、
回転造粒機、転勤造粒機、振動造粒機のような造粒機な
どによっても行うことができる。
The particle surface of this granular detergent has a particle size of 0.1-1.
5 μm, preferably (1,33-1 p) of precipitated calcium carbonate is deposited. The coating with this powder is carried out using a rotary mixer,
This can be done with a mixer such as a vibrating mixer, and
It can also be carried out using a granulator such as a rotary granulator, a transfer granulator, or a vibration granulator.

戻酸カルシウムの一次粒子径が1.5μmよりも大きく
なると粉体物性の改質効果が劣化し、一方、0.1μm
未満では凝集が激しく、粉体物性改良効果が小さいばか
りか、ハンドリングが困難になる。
When the primary particle size of the rehydrated calcium is larger than 1.5 μm, the effect of modifying the powder physical properties deteriorates;
If it is less than that, agglomeration will be severe and the effect of improving powder physical properties will be small, and handling will become difficult.

微細沈降炭酸カルシウム粉体の使用量は、粒状洗剤10
0重量部に対して0.5〜3重量部、好ましくは1〜2
重量部である。0.5重量部未満では粉体物性の改良効
果が不十分であり、一方、3重量部を越えると洗浄力が
低下してしまう。
The amount of finely precipitated calcium carbonate powder used is 10% of the granular detergent.
0.5 to 3 parts by weight, preferably 1 to 2 parts by weight
Parts by weight. If it is less than 0.5 parts by weight, the effect of improving the powder physical properties will be insufficient, while if it exceeds 3 parts by weight, the detergency will decrease.

また、本発明では微細沈降炭酸カルシウムの形状がサイ
コロ状であることが重要であり、粒子の最小径/最大径
比が0.3〜0.7のサイコロ状であることが好ましく
、さらに好ましい上記比率は0.4〜0.7である。こ
のようなサイコロ状の粒子とすることにより効率よく粒
状洗剤を被覆することができる。上記比率範囲を逸脱す
ると、粉体物性の改質効果が不十分となる。このような
サイコロ状の微細沈降炭酸カルシウムは、たとえば、フ
ァイザー・クイグレー社、奥多摩工業曲から入手するこ
とができる。
Further, in the present invention, it is important that the fine precipitated calcium carbonate has a dice-like shape, and it is preferable that the particle has a minimum diameter/maximum diameter ratio of 0.3 to 0.7, and more preferably the above-mentioned The ratio is 0.4-0.7. By forming such dice-shaped particles, the granular detergent can be efficiently coated. If the ratio is outside the above range, the effect of modifying the powder physical properties will be insufficient. Such dice-shaped finely precipitated calcium carbonate can be obtained, for example, from Pfizer Quigley, Okutama Kogyoku.

本発明で表面改質される粒状洗剤は、クエン酸塩、リン
ゴ酸塩、酒石酸塩、マレイン酸塩ポリマー、アルキル置
換コハク酸塩、オキシシml゛酸塩などの有機ビルター
、水溶性硫酸JIA、再汚染防止剤(CMC,PEG、
 PVAなど)、泡14 ント。
The granular detergents surface-modified in the present invention include organic bilters such as citrate, malate, tartrate, maleate polymers, alkyl-substituted succinates, oxysymbolates, water-soluble sulfuric acid JIA, and reagents. Anti-fouling agents (CMC, PEG,
(PVA, etc.), foam.

−ル剤、蛍光増白剤、漂白剤、色素、香料などを任意成
分として含有することもできる。
It may also contain optional ingredients such as brighteners, optical brighteners, bleaching agents, pigments, and fragrances.

償−那 粒状洗剤に微細沈降炭酸カルシウムを付着させることに
より、洗剤粒子の粉体物性が改善される。なお、一般に
沈降炭酸カルシウムは紡錘形か柱状であるか、このよう
な形状のものは洗剤粒子表面との接触面積が少くて付着
しにくいため粉体特性改良効果が劣る。
By attaching fine precipitated calcium carbonate to a granular detergent, the powder physical properties of the detergent particles are improved. Generally, precipitated calcium carbonate has a spindle shape or a columnar shape, and if it has such a shape, the contact area with the detergent particle surface is small and it is difficult to adhere to the surface of the detergent particle, so that the effect of improving powder properties is inferior.

肱□來 本発明の製造方法によれば、洗浄力を低下させることな
く、流動性、吸湿固化性、加圧固化性などの粉体特性、
特に吸湿時の加圧固化性を改良することができる。
According to the production method of the present invention, powder properties such as fluidity, moisture absorption solidification property, pressure solidification property, etc., can be improved without reducing detergency.
In particular, it is possible to improve the pressurized solidification properties upon moisture absorption.

実−絶倒− 以下の組成の平均粒径400〜500μmの粒状洗剤を
噴霧乾燥により製造した。
A granular detergent having the following composition and an average particle size of 400 to 500 μm was produced by spray drying.

アルキルベンゼンスルホン酸ソーダ (C: 1O−14) 12vt% α−オレフィンスルホン酸ソーダ (C: 13〜18) +2すt% 珪酸ソーダ(S j、 02/N a20=2.2) 
12wt%炭酸ソーダ 10νL% 水 5νt% 硫酸ソーダ バランス この粒状洗剤100重量部に対して、それぞれ第1表に
示した性状の沈降炭酸カルシウムを第1表に示した重量
部添加し、■型ミキサーで5分間混合し、炭酸カルシウ
ムを粒状洗剤の表面に付着させて被覆した。
Sodium alkylbenzenesulfonate (C: 1O-14) 12vt% Sodium α-olefin sulfonate (C: 13-18) +2st% Sodium silicate (S j, 02/N a20 = 2.2)
12 wt% Soda carbonate 10 νL% Water 5 νt% Sodium sulfate Balance To 100 parts by weight of this granular detergent, the parts by weight shown in Table 1 of precipitated calcium carbonate having the properties shown in Table 1 were added, and the mixture was mixed in a ■ type mixer. Mixed for 5 minutes to deposit and coat the calcium carbonate onto the surface of the granular detergent.

これら各試料(Nn2〜8)および炭酸カルシウムを付
着させなかった試料(No1.)の吸湿固化性および洗
浄力を以下の手順で測定して第1表に示した。なお、第
1表中の最小径/最大径の比は電子顕微鏡写真で各粒子
の最大径、最小径を測定し、n=50の平均をとった。
The hygroscopic solidification properties and detergency of each of these samples (Nn2-8) and the sample to which calcium carbonate was not attached (No. 1.) were measured according to the following procedure and are shown in Table 1. The minimum diameter/maximum diameter ratio in Table 1 was determined by measuring the maximum diameter and minimum diameter of each particle using an electron microscope photograph, and taking the average of n=50.

堺2賛閘(1: (! (]lてl)−洗剤用カル1−
ン(22X 15.5 X 5.5cm、透湿度300
に / nI′24hr )に粒子を充填し、:)5°
C−100%のヒューミディティボックス(Ilumj
diLy Box)に3 El静置後、カルトンを切り
開き、4メツシユのフルイーLに注意深くうつし、フル
イをゆるやかに振動したのちのフルイ」−の重量と原試
料の重量比によって示した。
Sakai 2 support gate (1: (! (]ltel)-Detergent Cal 1-
(22 x 15.5 x 5.5 cm, moisture permeability 300
/nI'24hr) filled with particles :)5°
C-100% Humidity Box (Ilumj
After leaving 3 El in a diLy Box), the carton was cut open, carefully transferred to a 4-mesh Fluie L, and the sieve was gently vibrated.The weight of the sieve was expressed as the ratio of the weight of the original sample to the weight of the sieve.

L1ヨ辺 拭布(綿)をワイシャツの衿に装着し、2〜7日間着用
して汚染したのち取りはずし、左右対称に切断したもの
を20枚づつ用意する。別に2〜3日間着用した肌シャ
ツ(綿メリヤス)を用意し、左右対称に分割する。この
ようにして汚染された拭布及び肌シャツの各一方を標準
洗剤(炭酸カルシウム付着なし、第1表のN01)によ
り、他方を被検試料(炭酸カルシウム付着。
Attach a L1 side cloth (cotton) to the collar of a dress shirt, wear it for 2 to 7 days until it becomes contaminated, then remove it and cut it symmetrically on the left and right sides to prepare 20 pieces each. Separately, prepare a skin shirt (cotton knitted) that has been worn for 2 to 3 days and divide it symmetrically. One of the wiping cloth and the skin shirt contaminated in this way was treated with a standard detergent (no calcium carbonate attached, No. 1 in Table 1), and the other was treated with a test sample (no calcium carbonate attached).

第1表のNo 2以降)により洗剤濃度0.15%、液
温25℃、浴比30倍で10分間洗濯した後、3分間づ
つ2回すすぐ。洗浄後の各拭布は各1対づつ左右を肉眼
で比較判定し、標準洗剤の洗浄力の評点で各試料洗剤の
評点を除して100倍した数値を洗浄力指数とした。
After washing for 10 minutes at a detergent concentration of 0.15%, a liquid temperature of 25°C, and a bath ratio of 30 times, using No. 2 onwards in Table 1, the clothes were rinsed twice for 3 minutes each. After cleaning, the right and left sides of each pair of wiping cloths were compared and judged with the naked eye, and the value obtained by dividing the rating of each sample detergent by the rating of the cleaning power of the standard detergent and multiplying the result by 100 was used as the cleaning power index.

(以下余白)(Margin below)

Claims (1)

【特許請求の範囲】 ■、少なくとも1種のアニオン界面活性剤と、アルカリ
金属珪酸塩と、アルカリ金属炭酸塩とを含有する粒状洗
剤の粒子表面に、−次粒子径が0.1〜1.5μlのサ
イコロ状の微細沈降炭酸カルシウムを、該粒状洗剤10
0重量部当り0.5〜3重量部付着することを特徴とす
る粒状洗剤の製造方法。 2、@細沈降炭酸カルシウムの形状が最小径/最大径比
で0.3〜0.7のサイコロ状であることを特徴とする
特許請求の範囲第1項記載の粒状洗剤の製造方法。
Scope of Claims: (1) A particle surface of a granular detergent containing at least one anionic surfactant, an alkali metal silicate, and an alkali metal carbonate has a particle size of 0.1 to 1. Add 5 μl of diced fine precipitated calcium carbonate to 10 μl of the granular detergent.
A method for producing a granular detergent, characterized in that 0.5 to 3 parts by weight are deposited per 0 parts by weight. 2. The method for producing a granular detergent according to claim 1, wherein the fine precipitated calcium carbonate has a dice-like shape with a minimum diameter/maximum diameter ratio of 0.3 to 0.7.
JP11834684A 1984-06-11 1984-06-11 Manufacture of granular detergent Granted JPS60262895A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11834684A JPS60262895A (en) 1984-06-11 1984-06-11 Manufacture of granular detergent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11834684A JPS60262895A (en) 1984-06-11 1984-06-11 Manufacture of granular detergent

Publications (2)

Publication Number Publication Date
JPS60262895A true JPS60262895A (en) 1985-12-26
JPH0550558B2 JPH0550558B2 (en) 1993-07-29

Family

ID=14734416

Family Applications (1)

Application Number Title Priority Date Filing Date
JP11834684A Granted JPS60262895A (en) 1984-06-11 1984-06-11 Manufacture of granular detergent

Country Status (1)

Country Link
JP (1) JPS60262895A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0385748A2 (en) * 1989-03-02 1990-09-05 Unilever Plc Agglomerates for addition to detergent powders
CN109415656A (en) * 2016-06-30 2019-03-01 狮王株式会社 Coat alpha-sulfo-fatty acid alkyl ester salt particle swarm

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5152404A (en) * 1974-09-06 1976-05-10 Unilever Nv Senzaisoseibutsunoseizoho
JPS53114807A (en) * 1977-03-18 1978-10-06 Lion Corp Modification of ranulated detergent

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5152404A (en) * 1974-09-06 1976-05-10 Unilever Nv Senzaisoseibutsunoseizoho
JPS53114807A (en) * 1977-03-18 1978-10-06 Lion Corp Modification of ranulated detergent

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0385748A2 (en) * 1989-03-02 1990-09-05 Unilever Plc Agglomerates for addition to detergent powders
CN109415656A (en) * 2016-06-30 2019-03-01 狮王株式会社 Coat alpha-sulfo-fatty acid alkyl ester salt particle swarm

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