JPS60133096A - Manufacture of granular detergent composition - Google Patents

Manufacture of granular detergent composition

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Publication number
JPS60133096A
JPS60133096A JP24002083A JP24002083A JPS60133096A JP S60133096 A JPS60133096 A JP S60133096A JP 24002083 A JP24002083 A JP 24002083A JP 24002083 A JP24002083 A JP 24002083A JP S60133096 A JPS60133096 A JP S60133096A
Authority
JP
Japan
Prior art keywords
fatty acid
acid ester
sulfo fatty
granular detergent
detergent composition
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.)
Pending
Application number
JP24002083A
Other languages
Japanese (ja)
Inventor
豊之 佐藤
向山 恒治
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 JP24002083A priority Critical patent/JPS60133096A/en
Publication of JPS60133096A publication Critical patent/JPS60133096A/en
Pending 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】 本発明は、α−スルホ脂肪酸エステル塩を含む洗剤組成
物であって、長期に保存した場合にもα−そルホ脂肪酸
エステル塩の加水分解が抑制された粒状洗剤組成物に関
す乙。
Detailed Description of the Invention The present invention provides a granular detergent composition containing an α-sulfo fatty acid ester salt, which suppresses hydrolysis of the α-sulfo fatty acid ester salt even when stored for a long period of time. Party related to things.

近年、洗剤中のリン酸塩が環境上の理由から規制される
方向にあ如、リン酸塩を用いることなくと本皮好々洗浄
力や粉体物性が得られる粒状洗剤の検討が、リン酸塩の
代替ビルダーや界面活性剤それ自体の四点からなされて
いる。
In recent years, phosphates in detergents have been regulated for environmental reasons, and research has begun on granular detergents that can provide good detergency and powder properties without using phosphates. It has been made from four points: an alternative builder to the acid salt and a surfactant itself.

この中でもα−スルホ脂肪酸エステル塩は、洗浄力、汚
れ分散性に優れ、しか屯、カルシウム不感性であって硬
度の高い沈水中でも洗浄力を発揮することから注目され
ており、特開昭47−6276号公報、同47−125
82号公報などにこの活性剤を用いた粒状洗剤が報告さ
れている。
Among these, α-sulfo fatty acid ester salts have attracted attention because they have excellent detergency and dirt dispersibility, are insensitive to calcium, and exhibit detergency even in submerged water with high hardness. Publication No. 6276, 47-125
Granular detergents using this activator have been reported in Publication No. 82 and others.

しかしながら、α−スルホ脂肪酸エステル塩は、噴霧乾
燥による製造に際してやその後の保存時におりて、加水
分解によりエステル結合が切断され、水に難溶で界面活
性能も之しいa −スルホ脂肪酸ジ塩に変化しやすいと
いう問題があった。
However, during production by spray drying and subsequent storage, the ester bond of α-sulfo fatty acid ester salts is broken by hydrolysis, resulting in α-sulfo fatty acid di-salts that are sparingly soluble in water and have no surface activity. The problem was that it was easy to change.

この対策としては、たとえば特開昭52−117908
号公報に、α−スルホ脂肪酸エステル塩を含有する洗剤
スラリーにポリエチレングリコールを添加し、噴霧乾燥
時のα−スルホ脂肪酸エステル塩の加水分解を防止する
ことが報告されている。また、特開昭50−15190
5号公報には、粒状洗剤中のa−スルホ脂肪酸エステル
塩が保存中にエステル結合の切断を受けやすいこと、お
よび、これは粒状洗剤を噴霧乾燥で調製する際に助長さ
れることが報告され、この対策としてヒンダードフェノ
ール系化合物とヒドロキシポリカル2ン酸またはその塩
との併用が提案されている。
As a countermeasure against this, for example, Japanese Patent Application Laid-Open No. 52-117908
It is reported in the above publication that polyethylene glycol is added to a detergent slurry containing an α-sulfo fatty acid ester salt to prevent hydrolysis of the α-sulfo fatty acid ester salt during spray drying. Also, JP-A-50-15190
Publication No. 5 reports that a-sulfo fatty acid ester salts in granular detergents are susceptible to ester bond cleavage during storage, and that this is facilitated when granular detergents are prepared by spray drying. As a countermeasure against this problem, the combined use of a hindered phenol compound and a hydroxypolycardiphosphoric acid or a salt thereof has been proposed.

さらに、特開昭52−28507号公報には、a−スル
ホ脂肪酸エステル塩がケイ酸ナトリウムのようなアルカ
リビルダーの共存下に経時的に加水分解しやすいことか
ら、特定のアルカリビルダーの使用が提案されている。
Furthermore, JP-A No. 52-28507 proposes the use of a specific alkali builder because a-sulfo fatty acid ester salts tend to be hydrolyzed over time in the coexistence of alkali builders such as sodium silicate. has been done.

しかし、上記の対策は未だ十分々本のではなく、特に保
存安定性が十分でないことは市場において経日劣化を紹
〈ことになり、その改善がまたれていた。また、衣料用
の洗剤にあってはアルカリビルダーは必須の成分であり
、粉体物性の上からも必要な成分であることから、汎用
のアルカリビルダーとa−スルホ脂肪酸エステル塩とを
長期にわたって安定に共存させることが望まれていた。
However, the above-mentioned measures are still insufficient, and in particular, the lack of storage stability has led to deterioration over time in the market, and improvements have been delayed. In addition, alkaline builder is an essential ingredient in laundry detergents, and it is also a necessary ingredient from the standpoint of powder physical properties. It was hoped that they would coexist.

本発明者らは上記観点から鋭意検討した給茶、a−スル
ホ脂肪酸エステル塩を配合した粒状洗剤を、酸性気体で
気−面接触処理することにより、α−スルホ脂肪酸エス
テル塩の経時による加水分解が抑制され、しかも、汎用
のアルカリビルダーとの共存下にあっても加水分解が抑
制されることを見出し、この知見に基いて本発明を完成
するに至った。
The present inventors have intensively studied from the above viewpoint, and by subjecting a granular detergent containing α-sulfo fatty acid ester salt to air-surface contact treatment with acidic gas, hydrolysis of α-sulfo fatty acid ester salt over time has been achieved. It was discovered that hydrolysis was suppressed even in the coexistence with a general-purpose alkali builder, and based on this knowledge, the present invention was completed.

す々わち、本発明の粒状洗剤組成物の製造方法は、a−
スルホ脂肪酸エステルを含む粒状洗剤を、酸性気体によ
シ気−°固接触処理することを特徴とする。
That is, the method for producing the granular detergent composition of the present invention comprises a-
The present invention is characterized in that a granular detergent containing a sulfo fatty acid ester is subjected to gas-solid contact treatment with an acidic gas.

本発明で主要活性剤成分として用いられるa−スルホ脂
肪酸エステル塩は、一般式(I)(式中、R,およびR
3はアルキル基であり、Mは陽イオンである。) で表わされ為化合物であシ、式中のR1としては炭素数
4〜20のアルキル基が、また、R2としては炭素数工
〜6のアルキル基が適当であジ、これらは直鎖状でも分
岐鎖状でもよい。また、R1としてはメチル基、エチル
基、n−プロピル基、イソプロピル基が好適である。M
としてはナトリウム、カリウムなどのアルカリ金属が好
適であシ、他にアンモニウム、マグネジ+7 A fx
どが例示される。このよりなa−スルホ脂肪酸エステル
塩は、たとえば炭素数6〜22の脂肪酸を原料として常
法に従って製造することができ、原料脂肪酸としては硬
化牛脂脂肪酸、硬化パーム油脂肪酸が好ましい。
The a-sulfo fatty acid ester salt used as the main active agent component in the present invention has the general formula (I) (wherein R, and R
3 is an alkyl group, and M is a cation. ) In the formula, R1 is suitably an alkyl group having 4 to 20 carbon atoms, and R2 is suitably an alkyl group having 6 to 6 carbon atoms, and these are straight-chain It may be in the form of a chain or a branched chain. Moreover, as R1, a methyl group, an ethyl group, an n-propyl group, and an isopropyl group are suitable. M
Alkali metals such as sodium and potassium are preferable, and ammonium and magnetic screw +7A fx are also suitable.
Examples include: This solid a-sulfo fatty acid ester salt can be produced by a conventional method using, for example, a fatty acid having 6 to 22 carbon atoms as a raw material, and hydrogenated beef tallow fatty acid or hydrogenated palm oil fatty acid is preferable as the raw fatty acid.

α−スルホ脂肪酸エステル塩を含む粒状洗剤は、たとえ
ば、α−スルホ脂肪酸エステル塩を、あるいはさらに必
要により他の活性剤成分、ビルダーなどの洗剤成分を含
む洗剤スラリーを噴霧乾燥したわ、a−スルホ脂肪酸エ
ステル塩を含む洗剤組成物を造粒する々どして粉粒状と
することにより得られる。
Granular detergents containing α-sulfo fatty acid ester salts can be prepared, for example, by spray-drying a detergent slurry containing α-sulfo fatty acid ester salts or, if necessary, detergent components such as other active ingredients and builders. It is obtained by granulating a detergent composition containing a fatty acid ester salt into powder.

本発明では、このようにして得られる粒状洗剤に対して
酸性気体による気−面接触処理を施す。気−面接触処理
は移動層、充填l−1流動!−又は内部を酸性気体雰囲
気にした回転容器などにより行なうことができるが、効
率の面からは流動層または充填層が好ましい。この処理
は別途に気−面接触処理装置を設けて行々うこともでき
るが、エアーリフトなどの粉体輸送装置の搬送気体とし
て酸性ガスを用い、搬送と同時に処理を施すこともでき
る。酸性気体と1.ではCO□ガスが最も適当であり、
その他so、 、 nozガスも使用できる。また、必
要応じこれらの酸性気体を空気などの非酸性気体によ如
希釈して用いてもよい。処理ガス貴は希釈ガス比、処理
時間と密接な関係にあるが、製造工程での効率よい処理
を行うには洗剤1 Kg当り20t/min以上の濃度
50係程度のガスで0.1〜5分程度処理することが好
ましい。
In the present invention, the granular detergent thus obtained is subjected to air-surface contact treatment with acidic gas. Air-surface contact treatment is a moving bed, packed l-1 flow! - or a rotating container with an acidic gas atmosphere inside, but from the viewpoint of efficiency, a fluidized bed or a packed bed is preferred. This treatment can be carried out by providing a separate air-surface contact treatment device, but it is also possible to carry out the treatment simultaneously with the transportation by using acidic gas as the carrier gas in a powder transportation device such as an air lift. Acid gas and 1. Then, CO□ gas is the most suitable,
Other SO, NOZ gases can also be used. Further, if necessary, these acidic gases may be diluted with a non-acidic gas such as air. The processing gas density is closely related to the dilution gas ratio and processing time, but in order to perform efficient processing in the manufacturing process, it is necessary to use a gas with a concentration of about 50% at a rate of 20t/min or more per 1 kg of detergent. It is preferable to process for about a minute.

本発明の粒状洗剤組成物中には、さらに必要に応じて以
下の任意成分を含有することができる。これらの成分と
しては、アルキルベンゼンスルホン酸塩、アルキルスル
ホン酸塩、a−オレフィンスルホン酸塩、アルキル硫酸
塩、アルキルポリエーテル硫酸塩、脂肪酸石けんなどの
アニオン界面活性剤、アルキルエトキシレート、アルキ
ルフェニルエトキシレート、アルキルアルカノールアマ
イドなどのノニオン界面活性剤、アルキルベタインなど
の両性界面活性剤、ケイ酸ナトリウム、炭酸ナトリウム
、炭酸水素ナトリウム、トリポリリン酸ナトリウム、ビ
ロリン酸ナトリウム、ゼオライト、硫酸ナトリウムなど
の無機ビルダー、クエン酸ナトリウム、エチレンジアミ
ン四酢酸ナトリウム、ニトリロ三酢酸ナトリウム々どの
有機ビルダーが挙げられる。
The granular detergent composition of the present invention may further contain the following optional components as required. These ingredients include alkylbenzene sulfonates, alkyl sulfonates, a-olefin sulfonates, alkyl sulfates, alkyl polyether sulfates, anionic surfactants such as fatty acid soaps, alkyl ethoxylates, and alkylphenyl ethoxylates. , nonionic surfactants such as alkyl alkanolamides, amphoteric surfactants such as alkyl betaines, inorganic builders such as sodium silicate, sodium carbonate, sodium bicarbonate, sodium tripolyphosphate, sodium birophosphate, zeolite, sodium sulfate, citric acid. Examples include organic builders such as sodium, sodium ethylenediaminetetraacetate, sodium nitrilotriacetate, and the like.

その他ポリエチレングリコール、カルゼキシメチルセル
ロース、酵素、香料、色素なども含有することができる
。これら成分は洗剤スラリー中にα−スルホ脂肪酸エス
テル塩とともに配合し噴霧乾燥するなどして粉粒体とし
、洗剤粒子中に共存せしめてもよく、また、別個に粉粒
体とし粉体ブレンドしてもよい。この粉体ブレンドは酸
性気体による処理の前後いずれでもよい。
In addition, polyethylene glycol, calxoxymethyl cellulose, enzymes, fragrances, pigments, etc. can also be contained. These components may be blended together with α-sulfo fatty acid ester salts in a detergent slurry and spray-dried to form a powder and coexist in the detergent particles, or they may be made into a powder and blended separately. Good too. This powder blend may be prepared either before or after treatment with acidic gas.

本発明の製造方法によれば、α−スルホ脂肪酸エステル
塩を含む粒状洗剤を酸性気体を用いて気−面接触処理す
ることにより、アルカリビルダーの存在下にあっても、
α−スルホ脂肪酸エステル塩の経時による分解が有効に
抑制され、長期保存時における洗剤組成物の性能の劣化
を防止することができる。
According to the production method of the present invention, even in the presence of an alkali builder, by subjecting a granular detergent containing an α-sulfo fatty acid ester salt to air-surface contact treatment using an acidic gas,
Decomposition of the α-sulfo fatty acid ester salt over time is effectively suppressed, and deterioration of the performance of the detergent composition during long-term storage can be prevented.

実施例1〜8 噴霧乾燥によ−り以下の組成の粒状洗剤を調製した。Examples 1-8 A granular detergent having the following composition was prepared by spray drying.

α−スルホ脂肪酸メチルエステルのナトリウム塩15w
t%(脂肪酸残基の炭素数:14〜18) 08.〜,6アルキル硫酸ナトリウム xowt12号
珪曹 10w1% ゼオライト l Owlチ 水 分 4wt% 芒 硝 ノ々ランス これらの粒状洗剤に対し、第1表に示した酸性気体によ
り流動層装置を用いて接触処理し、本発明の粒状洗剤組
成物を作成した(実施例1〜8)。また、対照として未
処哩のもの(比較例1)および空気で接触処理した粒状
洗剤組成物(比較例2)を作成した。
Sodium salt of α-sulfo fatty acid methyl ester 15w
t% (number of carbon atoms in fatty acid residue: 14-18) 08. ~, 6 Sodium alkyl sulfate xowt No. 12 silica 10w1% Zeolite l Owl water 4wt% Soybean salt Noronance These granular detergents were subjected to contact treatment using a fluidized bed apparatus with the acidic gas shown in Table 1. , granular detergent compositions of the present invention were prepared (Examples 1 to 8). In addition, as controls, an untreated granular detergent composition (Comparative Example 1) and a granular detergent composition subjected to contact treatment with air (Comparative Example 2) were prepared.

これらの組成物の加水分解増加率を以下の方法により測
定し、その結果を第1表に示した。
The rate of increase in hydrolysis of these compositions was measured by the following method, and the results are shown in Table 1.

全界面活性剤量をメチレンゾル−逆滴定法によってめ、
あらかじめ設定した界面活性剤の配合比率からα−スル
ホ脂肪酸エステル塩とα−スルホ脂脂肪レジ塩の合計i
Mをめる。次に、洗剤組成物をp’)IlF、50℃の
90%エタノール溶液で処理し、α−スルホ脂脂肪レジ
塩不溶分として分離する。このジ塩を50%エタノール
溶液に溶解し、メチレンブルー逆滴定法によ如ジ塩の−
518をめ、次式より加水分解率りをめる。
Determine the total amount of surfactant by methylene sol back titration method,
The total i of α-sulfo fatty acid ester salt and α-sulfo fatty acid resin salt is determined from the preset blending ratio of surfactants.
Enter M. Next, the detergent composition is treated with p')IIF, a 90% ethanol solution at 50° C., and is separated as an α-sulfolipid fat resin insoluble fraction. This di-salt was dissolved in a 50% ethanol solution, and the di-salt was determined by methylene blue back titration.
518, and calculate the hydrolysis rate from the following formula.

D :、 −X 100 上記操作によね、洗剤組成物の製造直後および35℃で
1ケ月放置後の加水分解率をめ、次式によシ加水分解増
加率を算出する。
D:, -X 100 According to the above operation, the hydrolysis rate is calculated immediately after the detergent composition is produced and after being left at 35°C for one month, and the rate of increase in hydrolysis is calculated according to the following formula.

加水分解増加率=(1ケ月後の加水分解率)−(製造直
後の加水分解率) (以下余白) 実施例9〜12 実施例1と同様にして粒状洗剤をKS’JJし、第2表
に示す00./空気比の輸送媒体を用いてエアーリフト
(内径9m、長さ20犠、風速15第2表
Hydrolysis increase rate = (Hydrolysis rate after 1 month) - (Hydrolysis rate immediately after production) (Left below blank) Examples 9 to 12 Granular detergents were subjected to KS'JJ in the same manner as in Example 1, and Table 2 00. / air ratio using an air lift (inner diameter 9 m, length 20 m, wind speed 15 Table 2)

Claims (1)

【特許請求の範囲】[Claims] 1 α−スルホ脂肪酸エステル塩を含む粒状洗剤を酸性
気体により気−同接触処理することを特徴とする粒状洗
剤組成物の製造方法。
1. A method for producing a granular detergent composition, which comprises subjecting a granular detergent containing an α-sulfo fatty acid ester salt to a gas-contact treatment with an acidic gas.
JP24002083A 1983-12-20 1983-12-20 Manufacture of granular detergent composition Pending JPS60133096A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP24002083A JPS60133096A (en) 1983-12-20 1983-12-20 Manufacture of granular detergent composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP24002083A JPS60133096A (en) 1983-12-20 1983-12-20 Manufacture of granular detergent composition

Publications (1)

Publication Number Publication Date
JPS60133096A true JPS60133096A (en) 1985-07-16

Family

ID=17053266

Family Applications (1)

Application Number Title Priority Date Filing Date
JP24002083A Pending JPS60133096A (en) 1983-12-20 1983-12-20 Manufacture of granular detergent composition

Country Status (1)

Country Link
JP (1) JPS60133096A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62116698A (en) * 1985-11-15 1987-05-28 花王株式会社 High concentration aqueous solution of alpha-sulfo-fatty acid ester

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62116698A (en) * 1985-11-15 1987-05-28 花王株式会社 High concentration aqueous solution of alpha-sulfo-fatty acid ester

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