JPS6141350B2 - - Google Patents

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Publication number
JPS6141350B2
JPS6141350B2 JP1340378A JP1340378A JPS6141350B2 JP S6141350 B2 JPS6141350 B2 JP S6141350B2 JP 1340378 A JP1340378 A JP 1340378A JP 1340378 A JP1340378 A JP 1340378A JP S6141350 B2 JPS6141350 B2 JP S6141350B2
Authority
JP
Japan
Prior art keywords
aqueous slurry
solid content
higher alkyl
powder
spray
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.)
Expired
Application number
JP1340378A
Other languages
Japanese (ja)
Other versions
JPS54106428A (en
Inventor
Norihiro Oono
Masanobu Nakamura
Akira Hayashi
Toshiaki Oogoshi
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 JP1340378A priority Critical patent/JPS54106428A/en
Publication of JPS54106428A publication Critical patent/JPS54106428A/en
Publication of JPS6141350B2 publication Critical patent/JPS6141350B2/ja
Granted legal-status Critical Current

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Description

【発明の詳細な説明】[Detailed description of the invention]

本発明は高級アルキル硫酸塩を含有する水性ス
ラリーの粉粒化方法に関する。 高級アルキル硫酸塩は代表的なアニオン活性剤
の一つであつて、他の界面活性剤及び/又はビル
ダーと組み合わせて台所用洗剤乃至シヤンプー等
に汎用されている外、粉末状のシヤンプー、洗浄
剤、発泡剤等を製造する際の中間原料として、高
級アルキル硫酸塩を粉粒状にして使用する例も多
い。一般に界面活性剤を含有する粉粒体は、吸湿
に原因してサラサラ性を失つたり、固結したりす
る問題があり、高級アルキル硫酸塩を含む粉粒体
もその例外ではない。本発明は、高級アルキル硫
酸塩を主成分とする粉粒体を、粉体物性が良好で
かつ嵩密度が比較的大きく、しかも粒子強度が高
い状態で取得できる方法を提供する。 周知の通り、高級アルキル硫酸塩を主成分とす
る粉粒体は、高級アルキル硫酸塩及びその他の添
加剤を含有する水性スラリーを調製し、このスラ
リーを噴霧乾燥することにより製造される。高級
アルキル硫酸塩に限らず水性スラリーを噴霧乾燥
して粉粒体を製造する場合、得られる粉粒体の嵩
密度と粒子強度とは、使用した噴霧乾燥の種類及
び乾燥条件にもよるが、一般的には噴霧乾燥に供
した水性スラリーの含水量に依存し、これが少な
い程得られる粉粒体の嵩密度と粒子強度は増大す
る傾向を示す。しかしながら、含水量を少なくす
ると水性スラリーの粘度は急激に増大するため、
これを噴霧乾燥することが難しく、事実水性スラ
リーの含水量が60〜70%以下に低下すると、噴霧
乾燥操作は著しく困難となる。こうした実情か
ら、噴霧乾燥によつて粉粒体を得んとする場合に
は、水性スラリーの粘度を増大させることなくそ
の含水量を低下させる工夫が従前から数多く試み
られている。 メタノール等の低級アルコールを添加する方法
はそうした工夫の代表例であるが、その外、石鹸
スラリーに低級脂肪酸アルカリ塩又は低級脂肪酸
ポリアルキレングリコールエステルを添加する方
法(特公昭36−23860号公報)、直鎖アルキルベン
ゼンスルホン酸塩スラリーに無機塩を介在させる
方法(特公昭46−11171号公報)、高級アルコール
硫酸塩スラリー等に対してポリエチレングリコー
ルを添加する方法(特開昭50−116383号公報)、
過剰のアルカリを添加する方法(特開昭52−
80285号公報)、あるいは逆にアニオン活性剤の部
分中和物を用いる方法(特開昭52−80309号公
報)等が提案されている。 しかし、低級アルコールの添加は噴霧乾燥時に
低級アルコールが揮散するため不経済であるばか
りでなく、火災もしくは爆発の危険を伴う点で
も、ま大気汚染の原因となる点でも好ましくな
い。一方、特定な添加物を使用するその他の方法
は、添加物を多量に用いなければ所期の効果を上
げることができないこともさることながら、粉粒
体中に添加物がそのまま残るため、それぞれの添
加物の種類によつて得られる粉粒体の用途が限定
されるという欠点があつた。 本発明者等は高級アルキル硫酸塩を主成分とす
る水性スラリーを噴霧乾燥して得られる粉粒体の
粉体物性を改良し、併せてその嵩密度と粒子強度
を増大させるべく、高級アルキル硫酸塩水性スラ
リーの物性について鋭意研究を重ねた結果、当該
スラリーは固型分濃度が40重量%以上(従つて含
水量は60重量%以下)になると粘度が急激に高く
なり、50重量%ではゲル状を呈するが、固型分濃
度をさらに増大させると、粘度は一旦低下して再
び上昇するとの知見を得た。そして固型分濃度70
重量%前後の領域に小さな粘度極小値があること
を究明した。従つて、この粘度極小値を持つ水性
スラリーを噴霧乾燥すれば、粉体物性が良好で嵩
密度も比較的大きく、粒子強度も高い高級アルキ
ル硫酸塩を主成分とする粉粒体を得ることができ
る。 本発明はこれらの知見を基礎に完成されたもの
であつて、その基本的な特徴点は高級アルキル硫
酸塩を主な固型分として含有する水性スラリー
を、固型分濃度60〜80重量%に調整すると共にそ
の温度を50〜120℃に保持し、この水性スラリー
を常法通り噴霧乾燥することにある。 本発明の水性スラリーは高級アルキル硫酸塩を
主な固型分とするが、その高級アルキル硫酸塩は
下記の一般式で表示される。 RSO4M ここでRは炭素数8〜18、好ましくは10〜16の
直鎖又は分岐アルキル基又はアルケニル基を示
し、Mはアルカリ金属を、好ましくはNaを示
す。上記の高級アルキル硫酸塩は、例えば抹香鯨
油からの天然高級アルコール、ヤシ脂肪酸、牛脂
脂肪酸等の天然脂肪酸からの還元アルコール、ワ
ツクスクラツキング或いはエチレンの重合等によ
り得られたα−オレフインのオキソ合成による高
級合成アルコールを原料とし、これら原料アルコ
ールをSO3によつて薄膜硫酸化するか、クロルス
ルホン酸によつて硫酸化することにより製造する
ことができる。 本発明の水性スラリーには必要に応じて、珪
酸、炭酸、硫酸、燐酸、クエン酸のアルカリ金属
塩等のビルダー、CMC(カルボキシメチルセル
ロース)等の再汚染防止剤、BHT(ブチルヒド
ロキシトルエン)、BHA(ブチルヒドロキシアニ
ソール)等の酸化防止剤、MgSO4等の添加剤を
少量添加してもよい。また硫酸化副生塩の食塩、
芒硝等が少量含まれてもよい。 しかし、これら任意成分の添加量はスラリー固
型分の10重量%以下とし、固型分中の高級アルキ
ル硫酸塩量を90重量%以上に維持することを可と
する。 既述した通り、本発明の水性スラリーはその固
型分濃度を60〜80重量%、好ましくは70〜78重量
%の範囲に調整することを要件とし、この濃度が
60重量%以下に低下した場合(但し40重量%以下
を除く)及び80重量%以上に上昇した場合は、何
れも水性スラリーはゲル化状態を呈して噴霧乾燥
が困難となり、仮令噴霧乾燥できても良質な粉粒
体を得ることができない。 噴霧乾燥時の水性スラリー温度は50〜120℃、
好ましくは70〜110℃に保持することを可とし、
50℃を下廻る場合はスラリーの粘度が急激に上昇
し、噴霧乾燥が困難となつたり、噴霧乾燥できて
も粉体物性が劣る。120℃を上廻る場合はスラリ
ー中のアルキル硫酸塩の分解が起り好ましくな
い。 本発明の噴霧乾燥は、通常の噴霧乾燥装置を使
用して通常の噴霧乾燥条件下にこれを行なうこと
ができる。 以上詳述したところから明らかな通り、本発明
は高級アルキル硫酸塩を主成分とする水性スラリ
ーを、固型分濃度が高い状態で噴霧乾燥するもの
であるから、得られる粉粒体は粉体物性が良好
で、特にその嵩密度及び粒子強度が高い。従つて
当該粉粒体は良好な貯蔵安定性を示す。さらにま
た本発明の水性スラリーは、固型分濃度が高いに
も拘らず比較的低粘度であるので、これを噴霧乾
燥した場合の効率が高い。従つて本発明は粉粒体
製造に際しての経費節減をも約束するものであ
る。 実施例 1 鎖長を異にする直鎖アルキル硫酸ナトリウムの
混合物(但し、C10;20%、C12;65%、C14;15
%)と少量の硫酸ナトリウムを使用して、固型分
濃度が異なる水性スラリーを調製し、この水性ス
ラリーを下記の条件で噴霧乾燥して得られた粉粒
体の粉体物性及び乾燥効率を比較した。結果を表
1に示す。 噴霧乾燥条件;装置 デイスク型スプレー乾燥機 熱風温度 約150〜200℃ 熱風の向き 並流
The present invention relates to a method for pulverizing an aqueous slurry containing higher alkyl sulfates. Higher alkyl sulfates are one of the typical anionic surfactants and are widely used in kitchen detergents and shampoos in combination with other surfactants and/or builders, as well as powdered shampoos and cleaning agents. There are many cases in which higher alkyl sulfates are used in the form of powder as an intermediate raw material in producing foaming agents and the like. Generally, powders containing surfactants have a problem of losing their smoothness or solidifying due to moisture absorption, and powders containing higher alkyl sulfates are no exception to this problem. The present invention provides a method for obtaining powder or granular material containing higher alkyl sulfate as a main component with good powder physical properties, relatively high bulk density, and high particle strength. As is well known, powders containing higher alkyl sulfates as a main component are produced by preparing an aqueous slurry containing higher alkyl sulfates and other additives, and spray-drying this slurry. When producing powder by spray drying an aqueous slurry of not only higher alkyl sulfates, the bulk density and particle strength of the resulting powder vary depending on the type of spray drying used and the drying conditions. In general, it depends on the water content of the aqueous slurry subjected to spray drying, and as the water content decreases, the bulk density and particle strength of the resulting powder tend to increase. However, as the water content decreases, the viscosity of the aqueous slurry increases rapidly;
This is difficult to spray dry, and in fact as the water content of the aqueous slurry falls below 60-70%, the spray drying operation becomes extremely difficult. Under these circumstances, many attempts have been made to reduce the water content of an aqueous slurry without increasing its viscosity when obtaining powder or granules by spray drying. The method of adding a lower alcohol such as methanol is a typical example of such a device, but there are also methods of adding a lower fatty acid alkali salt or lower fatty acid polyalkylene glycol ester to the soap slurry (Japanese Patent Publication No. 36-23860), A method of intervening an inorganic salt in a linear alkylbenzene sulfonate slurry (Japanese Patent Publication No. 11171/1971), a method of adding polyethylene glycol to a higher alcohol sulfate slurry, etc. (Japanese Patent Application Laid-open No. 116383/1983),
Method of adding excess alkali
80285) or, conversely, a method using a partially neutralized anionic activator (Japanese Patent Application Laid-open No. 80309/1983). However, the addition of lower alcohols is not only uneconomical since the lower alcohols volatilize during spray drying, but is also undesirable in that it is accompanied by the risk of fire or explosion, and is also a cause of air pollution. On the other hand, other methods that use specific additives require the use of large amounts of additives to achieve the desired effect, and the additives remain in the powder or granules, so The drawback is that the applications of the resulting powder and granules are limited depending on the type of additive. The present inventors aimed to improve the powder physical properties of powder obtained by spray drying an aqueous slurry containing higher alkyl sulfates as a main component, and to increase the bulk density and particle strength of higher alkyl sulfates. As a result of intensive research on the physical properties of salt water slurry, we found that the viscosity of the slurry increases rapidly when the solid content concentration is 40% by weight or more (therefore, the water content is 60% by weight or less), and at 50% by weight it becomes a gel. However, it was found that when the solid content concentration was further increased, the viscosity decreased once and then increased again. and solid content concentration 70
It was determined that there is a small viscosity minimum in the region of around % by weight. Therefore, by spray-drying an aqueous slurry having this minimum viscosity value, it is possible to obtain a powder mainly composed of higher alkyl sulfate, which has good powder physical properties, relatively large bulk density, and high particle strength. can. The present invention was completed based on these findings, and its basic feature is that an aqueous slurry containing higher alkyl sulfates as the main solid content is prepared at a solid content of 60 to 80% by weight. and maintain the temperature at 50 to 120°C, and spray dry this aqueous slurry in a conventional manner. The aqueous slurry of the present invention has a higher alkyl sulfate as the main solid content, and the higher alkyl sulfate is represented by the following general formula. RSO 4 M Here, R represents a straight chain or branched alkyl group or alkenyl group having 8 to 18 carbon atoms, preferably 10 to 16 carbon atoms, and M represents an alkali metal, preferably Na. The above-mentioned higher alkyl sulfates are, for example, natural higher alcohols from matcha whale oil, reduced alcohols from natural fatty acids such as coconut fatty acids and beef tallow fatty acids, wax cracking, or oxo-synthesis of α-olefins obtained by polymerization of ethylene. It can be produced by using higher synthetic alcohols as raw materials and sulfating these raw material alcohols with a thin film using SO 3 or sulfating them with chlorosulfonic acid. The aqueous slurry of the present invention may contain builders such as alkali metal salts of silicic acid, carbonic acid, sulfuric acid, phosphoric acid, and citric acid, recontamination preventive agents such as CMC (carboxymethylcellulose), BHT (butylated hydroxytoluene), and BHA. A small amount of an antioxidant such as (butylhydroxyanisole) or an additive such as MgSO 4 may be added. Also, sulfated by-product salt,
A small amount of Glauber's salt etc. may be included. However, the amount of these optional components added should be 10% by weight or less of the solid content of the slurry, making it possible to maintain the amount of higher alkyl sulfates in the solid content at 90% by weight or more. As mentioned above, the aqueous slurry of the present invention is required to have a solid content concentration in the range of 60 to 80% by weight, preferably 70 to 78% by weight;
If the slurry decreases to 60% by weight or less (excluding 40% by weight or less) or increases to 80% by weight or more, the aqueous slurry becomes gelled and spray drying becomes difficult, making spray drying impossible. However, it is not possible to obtain high-quality powder or granules. The aqueous slurry temperature during spray drying is 50~120℃,
Preferably, it can be maintained at 70 to 110°C,
If the temperature is below 50°C, the viscosity of the slurry will increase rapidly, making spray drying difficult, or even if spray drying is possible, the powder properties will be poor. If the temperature exceeds 120°C, the alkyl sulfate in the slurry will decompose, which is not preferable. The spray drying of the present invention can be carried out using conventional spray drying equipment and under conventional spray drying conditions. As is clear from the above detailed description, the present invention involves spray drying an aqueous slurry containing higher alkyl sulfate as a main component in a state where the solid content concentration is high. It has good physical properties, especially its bulk density and particle strength. Therefore, the powdered material exhibits good storage stability. Furthermore, the aqueous slurry of the present invention has a relatively low viscosity despite its high solid content concentration, and therefore has high efficiency when spray-dried. Therefore, the present invention also promises cost savings in the production of powder and granular materials. Example 1 A mixture of linear alkyl sodium sulfates with different chain lengths (C 10 ; 20%, C 12 ; 65%, C 14 ; 15
%) and a small amount of sodium sulfate to prepare aqueous slurries with different solid content concentrations, and then spray-dry this aqueous slurry under the following conditions to evaluate the powder physical properties and drying efficiency of the resulting powder. compared. The results are shown in Table 1. Spray drying conditions: Equipment Disk type spray dryer Hot air temperature Approximately 150 to 200℃ Hot air direction Parallel flow

【表】 表1から明らかな通り、本発明に準ずる実験
No.4、5の場合のみ、良好な粉体物性を備えた
粉粒体を得ることができ、乾燥効率も高い。 実施例 2 高級アルキル硫酸塩として、鎖長を異にする直
鎖アルキル硫酸ナトリウムの混合物(但し、
C12;65%、C14;25%、C16;10%)を使用し、
噴霧乾燥装置にノズル型噴霧乾燥機を使用した以
外は実施例1と全く同様な実験を行なつて、表2
に示す如き結果を得た。
[Table] As is clear from Table 1, experiments according to the present invention
Only in the case of Nos. 4 and 5, powder with good powder physical properties can be obtained and the drying efficiency is also high. Example 2 As a higher alkyl sulfate, a mixture of linear alkyl sodium sulfates with different chain lengths (however,
C 12 ; 65%, C 14 ; 25%, C 16 ; 10%),
An experiment was conducted in the same manner as in Example 1, except that a nozzle-type spray dryer was used as the spray dryer, and Table 2 was obtained.
The results shown are obtained.

【表】 実施例 3 実施例1で使用した直鎖アルキル硫酸ナトリウ
ムと硫酸ナトリウムに、各種の添加物を加えて、
固型分濃度が異なる水性スラリーを調製し、この
スラリーを実施例1と同一条件で噴霧乾燥して得
られた粉粒体の粉体物性を比較した。但し、乾燥
装置にはノズル型噴霧乾燥機を使用した。結果を
表3に示す。
[Table] Example 3 Various additives were added to the linear alkyl sodium sulfate and sodium sulfate used in Example 1,
Aqueous slurries having different solid content concentrations were prepared, and the slurries were spray-dried under the same conditions as in Example 1, and the powder physical properties of the resulting powders were compared. However, a nozzle type spray dryer was used as the drying device. The results are shown in Table 3.

【表】【table】

【表】 表3に示す結果から明らかな通り、水性スラリ
ー中に高級アルキル硫酸塩以外の任意固型分を加
えても、その量が固型分全体の10%以下であり、
且つその水性スラリーが本発明の要件を満足して
噴霧乾燥される限り、粉体物性に優れた粉粒体を
得ることができる。
[Table] As is clear from the results shown in Table 3, even if any solid content other than higher alkyl sulfate is added to the aqueous slurry, the amount will be less than 10% of the total solid content,
In addition, as long as the aqueous slurry is spray-dried while satisfying the requirements of the present invention, powder and granules with excellent powder physical properties can be obtained.

Claims (1)

【特許請求の範囲】 1 一般式RSO4M(ここでRは炭素数8〜18の
直鎖又は分岐アルキル基又はアルケニル基を示
し、Mはアルカリ金属を示す)で表わされる高級
アルキル硫酸塩を主な固型分として含有する水性
スラリーを、噴霧乾燥して粉粒化するに当り、前
記水性スラリーの固型分濃度を60〜80重量%に調
整すると共に、その温度を50〜120℃に保持して
これを噴霧乾燥することを特徴とする前記水性ス
ラリーの粉粒化法。 2 前記水性スラリー中の固型分の高級アルキル
硫酸塩含有量が90重量%以上である特許請求の範
囲第1項記載の方法。 3 一般式RSO4MのRが炭素数10〜16の直鎖又
は分岐アルキル基又はアルケニル基である特許請
求の範囲第1項記載の方法。 4 一般式RSO4MのMがナトリウムである特許
請求の範囲第1項記載の方法。 5 前記水性スラリーの温度を70〜110℃に保持
する特許請求の範囲第1項記載の方法。
[Claims] 1. A higher alkyl sulfate represented by the general formula RSO 4 M (where R represents a linear or branched alkyl group or alkenyl group having 8 to 18 carbon atoms, and M represents an alkali metal). When spray drying and pulverizing the aqueous slurry containing the main solid content, the solid content concentration of the aqueous slurry is adjusted to 60 to 80% by weight, and the temperature is adjusted to 50 to 120°C. A method for pulverizing the aqueous slurry, which comprises holding and spray-drying the aqueous slurry. 2. The method according to claim 1, wherein the solid content of the higher alkyl sulfate in the aqueous slurry is 90% by weight or more. 3. The method according to claim 1, wherein R in the general formula RSO 4 M is a straight chain or branched alkyl group or alkenyl group having 10 to 16 carbon atoms. 4. The method according to claim 1, wherein M in the general formula RSO 4 M is sodium. 5. The method according to claim 1, wherein the temperature of the aqueous slurry is maintained at 70 to 110°C.
JP1340378A 1978-02-10 1978-02-10 Granulation of higher alkyl sulfate Granted JPS54106428A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1340378A JPS54106428A (en) 1978-02-10 1978-02-10 Granulation of higher alkyl sulfate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1340378A JPS54106428A (en) 1978-02-10 1978-02-10 Granulation of higher alkyl sulfate

Publications (2)

Publication Number Publication Date
JPS54106428A JPS54106428A (en) 1979-08-21
JPS6141350B2 true JPS6141350B2 (en) 1986-09-13

Family

ID=11832152

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1340378A Granted JPS54106428A (en) 1978-02-10 1978-02-10 Granulation of higher alkyl sulfate

Country Status (1)

Country Link
JP (1) JPS54106428A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63249451A (en) * 1987-04-02 1988-10-17 Daikin Ind Ltd Motor for driving fan

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* Cited by examiner, † Cited by third party
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JPS61277661A (en) * 1985-05-31 1986-12-08 Kao Corp Production of higher alcohol sulfuric acid ester salt of high purity
JP4828058B2 (en) * 2001-09-11 2011-11-30 ライオン株式会社 Manufacturing method of detergent
DE602004012809T2 (en) 2003-08-06 2009-04-09 Kao Corp. Process for the preparation of a granular anionic surfactant
JP4319133B2 (en) 2003-12-26 2009-08-26 花王株式会社 Method for producing granular anionic surfactant
JP5020482B2 (en) 2005-01-13 2012-09-05 花王株式会社 Anionic surfactant powder
US8242070B2 (en) 2006-10-16 2012-08-14 Kao Corporation Method for producing anionic surfactant
JP5108403B2 (en) 2007-07-13 2012-12-26 花王株式会社 Method for producing anionic surfactant granules

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63249451A (en) * 1987-04-02 1988-10-17 Daikin Ind Ltd Motor for driving fan

Also Published As

Publication number Publication date
JPS54106428A (en) 1979-08-21

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