JPH0192476A - Production of concentration type softening finish agent - Google Patents

Production of concentration type softening finish agent

Info

Publication number
JPH0192476A
JPH0192476A JP24635787A JP24635787A JPH0192476A JP H0192476 A JPH0192476 A JP H0192476A JP 24635787 A JP24635787 A JP 24635787A JP 24635787 A JP24635787 A JP 24635787A JP H0192476 A JPH0192476 A JP H0192476A
Authority
JP
Japan
Prior art keywords
quaternary ammonium
water
concentrated
softener
alkyl
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
JP24635787A
Other languages
Japanese (ja)
Inventor
Masaaki Yamamura
正明 山村
Junichi Inokoshi
猪腰 淳一
Kazutoshi Ide
一敏 井手
Kiyoshi Sodebayashi
袖林 清
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.)
Kao Corp
Original Assignee
Kao 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 Kao Corp filed Critical Kao Corp
Priority to JP24635787A priority Critical patent/JPH0192476A/en
Publication of JPH0192476A publication Critical patent/JPH0192476A/en
Pending legal-status Critical Current

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Abstract

PURPOSE: To obtain a concentrated softener excellent in storage stability by dispersingly adding a previously mixed and adjusted mixture of a quaternary ammonium salt, isopropanol and water into warm water. CONSTITUTION: This concentrated softener is obtained by dispersingly adding a mixture into warm water (such amount of water as making the softener to be a concentrated type having 15 wt.% quaternary ammonium salt concentration or so in the softener) wherein the mixture is previously prepared and includes 50-70 wt.% asymmetric quaternary ammonium salt represented by the formula (R1 is a 10-14C alkyl; R2 is a 16-24C alkyl; R3 and R4 are each a 1-2C alkyl, hydroxyalkyl, benzyl or the like; X is a halogen or the like), 5-20 wt.% isopropanol and 17-40 wt.% water and the warm water includes an antigelling agent e.g. a polyoxyethylene alkyl ether as the essential component. This concentrated softener has suppressed thickening tendency with age and is excellent in storage stability.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は経時的な増粘の少ない濃縮型柔軟仕上剤の製造
方法に関する。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing a concentrated fabric softener that exhibits little thickening over time.

〔従来の技術〕[Conventional technology]

衣料は、着用及び洗濯を繰り返し行う間に繊維処理剤が
洗い落とされたり、あるいは繊維自体の劣化により硬く
なったりして好ましからざる風合を生ずる。そのため、
近年、多くの家庭において、繊維に柔軟性、帯電防止性
を付与することができる柔軟仕上剤が多用されている。
When clothing is repeatedly worn and washed, the fiber treatment agent may be washed off, or the fibers themselves may become hard due to deterioration, resulting in an undesirable feel. Therefore,
In recent years, fabric softeners that can impart flexibility and antistatic properties to fibers have been widely used in many households.

現在、家庭用柔軟仕上剤として市販されているものは、
その殆どが、−分子中に1〜2個の長鎖アルキル基を有
するカチオン性活性剤、なかんずくジ(硬化牛脂アルキ
ル)ジメチルアンモニウム塩を主成分とするものである
。
Currently, the commercially available household fabric softeners are:
Most of them are based on cationic surfactants having one or two long-chain alkyl groups in the molecule, especially di(hardened tallow alkyl) dimethylammonium salts.

これらの第4級アンモニウム塩を主゛成分とする柔軟基
剤は水に難溶であり、通常3〜5重量%の水分散液又は
乳濁液の形で製造されている。
Soft bases containing these quaternary ammonium salts as main components are poorly soluble in water and are usually produced in the form of 3 to 5% by weight aqueous dispersions or emulsions.

このような柔軟仕上剤は、一般に、第4級アンモニウム
塩液状物を加熱水中に添加分散することにより製造され
ているが、製造時あるいは製造後に増粘する傾向がある
。この問題を解決するために、添加剤の面では水溶性カ
チオン活性剤の配合、あるいは高級アルコールやアルキ
ルフェノールなどのエチレンオキシド付加物、低級アル
コール、エチレングリコール、尿素、水溶性の有機塩、
無機塩などのゲル化防止剤、低温安定性向上剤の配合の
検討がなされてきた。
Such fabric softeners are generally produced by adding and dispersing a liquid quaternary ammonium salt in heated water, but they tend to thicken during or after production. In order to solve this problem, additives such as water-soluble cationic activators, higher alcohols, ethylene oxide adducts such as alkylphenols, lower alcohols, ethylene glycol, urea, water-soluble organic salts, etc.
Studies have been conducted on the addition of anti-gelling agents such as inorganic salts and low-temperature stability improvers.

一方、製造方法の面では、第4級アンモニウム塩液状物
を水中で噴霧分散する方法(特開昭55−8837号公
報)、第4級アンモニウム塩液状物を攪拌槽又はライン
ミキサーの攪拌羽根に近い位置に添加又は供給する方法
(特開昭50−105997、特開昭57−5797、
特開昭57−102226号各公報)1水が流通する配
管内に備えたスリット弁の直前に第4級アンモニウム塩
液状物を供給する方法(特開昭59−160524号公
報)、超音波を照射する方法(特開昭62−11539
号公報)など種々の工夫がなされてきた。
On the other hand, in terms of manufacturing methods, there is a method in which a liquid quaternary ammonium salt is sprayed and dispersed in water (Japanese Unexamined Patent Application Publication No. 1988-8837), a liquid quaternary ammonium salt is dispersed in a stirring tank or a stirring blade of a line mixer, etc. Method of adding or supplying to a nearby position (JP-A-50-105997, JP-A-57-5797,
1. A method of supplying a quaternary ammonium salt liquid immediately before a slit valve provided in a pipe through which water flows (Japanese Unexamined Patent Publication No. 59-160524), Method of irradiation (Japanese Patent Application Laid-Open No. 62-11539
Various efforts have been made, such as the following:

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

近年、柔軟仕上剤を使用する対象衣料の増加に伴い、流
通コストや包装コストの減少、家庭や販売店等での在庫
スペースの縮小を目的に、高濃度の水分散液tある濃縮
型の衣料用柔軟仕上剤が強く要望されている。
In recent years, with the increase in the number of garments that use fabric softeners, concentrated clothing containing highly concentrated aqueous dispersions has been developed with the aim of reducing distribution costs, packaging costs, and inventory space at homes and retail stores. There is a strong demand for fabric softeners.

しかしながら、濃度が5重量%以上になると、上記の水
分散液は著しく増粘し、ハンドリング上、種々のトラブ
ルを生ずる。
However, when the concentration exceeds 5% by weight, the aqueous dispersion described above significantly thickens, causing various troubles in handling.

第4級アンモニウム塩の濃度が30重量%以下であれば
、ゲル化防止剤、低温安定性向上剤の選択、あるいは前
記種々の製造方法により、製造時および初期の増粘を抑
制できる。しかしながら、濃縮型柔軟仕上剤は経時的な
増粘傾向が著しく、家庭での常温での取り扱いという実
用化に際して大きな問題となっていた。
When the concentration of the quaternary ammonium salt is 30% by weight or less, thickening during production and in the initial stage can be suppressed by selecting an antigelation agent, a low-temperature stability improver, or by using the various production methods described above. However, concentrated fabric softeners tend to increase in viscosity over time, which poses a major problem when they are put to practical use in the home at room temperature.

〔問題点を解決するための手段〕[Means for solving problems]

かかる実情において、本発明者らは上記の問題点を解決
せんと製造法について鋭意研究を行った結果、温水中に
添加する第4級アンモニウム化合物の液状物を特定組成
の予備混合物として用いれば、経時的な増粘を著しく抑
制出来るという知見を得、本発明を完成した。
Under these circumstances, the inventors of the present invention have conducted extensive research on manufacturing methods to solve the above problems, and have found that if a liquid quaternary ammonium compound added to hot water is used as a premix of a specific composition, The present invention was completed based on the knowledge that thickening over time can be significantly suppressed.

即ち、本発明は、ゲル化防止剤を含有する濃縮型柔軟仕
上剤の製造法において、第4級アンモニウム化合物50
〜70重量%、イソプロパノール5〜20重量%、水1
7〜40重量%を含有する予備混合物を予め調整し、こ
の予備混合物を温水中に添加、分散することを特徴とす
る濃縮型柔軟仕上剤の製造方法を提供する。
That is, the present invention provides a method for producing a concentrated fabric softener containing an antigelation agent, in which a quaternary ammonium compound 50
~70% by weight, 5-20% by weight of isopropanol, 1% by weight of water
Provided is a method for producing a concentrated fabric softener, characterized in that a premix containing 7 to 40% by weight is prepared in advance, and the premix is added and dispersed in hot water.

従来の方法では、温水に添加する第4級アンモニウム化
合物の液状物は、第4級アンモニウム化合物そのものを
溶融し液状とするか、又は低級アルコール、エチレング
リコール、あるいは加温上液状となる非イオン活性剤、
高級アルコールなどと加温上混合し液状予備混合物とし
て用いられていた。そして予備混合物中の水含量は普通
非常に少なく、多くても約10〜約15重量%以下で用
いられていた。本願発明は予備混合物中の水含量を高く
することにより、得られる濃縮型柔軟仕上剤の経時的増
粘傾向が著しく抑えられるという驚くべき現象を見い出
し、完成されたものである。
In the conventional method, the liquid form of the quaternary ammonium compound added to hot water is either melted into a liquid state by melting the quaternary ammonium compound itself, or mixed with lower alcohol, ethylene glycol, or a nonionic active material that becomes liquid upon heating. agent,
It was used as a liquid premix by heating and mixing with higher alcohols. The water content in the premix is usually very low, at most about 10 to about 15% by weight or less. The present invention was completed based on the discovery of the surprising phenomenon that by increasing the water content in the premix, the tendency of the resulting concentrated fabric softener to thicken over time is significantly suppressed.

上記の現象についてその理由は明らかでないが、第4級
アンモニウム化合物の水和物をまず生成させ、この安定
な水和物構造を、後工程での剪断力により、切断し、微
粒子化させる事により、第4級アンモニウム化合物の水
和物を安定した状態で存在させ得る為と考えられる。
The reason for the above phenomenon is not clear, but it is possible to first generate a hydrate of a quaternary ammonium compound, and then cut this stable hydrate structure by shearing force in a subsequent process and make it into fine particles. This is thought to be because the hydrate of the quaternary ammonium compound can exist in a stable state.

本願発明の製造方法に使用される第4級アンモニウム化
合物は特に限定されない。柔軟効果を有するものであれ
ばいづれも適用できる。ジ硬化牛脂アルキルジメチルア
ンモニウム塩に代表される第4級アンモニウム塩、1−
メチル−2−タロ〜3−タローアミドエチルイミダゾリ
ニウム塩に代表されるイミダゾリニウム塩、ジーステア
ロイルーオキシエチルジメチルアンモニウム塩、ミリス
トイルオキシメチルステ了りルジメチルアンモニカム塩
に代表されるエステル型第4級アンモニウム塩などが挙
げられる。
The quaternary ammonium compound used in the production method of the present invention is not particularly limited. Any material having a softening effect can be applied. Quaternary ammonium salts represented by di-hardened beef tallow alkyl dimethyl ammonium salts, 1-
Imidazolinium salts represented by methyl-2-talo-3-tallowamidoethyl imidazolinium salts, ester types represented by di-stearoyloxyethyl dimethylammonium salts, myristoyloxymethylsteryl dimethyl ammonium salts Examples include quaternary ammonium salts.

本発明の製造方法は、前述したような汎用される第4級
化合物に対して効果を有することはもちろんであるが、
下記一般式で示される非対称型第4級アンモニウム塩に
対して特に優れた効果を発揮する。
The production method of the present invention is not only effective for the commonly used quaternary compounds as described above, but also
It exhibits particularly excellent effects on asymmetric quaternary ammonium salts represented by the following general formula.

〔式中、R1はCIO〜14のアルキル基、R,はC0
〜24のアルキル基、R,、R,はそれぞれC1〜3の
アルキル基もしくはヒドロキシアルキル基、ベンジル基
もしくは+CzHnO+−H(但し、nは1〜3)、X
はハロゲン又はCl−3のアルキル硫酸塩を示す〕本発
明における予備混合物は、前記第4級アンモニウム化合
物50〜70重量%、水17〜40重量%及びイソプロ
パノール5〜20重量%を20〜70℃で均質になるま
で攪拌することにより得られる。
[In the formula, R1 is a CIO to 14 alkyl group, R, is C0
-24 alkyl groups, R,, R, are each C1-3 alkyl group or hydroxyalkyl group, benzyl group or +CzHnO+-H (however, n is 1-3), X
represents a halogen or an alkyl sulfate of Cl-3] The premix in the present invention includes 50 to 70% by weight of the quaternary ammonium compound, 17 to 40% by weight of water, and 5 to 20% by weight of isopropanol at 20 to 70°C. It is obtained by stirring until homogeneous.

本発明の製造方法においては、前記組成の予備混合物を
、好ましくは20〜60℃の温水中に添加分散し、第4
級アンモニウム塩漬度を7〜30%、好ましくは10〜
20%に調整することにより濃縮型柔軟仕上剤を得る。
In the production method of the present invention, a premix having the above composition is preferably added and dispersed in hot water of 20 to 60°C, and a fourth
grade ammonium salting degree of 7 to 30%, preferably 10 to 30%
By adjusting the concentration to 20%, a concentrated fabric softener is obtained.

分散手段は羽根攪拌、ラインミキサー、高圧噴射などが
あるが特に、限定されるものではなく、効率良く均一に
攪拌できるものであればよい。羽根攪拌の場合、予備混
合物を攪拌羽根の近傍に注入するのが最も攪拌効率がよ
い。
Dispersion means include blade agitation, line mixer, high-pressure injection, etc., but are not particularly limited, and any means that can efficiently and uniformly agitate may be used. In the case of blade stirring, the best stirring efficiency is achieved by injecting the premix near the stirring blades.

濃縮型柔軟仕上剤にゲル化防止剤の添加は必須であり、
通常0.1〜5重景%配合される。ゲル化防止剤として
は、ポリオキシエチレンアルキルエーテル、ポリオキシ
エチレンアルキルフェニルエーテルなどの非イオン活性
剤、ポリエチレングリコール、ポリエチレンイミンなど
の高分子分散剤、塩化ナトリウム、塩化カルシウム、塩
化アンモニウムなどの水溶性無機塩が挙げられる。水溶
性無機塩と他のゲル化防止剤併用が望ましい。これらの
ゲル化防止剤は、予備混合物又は温水中に予め添加して
おいてもよい。
It is essential to add an anti-gelling agent to concentrated fabric softeners.
Usually 0.1 to 5% is added. Anti-gelling agents include nonionic surfactants such as polyoxyethylene alkyl ether and polyoxyethylene alkyl phenyl ether, polymeric dispersants such as polyethylene glycol and polyethylene imine, and water-soluble agents such as sodium chloride, calcium chloride, and ammonium chloride. Examples include inorganic salts. It is desirable to use a water-soluble inorganic salt in combination with another anti-gelling agent. These anti-gelling agents may be added in advance to the premix or hot water.

あるいは温水中に予備混合物を添加分散したのち添加し
てもよく、この場合添加位置は予備混合物と同様に攪拌
羽根の近傍に注入するのがよい。
Alternatively, the premix may be added after being added and dispersed in warm water, and in this case, the addition position is preferably injected near the stirring blade, similar to the premix.

本発明の製造方法により得られる濃縮型柔軟仕上剤には
、通常の柔軟仕上剤に使用されている例えば、エタノー
ル、エチレングリコール、プロピレングリコールなどの
低温安定化剤、香料、色素、シリコーン化合物、抗菌剤
などを配合でき、その添加順序もゲル化防止剤と同様い
づれの時点でもよ(特に制限されない。
The concentrated fabric softener obtained by the production method of the present invention contains, for example, low-temperature stabilizers such as ethanol, ethylene glycol, and propylene glycol, fragrances, pigments, silicone compounds, and antibacterial agents that are used in ordinary fabric softeners. Agents, etc. can be added, and the order of adding them can be at any point, just like the anti-gelling agent (there is no particular restriction).

かくして、濃縮型柔軟仕上剤が得られるが、予備混合物
の組成が本発明の範囲外の場合には、初粘度が高くなっ
たり、経時的増粘が充分に抑制されない。
In this way, a concentrated type fabric softener is obtained, but if the composition of the premix is outside the range of the present invention, the initial viscosity may become high or the thickening over time may not be sufficiently suppressed.

〔実施例〕〔Example〕

以下に実施例により、本発明を具体的に説明するが本発
明はこれらに限定されるものではない。
The present invention will be specifically explained below with reference to Examples, but the present invention is not limited thereto.

実施例1 第1表に示す組成の第4級アンモニウム塩、水およびイ
ソプロパノールを50〜70℃で均一に攪拌して予備混
合物を得た。上記の予備混合物を水に分散して得られる
柔軟仕上剤中の第4級アンモニウム塩漬度を15%にす
るに必要な量の水に、水溶性無機塩(柔軟仕上剤中で第
1表に示す濃度とするのに必要なi>を溶解し、50℃
に加温し、700rpm″′i?攪拌した。この温水中
に、予備混合物を攪拌羽根から2cmの位置に供給し、
均一に分散されるまで攪拌を続け、濃縮型柔軟仕上剤を
得た。
Example 1 A quaternary ammonium salt having the composition shown in Table 1, water and isopropanol were uniformly stirred at 50 to 70°C to obtain a premix. A water-soluble inorganic salt (Table 1 in the fabric softener) is added to the amount of water necessary to make the degree of quaternary ammonium salting in the fabric softener 15% by dispersing the above premix in water. Dissolve i> necessary to obtain the concentration shown in and heat at 50°C.
The premix was heated to 700 rpm and stirred at 700 rpm.The premix was supplied into the warm water at a position 2 cm from the stirring blade.
Stirring was continued until uniformly dispersed to obtain a concentrated fabric softener.

得られた濃縮型柔軟仕上剤の初期粘度、および−10℃
、室温、50℃に20日間保存した時の粘度を測定した
。結果を表−1に示す。
Initial viscosity of the obtained concentrated softener and -10°C
The viscosity was measured after storage at room temperature and 50°C for 20 days. The results are shown in Table-1.

実施例2 ヤシアルキル硬化牛脂アルキルジメチルアンモニウムク
ロライド15g1テトラエチレンペンタミンのポリオキ
シプロピレンポリオキシエチレン付加物(PO/ EO
モル比10/90、MW15000) 1gを水5g1
イソプロパノール3gと50℃で混合し、予備混合物を
得た。この予備混合物を水74g中に40℃にて添加、
攪拌したのち、10%CaC1g水溶液2gを添加して
、第4級アンモニウム塩15%の濃縮型柔軟仕上剤を得
た。
Example 2 Coconut alkyl cured beef tallow alkyl dimethyl ammonium chloride 15 g 1 tetraethylene pentamine polyoxypropylene polyoxyethylene adduct (PO/EO
Molar ratio 10/90, MW 15000) 1g to 5g 1 water
A premix was obtained by mixing with 3 g of isopropanol at 50°C. This premix was added to 74 g of water at 40°C,
After stirring, 2 g of an aqueous solution of 1 g of 10% CaC was added to obtain a concentrated fabric softener containing 15% of quaternary ammonium salt.

初期粘度180cps、−10℃、室温、50℃で20
日間保存後の粘度はそれぞれ190.184.210c
psであった。
Initial viscosity 180cps, -10℃, room temperature, 20℃ at 50℃
The viscosity after storage for days is 190.184.210c, respectively.
It was ps.

Claims (1)

【特許請求の範囲】 1、ゲル化防止剤を含有する濃縮型柔軟仕上剤の製造方
法において、第4級アンモニウム化合物50〜70重量
%、イソプロパノール5〜20重量%、および水17〜
40重量%を含有する予備混合物を予め調整し、該予備
混合物を温水中に添加分散することを特徴とする濃縮型
柔軟仕上剤の製造方法。 2、第4級アンモニウム化合物が下記一般式(1)で表
される非対称第4級アンモニウム塩である特許請求の範
囲第1項記載の濃縮型柔軟仕上剤の製造方法。 ▲数式、化学式、表等があります▼(1) 〔式中、R_1はC_1_0_〜_1_4のアルキル基
、R_2はC_1_6_〜_2_4のアルキル基、R_
3、R_4はそれぞれC_1_〜_3のアルキル基、ヒ
ドロキシアルキル基、ベンジル基もしくは■C_2H_
4O■_nH但し、nは1〜3)、Xはハロゲン又はC
_1_〜_3のアルキル硫酸塩を示す〕
[Scope of Claims] 1. A method for producing a concentrated fabric softener containing an antigelation agent, comprising: 50 to 70% by weight of a quaternary ammonium compound, 5 to 20% by weight of isopropanol, and 17 to 10% by weight of water.
A method for producing a concentrated fabric softener, comprising preparing a premix containing 40% by weight in advance, and adding and dispersing the premix in hot water. 2. The method for producing a concentrated fabric softener according to claim 1, wherein the quaternary ammonium compound is an asymmetric quaternary ammonium salt represented by the following general formula (1). ▲There are mathematical formulas, chemical formulas, tables, etc.▼(1) [In the formula, R_1 is an alkyl group of C_1_0_ to _1_4, R_2 is an alkyl group of C_1_6_ to _2_4, R_
3, R_4 is an alkyl group of C_1_ to_3, a hydroxyalkyl group, a benzyl group or ■C_2H_
4O ■_nH, where n is 1 to 3), X is halogen or C
Indicates the alkyl sulfate of _1_ to _3]
JP24635787A 1987-09-30 1987-09-30 Production of concentration type softening finish agent Pending JPH0192476A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP24635787A JPH0192476A (en) 1987-09-30 1987-09-30 Production of concentration type softening finish agent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP24635787A JPH0192476A (en) 1987-09-30 1987-09-30 Production of concentration type softening finish agent

Publications (1)

Publication Number Publication Date
JPH0192476A true JPH0192476A (en) 1989-04-11

Family

ID=17147353

Family Applications (1)

Application Number Title Priority Date Filing Date
JP24635787A Pending JPH0192476A (en) 1987-09-30 1987-09-30 Production of concentration type softening finish agent

Country Status (1)

Country Link
JP (1) JPH0192476A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0435451U (en) * 1990-07-18 1992-03-25

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0435451U (en) * 1990-07-18 1992-03-25

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