JP2000328454A - Transparent liquid softening agent - Google Patents

Transparent liquid softening agent

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Publication number
JP2000328454A
JP2000328454A JP11130112A JP13011299A JP2000328454A JP 2000328454 A JP2000328454 A JP 2000328454A JP 11130112 A JP11130112 A JP 11130112A JP 13011299 A JP13011299 A JP 13011299A JP 2000328454 A JP2000328454 A JP 2000328454A
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JP
Japan
Prior art keywords
component
carbon atoms
weight
alkyl
molecule
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
JP11130112A
Other languages
Japanese (ja)
Other versions
JP3859901B2 (en
Inventor
Kazutaka Shirato
和隆 白土
Kenji Takigami
賢二 瀧上
Hideji Tagata
秀次 田方
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
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Filing date
Publication date
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Priority to JP13011299A priority Critical patent/JP3859901B2/en
Publication of JP2000328454A publication Critical patent/JP2000328454A/en
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Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To obtain a transparent liquid softening agent without formulating a specific additive therewith. SOLUTION: This transparent liquid softening agent at pH 1.5-6.0 comprises the following components (a) to (c): (a) 5-25 wt.% of an acid salt of a quaternary ammonium compound or a tertiary amine compound having one or more ester groups and two or more 11-20C alkyl groups or 11-20C alkenyl groups in one molecule, (b) 0.1-15 wt.% of one or more kinds selected from the following compounds (b-1) and (b-2): (b-1) an acid salt of a quaternary ammonium compound or a tertiary amine compound having one 11-20C alkyl group or 11-20C alkenyl group in the molecule and (b-2) an amphoteric surfactant having one 6-20C alkyl or 6-20C alkenyl group in the molecule and (c) 0.05-2.0 wt.% of an 8-20C fatty acid or its salt.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は外観上透明な液体柔
軟剤に関する。
The present invention relates to a liquid softener which is transparent in appearance.

【0002】[0002]

【従来の技術及び発明が解決しようとする課題】従来の
液体柔軟剤は、柔軟基剤が水に難溶であるために水中で
0.1〜10μmの粒子径を有する粒子として分散し、
外観上濁ったものになる。柔軟剤の透明化については、
特開平3−27180号公報には、4級アンモニウム化
合物に特定の有機酸を配合することで透明化させる技術
が記載されており、また特開平2−300382号公報
には、特定の非イオン性高分子化合物を配合する技術が
開示されている。しかしながら、これらの柔軟剤は透明
化のために、柔軟基剤以外の化合物を配合するため、配
合組成の自由度を制限するものであった。本発明の目的
は、配合組成の自由度の高い透明柔軟剤を提供すること
にある。
2. Description of the Related Art A conventional liquid softener is dispersed in water as particles having a particle size of 0.1 to 10 μm because a soft base is hardly soluble in water.
It becomes cloudy in appearance. Regarding the transparency of the softener,
JP-A-3-27180 describes a technique for blending a quaternary ammonium compound with a specific organic acid to make it transparent, and JP-A-2-300382 discloses a specific non-ionic compound. A technique for blending a polymer compound is disclosed. However, these softeners contain a compound other than the softening base for transparency, and thus limit the flexibility of the composition. An object of the present invention is to provide a transparent softener having a high degree of freedom in the composition.

【0003】[0003]

【課題を解決するための手段】本発明は、下記(a)〜
(c)成分を含有し、pHが1.5〜6.0である透明
液体柔軟剤を提供するものである。 (a)分子中に1つ以上のエステル基及び2つ以上の炭
素数11〜20のアルキル基又はアルケニル基を有す
る、4級アンモニウム化合物又は3級アミン化合物の酸
塩 5〜25重量% (b)下記化合物(b−1)及び(b−2)から選ばれ
る1種以上 0.1〜15重量% (b−1)分子内に1つの炭素数11〜20のアルキル
基又はアルケニル基を有する、4級アンモニウム化合物
又は3級アミン化合物の酸塩 (b−2)分子内に1つの炭素数6〜20のアルキル基
又はアルケニル基を有する両性界面活性剤 (c)炭素数8〜20の脂肪酸又はその塩 0.05〜
2.0重量% 本発明の透明柔軟剤において、透明とは、光路長10m
mの石英セルを使用し、対照側セルにイオン交換水を用
いた時の660nmの波長の光透過率が30%以上のも
のを意味する。
The present invention provides the following (a) to (d):
It is intended to provide a transparent liquid softener containing component (c) and having a pH of 1.5 to 6.0. (A) an acid salt of a quaternary ammonium compound or a tertiary amine compound having one or more ester groups and two or more alkyl groups or alkenyl groups having 11 to 20 carbon atoms in the molecule 5 to 25% by weight (b ) One or more selected from the following compounds (b-1) and (b-2) 0.1 to 15% by weight (b-1) having one alkyl group or alkenyl group having 11 to 20 carbon atoms in the molecule Acid salts of quaternary ammonium compounds or tertiary amine compounds (b-2) amphoteric surfactant having one alkyl or alkenyl group having 6 to 20 carbon atoms in the molecule (c) fatty acid having 8 to 20 carbon atoms Or a salt thereof 0.05 to
2.0% by weight In the transparent softener of the present invention, “transparent” means that the optical path length is 10 m.
m means a cell having a light transmittance of 30% or more at a wavelength of 660 nm when ion-exchanged water is used for a control cell and a quartz cell of m.

【0004】[0004]

【発明の実施の形態】本発明で使用する(a)成分は、
分子中に1つ以上のエステル基及び2つ以上の炭素数1
1〜20のアルキル基もしくはアルケニル基を有する、
4級アンモニウム化合物もしくは3級アミン化合物の無
機又は有機酸塩である。より好ましくは、炭素数が11
〜20のアルキル基またはアルケニル基を2つ有するも
のであり、このような化合物としては一般式(I)及び
一般式(II)で示される化合物を挙げることができる。
BEST MODE FOR CARRYING OUT THE INVENTION The component (a) used in the present invention comprises:
At least one ester group and at least two carbon atoms in the molecule
Having 1 to 20 alkyl groups or alkenyl groups,
It is an inorganic or organic acid salt of a quaternary ammonium compound or a tertiary amine compound. More preferably, the carbon number is 11
These compounds have two to 20 alkyl groups or alkenyl groups, and examples of such compounds include compounds represented by general formulas (I) and (II).

【0005】[0005]

【化1】 Embedded image

【0006】[式中、R1 、R4 は炭素数11〜20の
アルキル基又はアルケニル基を示し、X、Yは、−CO
O−、−CONR7 −、−OCO−、−NR7 CO−を
示し、X、Yのうち少なくとも1つは−COO−であ
る。ここでR7 は水素原子、炭素数1〜3のアルキル基
又はヒドロキシアルキレン基を示す。また、R2 、R5
は炭素数1〜5のアルキレン基であり、R3 、R6 は炭
素数1〜3のアルキル基又はヒドロキシアルキレン基を
示すか、或いはR1 −X−R2 −であってもよい。ま
た、Zは1価又は2価のアニオンであり、好ましくはC
- 、SO4 2- 、HSO4 - 、R'OSO3 - (R'は炭素
数1〜3のアルキル基)、R''COO- (R''は炭素数
8〜18の直鎖のアルキル基)である。尚、柔軟剤中で
他成分とイオン交換されている場合はこの限りでな
い。] より具体的には以下の化合物(1)〜(4)を挙げるこ
とができる。
Wherein R 1 and R 4 each represent an alkyl or alkenyl group having 11 to 20 carbon atoms, and X and Y represent —CO
O -, - CONR 7 -, - OCO -, - indicates NR 7 CO-, X, at least one of Y is -COO-. Here, R 7 represents a hydrogen atom, an alkyl group having 1 to 3 carbon atoms or a hydroxyalkylene group. Also, R 2 , R 5
Is an alkylene group having 1 to 5 carbon atoms, and R 3 and R 6 each represent an alkyl group or a hydroxyalkylene group having 1 to 3 carbon atoms, or may be R 1 —X—R 2 —. Z is a monovalent or divalent anion, preferably C
l , SO 4 2− , HSO 4 , R OSO 3 (R is an alkyl group having 1 to 3 carbon atoms), R COO (R is a straight chain having 8 to 18 carbon atoms) Alkyl group). Note that this does not apply when the softening agent is ion-exchanged with another component. More specifically, the following compounds (1) to (4) can be mentioned.

【0007】[0007]

【化2】 Embedded image

【0008】[前記化合物(1)〜(4)中、R8 は炭
素数11〜17のアルキル基又はアルケニル基であり、
さらには炭素数15〜17のアルキル基がより好まし
い。Z'はCl- 、SO4 2- 、HSO4 - 、R'OSO3 -
(R'は炭素数1〜3のアルキル基)、R''COO
- (R''は炭素数8〜18の直鎖のアルキル基)であ
る。] また、一般式(I)及び一般式(II)で示される化合物
以外にも下記化合物(5)を用いてもよい。
[In the compounds (1) to (4), R 8 is an alkyl or alkenyl group having 11 to 17 carbon atoms;
Further, an alkyl group having 15 to 17 carbon atoms is more preferable. Z is Cl , SO 4 2− , HSO 4 , R OSO 3
(R is an alkyl group having 1 to 3 carbon atoms), R COO
- (R is a linear alkyl group having 8 to 18 carbon atoms). Further, the following compound (5) may be used in addition to the compounds represented by the general formulas (I) and (II).

【0009】[0009]

【化3】 Embedded image

【0010】[前記化合物(5)中、R8 及びZ'は前
記記載の通りである。] 本発明では特にエステル基とアミド基を有する化合物
(1)、(3)あるいはこれらの混合物が特に柔軟性能
と透明化の点から好ましい。(a)成分は、柔軟効果の
点から、好ましくは5〜20重量%配合される。
[In the compound (5), R 8 and Z are as described above. In the present invention, compounds (1) and (3) each having an ester group and an amide group or a mixture thereof are particularly preferable from the viewpoints of flexibility and transparency. The component (a) is preferably blended in an amount of 5 to 20% by weight from the viewpoint of a softening effect.

【0011】本発明の(b−1)成分としては、下記一
般式(III)〜(VI)で示される化合物を挙げることがで
きる。
As the component (b-1) of the present invention, there can be mentioned compounds represented by the following general formulas (III) to (VI).

【0012】[0012]

【化4】 Embedded image

【0013】[式中、R9 炭素数11〜20のアルキル
基又はアルケニル基を示し、X' は、−COO−、−C
ONR14−、−OCO−、−NR14CO−であり、ここ
でR14は水素原子、炭素数1〜3のアルキル基又はヒド
ロキシアルキレン基を示す。また、R10は炭素数1〜5
のアルキレン基であり、R11、R12、R13は炭素数1〜
3のアルキル基又はヒドロキシアルキレン基を示す。Z
は前記記載の通りである。] より具体的には以下の化合物(6)〜(11)を挙げる
ことができる。
Wherein R 9 represents an alkyl group or an alkenyl group having 11 to 20 carbon atoms, and X represents —COO—, —C
ONR 14 —, —OCO—, and —NR 14 CO—, wherein R 14 represents a hydrogen atom, an alkyl group having 1 to 3 carbon atoms, or a hydroxyalkylene group. R 10 has 1 to 5 carbon atoms.
Wherein R 11 , R 12 and R 13 have 1 to 1 carbon atoms
3 represents an alkyl group or a hydroxyalkylene group. Z
Is as described above. More specifically, the following compounds (6) to (11) can be mentioned.

【0014】[0014]

【化5】 Embedded image

【0015】[前記化合物(6)〜(11)中、R15
炭素数12〜18のアルキル基又はアルケニル基であ
り、さらには炭素数16〜18のアルキル基が好まし
い。R16は炭素数11〜17のアルキル基又はアルケニ
ル基であり、さらには炭素数15〜17のアルキル基が
好ましい。Z'は前記記載の通りである。] また、本発明の(b−2)成分としては、下記一般式
(VII)及び一般式(VIII) で示される化合物を挙げるこ
とができる。
[In the compounds (6) to (11), R 15 is an alkyl or alkenyl group having 12 to 18 carbon atoms, and more preferably an alkyl group having 16 to 18 carbon atoms. R 16 is an alkyl group or alkenyl group having 11 to 17 carbon atoms, and more preferably an alkyl group having 15 to 17 carbon atoms. Z is as described above. Further, examples of the component (b-2) of the present invention include compounds represented by the following general formulas (VII) and (VIII).

【0016】[0016]

【化6】 Embedded image

【0017】[式中、R17は炭素数6〜20のアルキル
基又はアルケニル基、R10、R11、R12、X' は前記記
載の通りであり、WはCOO−、SO3−、OSO3−で
ある。] より具体的には以下の化合物(12)〜(16)を挙げ
ることができる。
Wherein R 17 is an alkyl or alkenyl group having 6 to 20 carbon atoms, R 10 , R 11 , R 12 and X are as described above, and W is COO—, SO 3 —, OSO 3 —. More specifically, the following compounds (12) to (16) can be exemplified.

【0018】[0018]

【化7】 Embedded image

【0019】[前記化合物(12)〜(16)中、R18
は炭素数7〜16のアルキル基又はアルケニル基であ
る。] 本発明の(c)成分は炭素数8〜20の脂肪酸又はその
塩類であり、具体的にはカプリル酸、カプリン酸、ラウ
リン酸、ミリスチン酸、パルミチン酸、ステアリン酸、
オレイン酸、あるいはこれらの混合物であり、ラウリン
酸、ステアリン酸、オレイン酸から選ばれる1種以上が
特に好ましい。また、ヤシ油、パーム油、パーム核油、
牛脂から誘導されるアルキル組成を有する脂肪酸も好ま
しい。本発明において、(b)成分は、好ましくは0.
5〜10重量%含有されるが、(b−1)成分だけを用
いる場合、透明化及び安定性の点から、(b−1)成分
は(a)成分に対して好ましくは(b−1)成分/
(a)成分=20/80〜60/40(重量比)であ
り、好ましくは40/60〜60/40である。また、
(b−2)成分だけを配合する場合、(b−2)成分の
含有量は、透明性及び安定性の点から、柔軟剤中に好ま
しくは0.5〜3重量%である。また、(b−1)成分
及び(b−2)成分を併用する場合は、(b−1)成分
は透明性、安定性の点から、好ましくは(b−1)成分
/(a)成分=0.3/99.7〜60/40(重量
比)、より好ましくは、0.5/99.5〜60/40
であり、且つ(b−2)成分は柔軟剤中に好ましくは
0.5〜5重量%、より好ましくは0.5〜3重量%配
合される。
[In the above compounds (12) to (16), R 18
Is an alkyl group or an alkenyl group having 7 to 16 carbon atoms. The component (c) of the present invention is a fatty acid having 8 to 20 carbon atoms or a salt thereof, and specifically, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid,
Oleic acid or a mixture thereof, and one or more selected from lauric acid, stearic acid, and oleic acid are particularly preferable. In addition, palm oil, palm oil, palm kernel oil,
Also preferred are fatty acids having an alkyl composition derived from tallow. In the present invention, the component (b) is preferably contained in an amount of 0.1 to 0.1.
Although it is contained in an amount of 5 to 10% by weight, when only the component (b-1) is used, the component (b-1) is preferably (b-1) with respect to the component (a) in terms of transparency and stability. )component/
Component (a) = 20/80 to 60/40 (weight ratio), preferably 40/60 to 60/40. Also,
When only the component (b-2) is blended, the content of the component (b-2) is preferably 0.5 to 3% by weight in the softener in terms of transparency and stability. When the components (b-1) and (b-2) are used in combination, the component (b-1) is preferably component (b-1) / component (a) from the viewpoint of transparency and stability. = 0.3 / 99.7 to 60/40 (weight ratio), more preferably 0.5 / 99.5 to 60/40.
And the component (b-2) is preferably incorporated in the softener in an amount of 0.5 to 5% by weight, more preferably 0.5 to 3% by weight.

【0020】(c)成分は安定性の点から、柔軟剤中に
好ましくは0.05〜1.5重量%配合される。特に
(b−1)成分だけを配合する場合、(c)成分は好ま
しくは[(a)成分+(b−1)成分]/(c)成分=
85/15〜99.9/0.1、より好ましくは90/
10〜99.5/0.5、最も好ましくは90/10〜
99/1の割合で配合される。また、(b−2)成分だ
けを配合する場合、(c)成分は好ましくは(a)成分
/(c)成分=90/10〜99.9/0.1、より好
ましくは93/7〜99.5/0.5、最も好ましくは
95/5〜99.5/0.5の割合で配合される。ま
た、(b−1)成分、(b−2)成分を併用する場合
は、(c)成分は好ましくは[(a)成分+(b−1)
成分]/(c)成分=85/15〜99.9/0.1、
より好ましくは90/10〜99.5/0.5、最も好
ましくは90/10〜99/1の割合で配合される。
The component (c) is preferably incorporated in the softener in an amount of 0.05 to 1.5% by weight from the viewpoint of stability. In particular, when only the component (b-1) is blended, the component (c) is preferably [component (a) + component (b-1)] / component (c) =
85/15 to 99.9 / 0.1, more preferably 90 /
10-99.5 / 0.5, most preferably 90/10
It is blended at a ratio of 99/1. When only the component (b-2) is blended, the component (c) is preferably component (a) / component (c) = 90/10 to 99.9 / 0.1, more preferably 93/7 to 0.1. 99.5 / 0.5, most preferably 95/5 to 99.5 / 0.5. When the components (b-1) and (b-2) are used together, the component (c) is preferably [component (a) + (b-1)].
Component] / (c) component = 85/15 to 99.9 / 0.1,
More preferably, it is blended at a ratio of 90/10 to 99.5 / 0.5, most preferably at a ratio of 90/10 to 99/1.

【0021】本発明の透明柔軟剤には、更に(d)成分
として炭素数8〜18のアルコール又はアミンのアルキ
レンオキシド付加物(アルキレンオキシド付加モル数は
8〜60、好ましくは15〜40)を0.3〜10重量
%、好ましくは0.5〜7重量%含有することが透明化
及び安定性の点で好ましい。
The transparent softener of the present invention further comprises, as a component (d), an alkylene oxide adduct of an alcohol or amine having 8 to 18 carbon atoms (the number of moles of alkylene oxide added is 8 to 60, preferably 15 to 40). The content of 0.3 to 10% by weight, preferably 0.5 to 7% by weight is preferable in terms of transparency and stability.

【0022】(d)成分としては以下の化合物(17)
〜(20)を挙げることができる。 R20−O−(C24O)p−H (17) [式中、R20は炭素数8〜18のアルキル基であり、p
は8〜60、好ましくは20〜40の数である。] R20−O−(C24O)q(C36O)r−H (18) [式中、R20は炭素数8〜18のアルキル基であり、q
及びrはそれぞれ独立に2〜40、好ましくは5〜40
の数であり、エチレンオキシドとプロピレンオキシドは
ランダムあるいはブロック付加体であってもよい。]
As the component (d), the following compound (17)
To (20). R 20 -O- (C 2 H 4 O) p -H (17) [ wherein, R 20 is an alkyl group having 8 to 18 carbon atoms, p
Is a number from 8 to 60, preferably from 20 to 40. ] R 20 -O- (C 2 H 4 O) q (C 3 H 6 O) r -H (18) [ wherein, R 20 is an alkyl group having 8 to 18 carbon atoms, q
And r are each independently 2 to 40, preferably 5 to 40
And ethylene oxide and propylene oxide may be random or block adducts. ]

【0023】[0023]

【化8】 Embedded image

【0024】[式中、R20は炭素数8〜18のアルキル
基であり、s及びtの合計は5〜60、好ましくは5〜
40の数である。] 本発明の透明液体柔軟剤には、透明化の妨げにならない
程度に通常配合される香料、抗菌剤あるいは色素等の成
分を配合しても差し支えない。しかしながら、通常、粘
度改変剤、抗ゲル化剤として柔軟剤に配合される塩化カ
ルシウムは透明化の妨げとなるため、500ppm以下
にとどめるべきであり、好ましくは実質上添加しないこ
とが望ましい。但し、脂肪酸塩類などの界面活性剤には
ナトリウム塩やカリウム塩が含まれているが、このよう
な界面活性剤の使用によって組成物に混入する無機塩は
上記制限を受けるものではない。また、柔軟性向上剤及
び安定性の点から配合されることが多い、(d)成分以
外の炭素数8〜20のアルキル基またはアルケニル基を
1つ以上有する非イオン性化合物、特にトリグリセライ
ド、ジグリセライド、モノグリセライド、ペンタエリス
リトールのモノ、ジ、トリエステル、ソルビタンエステ
ルなどの多価アルコールの脂肪酸エステルの配合量は1
重量%以下にすることが良く、実質上配合しないことが
透明化の点で好ましい。
Wherein R 20 is an alkyl group having 8 to 18 carbon atoms, and the sum of s and t is 5 to 60, preferably 5 to 60.
The number is forty. The transparent liquid softener of the present invention may contain components such as fragrances, antibacterial agents, and pigments that are usually added to such an extent that they do not hinder transparency. However, calcium chloride, which is usually blended in a softener as a viscosity modifier and an anti-gelling agent, hinders transparency, so it should be kept at 500 ppm or less, and it is desirable that substantially no calcium chloride be added. However, surfactants such as fatty acid salts include sodium salts and potassium salts, but the inorganic salts mixed into the composition by use of such surfactants are not limited to the above. In addition, nonionic compounds having at least one alkyl or alkenyl group having 8 to 20 carbon atoms other than the component (d), such as triglyceride and diglyceride, which are often compounded in view of flexibility and stability, are preferred. , Monoglyceride, pentaerythritol mono-, di-, triester, sorbitan ester and other polyhydric alcohol fatty acid esters are compounded in an amount of 1
% By weight or less, and it is preferable not to mix them substantially in terms of transparency.

【0025】さらに本発明では通常配合されるエタノー
ルやイソプロパノールなどの溶媒成分を実質上配合しな
いことが透明化の点から望ましい。但し、4級アンモニ
ウム化合物や3級アミンの酸塩を製造するときには、反
応溶媒としてエタノールやイソプロパノールが一般に使
用されるため、4級アンモニウム化合物や3級アミンの
酸塩中には1〜30重量%溶媒が混入している。このた
め、このような柔軟基剤を使用する場合、上記溶媒が本
発明の組成物に入ることになるが、このような溶媒は組
成物中に5重量%以下、好ましくは3重量%以下、より
好ましくは1重量%以下にすることが望ましい。
Further, in the present invention, it is desirable from the viewpoint of clarification that a solvent component such as ethanol or isopropanol which is usually added is not substantially added. However, when an acid salt of a quaternary ammonium compound or a tertiary amine is produced, since ethanol or isopropanol is generally used as a reaction solvent, 1 to 30% by weight is contained in the acid salt of a quaternary ammonium compound or a tertiary amine. Solvent is mixed. For this reason, when using such a soft base, the above-mentioned solvent is included in the composition of the present invention, and such a solvent is contained in the composition in an amount of 5% by weight or less, preferably 3% by weight or less, More preferably, the content is desirably 1% by weight or less.

【0026】本発明の液体柔軟剤組成物のpHは、安定
性の点から1.5〜6.0、好ましくは1.5〜5.0
である。このような範囲外では、柔軟基剤のエステル結
合が貯蔵中に分解するため好ましくない。
The pH of the liquid softener composition of the present invention is from 1.5 to 6.0, preferably from 1.5 to 5.0, from the viewpoint of stability.
It is. Outside of such a range, the ester bond of the flexible base is undesirably decomposed during storage.

【0027】本発明の透明液体柔軟剤の調製法は特に制
限されないが、液体柔軟剤の配合成分のうち少なくとも
(a)成分、(b)成分、(c)成分及び水を50〜8
0℃で混合した後、0〜30℃に冷却し、再度加熱し5
0〜80℃の状態で1〜60分間置いた後、再度0〜3
0℃に冷却して調製する方法が最も透明性を与える好ま
しい製法である。具体的な製法を下記する。 工程(A);攪拌羽を有する混合機を取り付けた攪拌槽
に水を入れ、55〜80℃、好ましくは55〜70℃に
水浴により加熱しながら混合する。(a)、(b)およ
び(c)成分、所望により香料、色素、あるいは抗菌剤
を逐次添加し、硫酸、塩酸などの酸或いは水酸化ナトリ
ウムなどの塩基でpHを所望の値に調整する。50〜8
0℃、好ましくは55〜70℃で十分内容物が均一にな
るまで混合する。次に、内容物を冷媒などを使用して0
〜30℃まで冷却する。冷却速度は1〜20℃/分で冷
却することが好ましい。また(d)成分を併用する場合
は、この工程で配合するのが好ましい。 工程(B);工程(A)に引き続いて混合物を再度50
〜80℃、好ましくは55〜70℃に加熱混合する。所
望の温度に到達した段階で1〜30分間、好ましくは1
〜15分間攪拌混合し、その後30℃以下まで冷却す
る。この時の冷却速度は3℃/分〜20℃/分、好まし
くは5℃/分〜15℃/分が好ましく、冷媒等を使用し
て冷却する。(b−2)成分を配合する場合、工程
(B)の直前で配合するのが、より透明感を与える上で
好ましい。
The method for preparing the transparent liquid softener of the present invention is not particularly limited, but at least the components (a), (b), and (c) and water of the compounding components of the liquid softener are 50 to 8%.
After mixing at 0 ° C., cool to 0-30 ° C. and heat again to
After leaving for 1 to 60 minutes at 0 to 80 ° C, 0 to 3 again
The method of preparing by cooling to 0 ° C. is the preferred production method that gives the most transparency. The specific production method is described below. Step (A): Water is put into a stirring tank equipped with a mixer having stirring blades, and mixed while heating to 55 to 80 ° C, preferably 55 to 70 ° C by a water bath. The components (a), (b) and (c) and, if desired, a fragrance, a dye or an antibacterial agent are sequentially added, and the pH is adjusted to a desired value with an acid such as sulfuric acid or hydrochloric acid or a base such as sodium hydroxide. 50-8
Mix at 0 ° C., preferably 55-70 ° C., until the contents are sufficiently uniform. Next, the contents are reduced to 0 using a refrigerant or the like.
Cool to 3030 ° C. The cooling rate is preferably 1 to 20 ° C./min. When the component (d) is used in combination, it is preferable to mix it in this step. Step (B); following step (A), the mixture is again
To 80 ° C, preferably 55 to 70 ° C. Once the desired temperature has been reached, 1-30 minutes, preferably 1 minute
Stir and mix for ~ 15 minutes, then cool to 30 ° C or less. The cooling rate at this time is 3 ° C./min to 20 ° C./min, preferably 5 ° C./min to 15 ° C./min, and cooling is performed using a refrigerant or the like. In the case of blending the component (b-2), it is preferable to blend the component immediately before the step (B) in order to give a more transparent feeling.

【0028】本発明では上述のように、2回加熱、冷却
を繰り返すことにより液体柔軟剤に効率よく透明性を与
えることができる。
In the present invention, transparency can be efficiently imparted to the liquid softener by repeating heating and cooling twice as described above.

【0029】[0029]

【発明の効果】本発明によれば、配合の自由度の高い透
明な液体柔軟剤を提供することができる。
According to the present invention, a transparent liquid softener having a high degree of freedom in compounding can be provided.

【0030】[0030]

【実施例】実施例1〜5、比較例1〜3 1.柔軟基剤の合成 1−1.柔軟基剤(a−1)の合成EXAMPLES Examples 1 to 5 and Comparative Examples 1 to 3 1. Synthesis of flexible base 1-1. Synthesis of flexible base (a-1)

【0031】[0031]

【化9】 Embedded image

【0032】[R; 炭素数17および15が混合した飽
和アルキル基(炭素数17:炭素数15=60/40、
重量比)] N−メチルエタノールアミンとアクリロニトリルの付加
物を用いて公知の方法[ J. Org. Chem.,26,
3409,(1960)]で合成したN−(2−ヒドロキシ
エチル)−N−メチル−1,3−プロピレンジアミン6
6gとステアリン酸/パルミチン酸混合脂肪酸(モル比
60/40)284gをフラスコに仕込み、180℃ま
で昇温した。その温度で約10時間、生成する水を留去
しながら加熱した。反応終了後室温まで冷却し、アミン
化合物(a−1' )を得た。次に(a−1' )をアミン
に対して当量の塩酸水溶液に溶解し、得られた水溶液を
凍結乾燥して(a−1)を得た。
[R; a saturated alkyl group having 17 and 15 carbon atoms mixed (17 carbon atoms: 15 carbon atoms = 60/40;
Weight ratio)] A known method using an adduct of N-methylethanolamine and acrylonitrile [J. Org. Chem., 26 ,
3409, (1960)] and N- (2-hydroxyethyl) -N-methyl-1,3-propylenediamine 6
6 g and 284 g of stearic acid / palmitic acid mixed fatty acid (molar ratio 60/40) were charged into a flask, and the temperature was raised to 180 ° C. The mixture was heated at that temperature for about 10 hours while distilling off generated water. After the completion of the reaction, the resultant was cooled to room temperature to obtain an amine compound (a-1 ′). Next, (a-1 ′) was dissolved in an aqueous hydrochloric acid solution equivalent to the amine, and the resulting aqueous solution was freeze-dried to obtain (a-1).

【0033】1−2.柔軟基剤(a−2)の合成1-2. Synthesis of flexible base (a-2)

【0034】[0034]

【化10】 Embedded image

【0035】[R; 炭素数17および15が混合した飽
和アルキル基(炭素数17:炭素数15=60/40、
重量比)] 1−1で合成したアミン化合物(a−1' )300gを
8−アセチル化ショ糖変性エタノール60gに溶解し、
オートクレーブに仕込み、メチルクロライド28gを圧
入した。100℃で8時間反応した後、減圧で8−アセ
チル化ショ糖変性エタノールを留去して化合物(a−
2)を得た。(a−2)中には8−アセチル化ショ糖変
性エタノールが1.3重量%含まれていた。
[R: a saturated alkyl group having a mixture of 17 and 15 carbon atoms (17 carbon atoms: 15 carbon atoms = 60/40;
(Weight ratio)] 300 g of the amine compound (a-1 ′) synthesized in 1-1 was dissolved in 60 g of 8-acetylated sucrose-modified ethanol,
The autoclave was charged, and 28 g of methyl chloride was injected. After reacting at 100 ° C. for 8 hours, the 8-acetylated sucrose-denatured ethanol was distilled off under reduced pressure to remove the compound (a-
2) was obtained. (A-2) contained 1.3% by weight of 8-acetylated sucrose-denatured ethanol.

【0036】2.透明液体柔軟剤の調製 表1に示す組成の柔軟剤を下記に示す製法で調製した。 2−1.配合成分の詳細 (a)成分;前記の方法にて合成した化合物(a−1)
及び(a−2) (b)成分; (b−1)成分 (b−1−1)
2. Preparation of Transparent Liquid Softener A softener having the composition shown in Table 1 was prepared by the following production method. 2-1. Details of compounding components (a) component; compound (a-1) synthesized by the above method
And (a-2) a component (b); (b-1) a component (b-1-1)

【0037】[0037]

【化11】 Embedded image

【0038】[R; 炭素数17および15が混合した直
鎖のアルキル基(炭素数17:炭素数15=60/4
0、重量比)] (b−1−2)
[R; a linear alkyl group having 17 and 15 carbon atoms mixed (17 carbon atoms: 15 carbon atoms = 60/4)
0, weight ratio)] (b-1-2)

【0039】[0039]

【化12】 Embedded image

【0040】[R; 炭素数17および15が混合した直
鎖のアルキル基(炭素数17:炭素数15=60/4
0、重量比)] (b−2)成分 (b−2−1)前記化合物(13)において、R18が炭
素数11の直鎖アルキルのもの (b−2−2)前記化合物(16)において、R18が炭
素数12、14、16の直鎖アルキルであり、C12/C
14/C16=60/25/15のもの (c)成分;(c−1)ルナックS−50(ステアリン
酸、花王(株)製) (d)成分;(d−1)ラウリルアルコールにエチレン
オキシドを平均21モル付加したもの (d−2)ラウリルアミンにエチレンオキシドを平均4
0モル付加したもの その他の成分((e)成分) (e−1)塩化カルシウム (e−2)エキセル150(ステアリン酸モノ,ジ、ト
リグリセリド混合物(モノ:ジ:トリ=60:35:
5、重量比)花王(株)製) (e−3)香料 2−2.液体柔軟剤の調製方法 1Lガラス製ビーカーにイオン交換水を入れ、ウォータ
ーバスにより60℃まで加熱した。(a)〜(e)成分
を攪拌しながら逐次添加し、pHをN/10HCl溶液
により3.0に調整した。さらに30分間、60℃に保
ったまま混合した後、20℃の水浴により攪拌しながら
30℃以下まで冷却した(冷却速度1.5℃/分)。
(b−2)成分を使用する場合は、冷却後に添加した。
次にウォーターバスにより再度60℃まで加熱し、5分
間攪拌後、5℃の水浴により急冷した。30℃以下の温
度に達するまで約4分を要した(7.5℃/分)。最終
的に20℃の温度にまで冷却後、攪拌を止め、1時間放
置した後、柔軟剤組成物の透明性を評価した。透明性
は、島津製作所製UV−2500PC型測定機器を用
い、測定セルは光路長10mmの石英セルを使用し、対
照側セルにイオン交換水を入れた場合の660nmの波
長の光透過率により評価した。結果を表1に示す。
[R; a linear alkyl group having 17 and 15 carbon atoms mixed (17 carbon atoms: 15 carbon atoms = 60/4)
(0, weight ratio)] (b-2) Component (b-2-1) In the compound (13), R 18 is a straight-chain alkyl having 11 carbon atoms. (B-2-2) The compound (16) In the formula, R 18 is linear alkyl having 12, 14, 16 carbon atoms, and C 12 / C
14 / C 16 = 60/25/15 (c) component; (c-1) LUNAC S-50 (stearic acid, manufactured by Kao Corporation) (d) component; (d-1) lauryl alcohol to ethylene oxide (D-2) laurylamine and ethylene oxide on average 4 mol
0 mol added Other components (component (e)) (e-1) Calcium chloride (e-2) Exel 150 (mono, di, triglyceride mixture of stearic acid (mono: di: tri = 60: 35:
(5, weight ratio) manufactured by Kao Corporation) (e-3) Fragrance 2-2. Preparation Method of Liquid Softener Ion-exchanged water was placed in a 1 L glass beaker, and heated to 60 ° C. in a water bath. The components (a) to (e) were sequentially added with stirring, and the pH was adjusted to 3.0 with a N / 10 HCl solution. After mixing for another 30 minutes while maintaining the temperature at 60 ° C., the mixture was cooled to 30 ° C. or less while stirring with a water bath at 20 ° C. (cooling rate: 1.5 ° C./min).
When the component (b-2) was used, it was added after cooling.
Next, the mixture was heated again to 60 ° C. in a water bath, stirred for 5 minutes, and then rapidly cooled in a 5 ° C. water bath. It took about 4 minutes to reach a temperature below 30 ° C. (7.5 ° C./min). Finally, after cooling to a temperature of 20 ° C., stirring was stopped, and the mixture was allowed to stand for 1 hour, and then the transparency of the softener composition was evaluated. Transparency was evaluated using a UV-2500PC type measuring device manufactured by Shimadzu Corporation, a quartz cell having an optical path length of 10 mm, and a light transmittance at a wavelength of 660 nm when ion-exchanged water was placed in the control cell. did. Table 1 shows the results.

【0041】[0041]

【表1】 [Table 1]

───────────────────────────────────────────────────── フロントページの続き (72)発明者 田方 秀次 和歌山県和歌山市湊1334 花王株式会社研 究所内 Fターム(参考) 4L033 AC02 BA14 BA17 BA45 BA71 BA86  ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Hideji Takata 1334 Minato, Wakayama-shi, Wakayama Prefecture Kao Research Laboratory F-term (reference) 4L033 AC02 BA14 BA17 BA45 BA71 BA86

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 下記(a)〜(c)成分を含有し、pH
が1.5〜6.0である透明液体柔軟剤。 (a)分子中に1つ以上のエステル基及び2つ以上の炭
素数11〜20のアルキル基又はアルケニル基を有す
る、4級アンモニウム化合物又は3級アミン化合物の酸
塩 5〜25重量% (b)下記化合物(b−1)及び(b−2)から選ばれ
る1種以上 0.1〜15重量% (b−1)分子内に1つの炭素数11〜20のアルキル
基又はアルケニル基を有する、4級アンモニウム化合物
又は3級アミン化合物の酸塩 (b−2)分子内に1つの炭素数6〜20のアルキル基
又はアルケニル基を有する両性界面活性剤 (c)炭素数8〜20の脂肪酸又はその塩 0.05〜
2.0重量%
1. A composition containing the following components (a) to (c):
Is 1.5 to 6.0. (A) an acid salt of a quaternary ammonium compound or a tertiary amine compound having one or more ester groups and two or more alkyl groups or alkenyl groups having 11 to 20 carbon atoms in the molecule 5 to 25% by weight (b ) One or more selected from the following compounds (b-1) and (b-2) 0.1 to 15% by weight (b-1) having one alkyl group or alkenyl group having 11 to 20 carbon atoms in the molecule Acid salts of quaternary ammonium compounds or tertiary amine compounds (b-2) amphoteric surfactant having one alkyl or alkenyl group having 6 to 20 carbon atoms in the molecule (c) fatty acid having 8 to 20 carbon atoms Or a salt thereof 0.05 to
2.0% by weight
【請求項2】 更に(d)成分として炭素数8〜18の
アルコール又はアミンのアルキレンオキシド付加物(ア
ルキレンオキシド付加モル数8〜60)を0.3〜10
重量%含有する請求項1記載の透明液体柔軟剤。
2. An alkylene oxide adduct of an alcohol or amine having 8 to 18 carbon atoms (8 to 60 moles of alkylene oxide added) of 0.3 to 10 as a component (d).
The transparent liquid softener according to claim 1, which is contained by weight.
【請求項3】 請求項1又は2記載の液体柔軟剤の配合
成分のうち少なくとも(a)成分、(b)成分、(c)
成分及び水を50〜80℃で混合した後、0〜30℃に
冷却し、再度加熱し50〜80℃の状態で1〜60分間
置いた後、再度0〜30℃に冷却する請求項1又は2記
載の透明液体柔軟剤の製法。
3. A component of the liquid softener according to claim 1 or 2, wherein at least component (a), component (b) and component (c).
The component and water are mixed at 50 to 80 ° C, cooled to 0 to 30 ° C, heated again, left at 50 to 80 ° C for 1 to 60 minutes, and then cooled to 0 to 30 ° C again. Or a method for producing the transparent liquid softener according to 2.
JP13011299A 1999-05-11 1999-05-11 Transparent liquid softener Expired - Fee Related JP3859901B2 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002074729A2 (en) * 2001-03-20 2002-09-26 Cognis Ibéria S.L. Quaternary surfactants
US7824667B2 (en) 2001-04-30 2010-11-02 Cognis Ip Management Gmbh Use of cationic preparations

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002074729A2 (en) * 2001-03-20 2002-09-26 Cognis Ibéria S.L. Quaternary surfactants
WO2002074729A3 (en) * 2001-03-20 2003-10-02 Cognis Iberia Sl Quaternary surfactants
US7824667B2 (en) 2001-04-30 2010-11-02 Cognis Ip Management Gmbh Use of cationic preparations

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Publication number Publication date
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