JPH0778234B2 - Method for producing detergent composition - Google Patents

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a method for producing a liquid detergent composition containing an anionic surfactant and a nonionic surfactant. The present invention more particularly relates to a continuous process for the preparation of high surfactant content liquid detergent compositions comprising anionic and nonionic surfactants.

[0002]

2. Description of the Related Art European patent application EP-A-265 203
No. (Univerer) shows fluidity at 20 to 80 ° C., and contains 80% by weight or less of sodium salt or potassium salt of alkylbenzene sulfonate or alkyl sulfate, 80% by weight or less of ethoxylated nonionic surfactant, and water. Liquid surfactant compositions are disclosed that include less than or equal to 10% by weight. Liquid surfactant compositions of this type can be used as concentrated liquid detergents, such as dishwashing liquids. This liquid surfactant composition is sprayed onto a solid particle absorbent material, such as a porous spray-dried base powder having low bulk density and little or no active to form a larger bulk density detergent base powder. You can also do it.

EP-A-265 203 discloses two methods for producing such concentrated liquid surfactant compositions. In the first method, a neutralized alkylbenzene paste (neutralizing salt), which usually contains about 50% by weight of the active substance.
Slowly add liquid nonionic surfactant to. Then, the obtained viscous mixture having a water content of 10% or more is heated, and a sufficient amount of water is evaporated so that the final water content is 10% or less.

In the second method, the alkylbenzene sulfonic acid is mixed with a nonionic surfactant and the mixture is treated with a sufficient amount of concentrated aqueous sodium hydroxide or potassium hydroxide solution to partially or completely neutralize it. .

Good results may be obtained in the production of liquid detergent compositions using the above-mentioned method. However,
The first method requires evaporation of water, which is time consuming and energy intensive. The disadvantage of the second method is that the long interaction between the nonionic surfactant and the acidic substance, eg the acidic anionic surfactant precursor, can result in chemical degradation of the nonionic surfactant, which results in Dioxane can be produced. Thus, the present invention provides a better method for making a liquid surfactant composition having an anionic surfactant and a nonionic surfactant and having a relatively low water content.

It has been found in accordance with the present invention that a better method for producing a liquid surfactant composition as described above is obtained. In this method, essentially equimolar amounts of a liquid acidic anionic surfactant precursor and a neutralizing agent are simultaneously blended in the presence of a nonionic surfactant.

DEFINITION OF THE INVENTION The present invention is a process for preparing a liquid surfactant composition comprising an anionic surfactant and a nonionic surfactant having a relatively low water content, which is essentially equimolar. And a liquid acidic precursor of an anionic surfactant are simultaneously blended in the presence of a nonionic surfactant. The process is preferably carried out continuously, more preferably in a loop reactor.

[0008] The principle of the method of the details present invention relates to a fluid that functions as a solvent or diluent nonionic surfactant includes a and neutralizing anionic surfactant corresponds to an anionic surfactant The addition of an acid and a neutralizing agent consists in neutralizing the acid with a neutralizing agent of a strength such that the final product has a desired low water content.

The liquid acid or acidic anionic surfactant precursor corresponding to the anionic surfactant is usually a commercially available stable organic compound. Specific examples thereof include Dobanic 113, C ₁₂ -C ₁₅ alkylbenzene sulfonic acid available from Shell.

However, since the acidic anionic surfactant precursor of the primary alkyl sulfate is considered to be inferior in stability, it is advantageous that it is formed immediately before the neutralization reaction by sulfation of the corresponding alcohol.

As neutralizing agent, in principle any suitable alkaline substance may be used, preferably in the form of a concentrated aqueous solution. A preferred neutralizing agent is a concentrated aqueous solution of alkali metal hydroxide, such as a 50 wt% aqueous solution of sodium hydroxide. Alternatively, a concentrated alkaline silicate solution may be used.

The process according to the invention for producing a surfactant mixture is, for example, carried out with continuous stirring at a controlled temperature and an equimolar amount of anion in a reaction vessel containing the required amount of nonionic surfactant. It can be carried out batchwise by adding an ionic precursor and a neutralizing agent. However, this method continuously feeds the anionic surfactant precursor, the nonionic surfactant and the neutralizing agent in the required amounts into the reactor, and the liquid surfactant composition produced after neutralization occurs. It is preferred to carry out continuously by recovering the product.

In a particularly preferred embodiment of the invention, the process is carried out continuously in a loop reactor. Loop reactors are known to those skilled in the art and, to the knowledge of the inventors, they have only been used to neutralize acidic anionic surfactant precursors with aqueous sodium hydroxide.

In the method according to the invention, it is usually the case in European patent application No. 2
A liquid surfactant composition corresponding to the liquid surfactant composition described in No. 65,203 is produced, but it is also possible to produce a liquid composition having a higher water content. The water content of the surfactant mixture prepared by the method of the present invention is 25% by weight or less, preferably 15% by weight or less. A particularly preferable water content is 10% by weight or less.

The liquid surfactant composition produced by the method of the present invention contains one or more anionic surfactants so that the composition maintains fluidity in the temperature range of 20 to 95 ° C.
-80% by weight, preferably 15-80% by weight, one or more nonionic surfactants 10-99% by weight, preferably 10-85% by weight and a minimum of water. The most preferable content range of the surfactant is 30 to 70% by weight of the anionic surfactant and 30 to 70% by weight of the nonionic surfactant.

As the anionic surfactant component of this composition, the sodium or potassium salt of a liquid acidic surfactant precursor may be used. Alkyl sulphates, alkyl benzene sulphonates, alkyl ether sulphates or fatty acid ether sulphates may be used.
Particularly suitable are sodium alkylsulfates having an alkyl group of 10 to 20, preferably 12 to 18 carbon atoms, and sodium alkylbenzenesulfonate having an alkyl group of 10 to 18 carbon atoms. It is also possible to use mixtures of these anionic surfactants.

The nonionic surfactant may be any suitable nonionic surfactant which is liquid at temperatures below about 80 ° C. or which can be easily liquefied. Suitable nonionic surfactants of this type are C ₁₂ -C ₁₅ aliphatic alcohols ethoxylated with ethoxylated fatty alcohols, for example an alcohol per mole 2-10 moles of ethylene oxide. Specific examples of preferable nonionic surfactants include 3
Pieces or 7 C ₁₃ fused ethoxy group ~C ₁₅ Synper commercially available fatty alcohols, for example ICI
onics A3 or A7 ™.

The prepared surfactant mixture has a weight ratio of anionic surfactant to nonionic surfactant of 0.125:
1 to 4: 1 is preferable. However, compositions with anionic surfactant to nonionic surfactant ratios of greater than about 1.5: 1 have generally been found to be more viscous and therefore less preferred. Particularly preferred compositions prepared by the method of the present invention have a ratio of anionic surfactant to nonionic surfactant of 0.2: 1 to 2: 1.

The liquid surfactant composition produced by the method of the present invention may further comprise free fatty acids. For example, these compositions contain 0.5 to 20% by weight of fatty acids having 8 to 22 carbon atoms, preferably 2 to 15% by weight, more preferably 2 to
It may comprise 7% by weight. Fatty acids preferably have 12 carbon atoms.
It is preferable to contain ~ 20, more specifically 16-18.

The liquid surfactant composition prepared by the method of the present invention is advantageously used in the preparation of a high bulk density granular detergent composition having a high active detergent content as described in EP-A-367 339. obtain.

The present invention will be described in more detail below with reference to non-limiting examples. Parts and% are parts by weight and% by weight, unless otherwise specified.

The abbreviations used are as follows: ABS: C ₁₂ -C ₁₅ alkylbenzene sulfonic acid, Sh
ell's _{Dobanic 113, PAS: C 12 ~C} 13 , or C ₁₂ -C ₁₅ primary alkyl sulphates obtained by sulphating alcohols (each Enichem Co. Lial 123 or 1
25), LES: lauryl ether sulfate, NI: nonionic surfactant (ethoxylated C ₁₃ -C ₁₅ fatty alcohols).

Examples 1-3 The following fluid liquid alkylbenzene sulfonate / nonionic surfactant mixtures were prepared in a typical neutralization loop reactor. The reactor is essentially a closed loop type and has an in-line mix.
r). Downstream is the heat exchanger, and in front of the mixer there are three inlets used for the liquid anionic acid precursor, the nonionic surfactant and the aqueous sodium hydroxide solution. Further upstream is provided an outlet through which the neutralized surfactant composition can be discharged. Most of the product is recycled into the loop.

First, in a loop, Synperonic A
3 and Synperonic A7 with a ratio of 4: 3
Filled with nonionic surfactant. Next
Then, mix this nonionic surfactant mixture with sodium hydroxide.
48 wt% aqueous solution and liquid anionic acid precursor (Doba
nic 113) and were continuously added. Natri hydroxide
The amount of um should be just enough to neutralize the acid.
Selected. Of anionic vs. nonionic surfactants
Feed stream of nonionic surfactant to vary the ratio
The amount was set at three different levels. Starting material supply flow
The amount and calculated composition of the surfactant blend prepared.
Shown in. The temperature of the cooling liquid was 50 ° C. Fruit Example1 Two Three Anionic acid supply flow rate (kg / hour) 10 10 10 NaOH (48%) supply flow rate (kg / hour) 2.59 2.59 2.59 NI supply flow rate (kg / hour) 21 11.5 5.25 Anionic detergent% 30.7 44.0 54.7 Nonionic detergent% 63.6 48.3 35.7 H₂O% 5.7 7.7 10 Anionic Surfactant / Nonionic Surfactant Ratio 0.5 1 2 The surfactant compositions of Examples 1 and 2 were readily prepared in loops.
It was operable and showed a liquid state at room temperature. Set of Example 3
The product is more viscous and therefore more difficult to handle.
It was

Examples 4 to 6 The procedure of Examples 1 to 3 was repeated using primary alkyl sulphate (PAS) as an anionic surfactant and Synperonic A7 as the only nonionic surfactant. . The PAS acid precursor is used in a falling film reactor (FFR = falling film).
reactor), ie, Lial 123, that is, C _{12 to} C ₁₃
Prepared by sulphating an alkanol with SO ₃ . This PAS acid was introduced into the loop reactor immediately after preparation. The feed rates of the starting materials and the calculated composition of the prepared surfactant blends are shown below. Coolant temperature is 5
It was 0 ° C. and the pH of the final composition was 11-14.

Example 4 Supply flow rate of Lial 125 to 5 6 FFR (kg / hour) Supply flow rate of SO ₃ (4% in air) to 10 10 10 FFR (kg / hour) 4.9 4.9 4.9 NaOH (48%) supply Flow rate (kg / hour) 4.2 4.2 4.2 NI supply flow rate (kg / hour) 29 14.5
7.25 Anionic Detergent% 31.5 45.4 58.3 Nonionic Detergent% 61.3 44.2 28.4 H ₂ O% 6.5 9.4 12.1 Anionic Surfactant / Nonionic Surfactant Ratio 0.5 1 2 The surfactant compositions of Examples 4 and 5 were It was easy to operate in the loop and showed a liquid state at room temperature. The composition of Example 6 was more viscous and therefore more difficult to operate.

[0027] Using slightly changed embodiment 7-8 condition, and Lial 125 a (C ₁₂ -C ₁₅ alcohol) as the starting alcohol, Example 4
The operation of 6 was repeated. The feed flow rate of the starting materials and the composition of the prepared surfactant blend are shown below.

Example 7 Lial 125 supply flow rate to 8 FFR (kg / hour) SO ₃ (4% in air) supply flow rate to 10 10 FFR (kg / hour) 4.42 4.42 NaOH (48%) supply flow rate (kg) 4.17 4.17 NI supply flow rate (kg / hour) 25.2 12.6 Anionic detergent% (analytical value) 28.4 41.1 Nonionic detergent% (calculated value) 58.4 41.2 H ₂ O% 7.1 10.0 Anionic surfactant / nonionic interface Activator ratio 0.5 1 Example 9 The procedure of Examples 4-6 was repeated using lauryl ether sulphate (LES) as the anionic surfactant. LES acid precursor is Synperonic in FFR
It was prepared by sulphating an A3 nonionic surfactant. Sy as the only nonionic surfactant
nperonic A7 was used. The feed flow rate of the starting materials and the composition (analytical value) of the prepared surfactant blend are shown below. The temperature of the cooling liquid was 50 ° C. and the pH of the final composition was 11-14.

Example 9 Synperonic A3 supply flow rate (kg / hr) to FFR 10 SO ₃ (4% in air) supply flow rate (kg / hr) 4.54 NaOH (48%) supply flow rate (kg / hr) to 10 FFR 4.1 NI supply flow rate (kg / hour) 29 Anionic detergent% 30.4 Nonionic detergent% 62.5 H ₂ O% 7.1 Anionic surfactant / nonionic surfactant ratio 0.5 The resulting surfactant composition is in the loop. It was easy to operate and was fluid at room temperature.

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁶ Identification number Internal reference number FI technical display part C11D 1:72) (72) Inventor Amanda Jane Jeffreys Merseyside El 63, England 2. El-F, Willal, Bebington, Derwent Road, 53 (72) Inventor David T. William Roberts United Kingdom, Merseyside El 63, 9 El Day, Willar, Bebington, Poulton Road 63 (56) Reference JP-A-52-78828 (JP, A)

Claims (9)

[Claims] 1. A method for producing a liquid surfactant composition having an anionic surfactant and a nonionic surfactant and having a relatively low water content, which comprises essentially equimolar amounts of a neutralizing agent and an anionic surfactant. A method comprising simultaneously blending a liquid acidic precursor of an ionic surfactant in the presence of a nonionic surfactant. 2. The method according to claim 1, which is carried out continuously. 3. The process according to claim 1, which is carried out continuously in a loop reactor. 4. The method according to claim 1, wherein the anionic surfactant is an alkylbenzene sulfonate. 5. The method according to any one of claims 1 to 3, wherein the anionic surfactant is a primary alkyl sulfate. 6. The method according to claim 1, wherein the nonionic surfactant is an ethoxylated fatty alcohol. 7. The method according to claim 6, wherein the nonionic surfactant is a C _{12 to} C ₁₅ fatty alcohol ethoxylated with 3 to 7 ethoxy groups. 8. The method according to claim 1, wherein the neutralizing agent is a concentrated aqueous solution of an alkali metal hydroxide. 9. The water content of the resulting surfactant composition is 2.
The method according to any one of claims 1 to 8, which is 5% by weight or less.