JPH02189399A - Monogyceride sodium sulfate detergent composition and its preparation - Google Patents

Abstract

PURPOSE: To provide the bar-like subject composition excellent is homogeneity and foaming property, and minimized in manifestion of rough deposits even when washed in cold water by preparing a solvent solution of a water-soluble higher fatty acid monoglyceride sulfate, a water-soluble higher fatty acid soap and a higher fatty acid, and subjecting the solution to a specified treatment.

CONSTITUTION: The subject composition is produced by preparing a solvent of a higher fatty acid (e.g. isopropanol) which comprises a mixture of a water- soluble fatty acid monoglyceride sulfate, preferably, a higher fatty acid monoglyceride sodium sulfate preferably having 12-18C within higher aliphatic acyl groups in monoglyceride part; a water-soluble higher fatty acid soap, preferably, a Na soap of a higher fatty acid having 12-18C within higher aliphatic acyl group; and a higher fatty acid preferably having 12-18C, removing the solvent preferably by drying while raising the temperature to recover a homogenous solid composition, and extruding the composition into a bar shape.

COPYRIGHT: (C)1990,JPO

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a monoglyceride sulfate detergent composition wound bar and a method for producing the same. The method of the present invention relates to a wound rod of the above composition with good hardness, gentleness (to the skin), tactile sensation and homogeneity properties, in particular to a product with improved homogeneity without surface roughness even when washed in cold water. dissolves the main components of its detergent composition in an aqueous organic solvent solution and rapidly dries it to produce homogeneous detergent composition "chips" or solids, which are subsequently processed into bar and cake forms.

(Prior Art) Monoglyceride sulfate detergents are known in the art (4:i) and are added to detergents sold in the United States and other countries. IIALO■) is based on the ammonium salt of cocomonoglyceride KM. The applicant also sells a synthetic detergent under the trade name VEL■, which essentially consists of sodium cocomonoglyceride sulfate and soap. Synthetic detergent bar Charmis (CIIA)
RMIS (■)), which is mainly composed of soap and contains a small amount of sodium cocomoglyceride sulfate.

However, prior to the present invention, no known synthetic detergent composition bar containing monoglyceride sulfate, soap, and higher fatty acids in which the synthetic organic detergent was present in a greater proportion than the majority component, i.e., the soap and higher fatty acid components. The bars of the present invention, which were not commercially available, have different properties than Vuel and Charmis, presenting other and different problems for compounders and processors.

As a result of searching related prior art, U.S. Patent No. 2.67
No. 8,921; No. 2,868,731; No. 2,8
No. 94.912; No. 3,226,330; No. 3,
No. 376.229; and Japanese Patent Publication No. 137208/1983, in which No. 3.879,309 was found, are also considered to be related. U.S. Patent No. 2,678,921
Describing a monoglyceride sulfate detergent containing a small amount of soap (Example ■), this patent also points to the use of plasticizers such as lower alkylene glycols of higher fatty acids and It also teaches incorporating water-insoluble soaps. U.S. Patent No. 2,868,
No. 731 is a method patent in which water-soluble soaps, anionic and/or nonionic synthetic organic detergent(s) and higher aliphatic carboxylic acids are mixed with a limited proportion of water, and the mixture is heated and slowly It states that it should be in the form of a keyaki. U.S. Pat. No. 2,894,912 (doped (
DOVE's patent) relates to isethionate detergent bars, which may contain soap and free fatty acids (Example v), and may contain other detergents and plasticizers; however, Other detergents mentioned in that patent do not include monoglyceride sulfates; U.S. Pat. A soap-synthetic detergent combination containing water with a limited content of inorganic salts is described. U.S. Patent No. 3,376.229 is
This invention relates to a water-soluble higher fatty acid soap and an isethionic acid ester detergent ring containing a higher fatty acid. The presence of an unesterified water-soluble alkali metal salt of isethionate in the detergent ring at up to about 17% improves firmness, extrudability,
Processing properties are improved. U.S. Patent No. 3,879,3
No. 09 describes a detergent ring based on a mixture of acyl isethionates of a specific chain length range, which provides excellent foaming (L
It is said that it exhibits (atl+ering) characteristics. This bar contains sodium soap, higher fatty acids, sodium isethionate and other synthetic organic detergents, but does not contain monoglyceride sulfate detergents. A detergent ring containing is described, and various additives may be included in this detergent ring, however, the only additives described are water, titanium oxide, cetyl alcohol and sugar 9x.

This detergent ring is said to be harsh on the skin, and is said to be less softening when immersed in soft water than detergent rings made from tallow-coconut oil soap or N-acyl amino acid salts. (Table 2).

(Problems to be Solved by the Invention) Based on the research and analysis of the prior art and commercial products as described above, the subject matter of the present invention is considered to be novel, and both its composition and method are non-obvious.

(Means for Solving the Problems) The method of the present invention for producing a monoglyceride sulfate detergent composition with improved homogeneity and less tendency to roughness when washed with cold water comprises: a water-soluble higher fatty acid monoglyceride sulfate; Preparing a water-soluble higher fatty acid soap and a warm solvent solution of higher fatty acids, removing the solvent from the solution, recovering the resulting homogeneous solid composition, and extruding the composition into rods. Become. Products obtained by such processes and products with similar composition and properties are also encompassed by the invention. In one preferred embodiment of the process of the invention, as a solvent (such as an aqueous solution of Impropatol) A medium is used in which the neutralized monoglyceride sulfate is separated from the sodium sulfate (with which it is present after production due to the neutralization by excess Vi acid), and the monoglyceride sulfate, monoglyceride sulfate,
dissolving soap (kettle soap is preferred) and free fatty acids to produce a soap solution of monoglyceride sulfate, soap and higher fatty acids, and then drying the solution using a smear dryer or evaporator; The homogeneous dry mixture, with further admixture of detergent ring additives if desired, is processed into bars and cakes.

Monoglyceride sulfate, which is the main detergent of the detergent ring of the present invention, is a water-soluble detergent such as a higher fatty acid monoglyceride sulfate alkali metal salt. In some cases, some potassium detergent may be present, for example up to 25% of the monoglyceride sulfate detergent content, but normally such detergents are preferably sodium salts, the higher fatty acyl of the monoglyceride sulfate being between 1O and 10%. 20 carbon atoms, but preferably 12 to 18 carbon atoms, which means that the various mixtures of higher aliphatic acyls present are on average within that range, and substantially (90% or more) The higher aliphatic acyl of the monoglyceride sulfate, preferably in this range, will normally be saturated.

This is because during the sulfation reaction, which is usually carried out in a strongly acidic medium, the unsaturated bond is susceptible to reaction with the sulfating agent and the acyl is cleaved at the bond site. However, using milder conditions (or other manufacturing processes)
It is also possible to prepare monoglyceride sulfates that are unsaturated in the aliphatic acyl moieties and may be used as such ingredients may impart particularly desirable properties to the detergent ring of the product, but typically monoglyceride sulfates Only a portion of the amount, for example up to 40%, is used.

Although it is possible to synthesize fatty acids and make monoglyceride sulfate detergents from this "synthetic" fatty acyl, it is preferable to use saturated to substantially saturated vegetable and/or animal oil(s). ) and/or fat (
It is usually very suitable to prepare monoglyceride sulfates from one or more monoglyceride sulfates. In one preferred method of producing monoglyceride sulfates, such materials may be hydrogenated to minimize the presence of unsaturated groups and facilitate production of the desired monoglyceride sulfates without decomposition of the fatty acyl. Excess fuming sulfuric acid was reacted at elevated temperature (35°C). - to produce glycerol trisulfate (and excess sulfuric acid), and then transesterify 2 moles of glycerol trisulfate with 1 mole of triglyceride (oil and/or fat, preferably hydrogenated) at about 50°C. Then, a 3 mol acid mixture is prepared, namely C11,0OCfl C1l 05Osl-1 Cf (20S Os H plus sulfuric acid, and subsequently 3 mol of this monoesterified glycerol disulfuric acid is mixed with about 4 mol of sulfuric acid and 9 mol of sulfur hydroxide.
Neutralize at 0°C to produce 3 moles of the desired monoglyceride sulfuric acid and 1 to 3 moles of sodium sulfate. Next, the monoglyceride sulfate is preferably dissolved in an aqueous solution of a lower alcohol extractant, preferably Impropatool. Solvent extraction from sodium sulfate using an aqueous solution.

The commercially most desirable "pure" monoglyceride sulfate is 11-cocomoglyceride sulfate.

This is because the products of the invention based on such detergents have the best balance of the desired properties (good foaming and acceptable sulfurate). However, other useful detergents include coco, 1to beef tallow, beef tallow,
Palm, old palm, palm kernel, palm kernel, other vegetable and/or animal oils and/or fats, and various mixtures thereof, preferably hydrogenated.
One particularly good mixture is a mixture of monoglyceride sulfate with cocomonoglyceride [6sodium and sodium palm monoglyceride FILate, usually from 4:1 to 1:2].
A further preferred product is a mixture of palm monoglyceride sulfate (or its H-homogen), preferably in the 1:1 range, preferably in the 1:1 range, both monoglyceride sulfates being hydrogenated. Improved sluff (sl
oth) properties (low slough) and very good foaming properties. Mixtures of coco monoglyceride sulfate and toco monoglyceride sulfate are used, but depending on the application, mixtures of monoglyceride sulfate of beef tallow and coco, beef tallow and [to coco, beef tallow and H-coco, and H-beef tallow and coco are particularly used. In such mixtures (hydrogenated or Detergents containing higher acyls (from coconut and/or palm kernel oil) improve the durability of the detergent bar during use and reduce sloughing and gelling, whereas detergents containing lower acyls (from coconut and/or palm kernel oil) is foaming (fo
aming) as well as lathering (IaLbering). That is, by combining detergents in this manner, the overall performance of the product of the present invention can be improved.

Other types of detergents, such as anionic detergents known as sulfated and/or sulfonated detergents, as well as other sulfated lipophilic substances and sulfonated lipophilic substances, which usually have higher alkyl or acyl moieties, can be supplemented with monoglyceride sulfates. These supplemental detergents which may be included in the detergent bars of the present invention include higher aliphatic alcohol sulfates or alkyl sulfates, olefin sulfonates, paraffin sulfonates, higher alkylbenzene sulfonates, higher aliphatic alcohol polyethoxy sulfates, isethionates and taurides. However, it is preferred that such supplementary detergents be omitted or used in an amount less than 25% of the total detergent content (based on total detergent) of the detergent bar of the present invention.

Higher fatty acid soaps are produced from the vegetable and/or animal oils and/or fats and mixtures thereof mentioned above with respect to the production of monoglyceride sulfates, or fatty acids obtained from such materials.

The soap is usually an alkali metal soap, with sodium soap being highly preferred, or a potassium soap that is compatible with the final product formulation and does not significantly adversely affect its useful properties (preferably some of those properties). Other water-soluble soaps (significantly improved) also total soap content (total soap content)
Such fatty acid soaps typically contain lO in their fatty acyl moiety(s).
20 to 20 carbon atoms, preferably those having 12 to 18 carbon atoms in the aliphatic acyl group(s), oils and/or fats or mixtures thereof, or corresponding fatty acid mixtures. are often hydrogenated before or after mixing, and usually some amount of unsaturation (
up to 10% of the soap content) are preferred;
It has been found that unsaturation improves plasticity and processing properties and aids in the production of homogeneous detergent bars. A highly preferred blended soap comprising a mixture of sodium beef tallow soap and sodium coco soap, in which neither soap is produced from previously hydrogenated raw materials, with beef tallow soap in the majority proportion, and coco soap on the other hand. The ratio of tallowstone@:coco soap, in which the amount will be less than half, is usually from 3:1 to 9:l, preferably from 4:l to 7:1, more preferably from 5:1 to 6.
:1, for example, in the range of about 85:15.

The higher fatty acid(s) used in the WA manufacturing of the detergent rods of the present invention may be higher fatty acids of the type mentioned above or various vegetable and/or animal oils and/or fats or their hydrogenated derivatives (monoglyceride sulfates). and higher fatty acids derived by hydrolysis from soaps (described above with respect to soaps). It is highly preferred that such fatty acid component is at least in part stearic acid, a C18 saturated fatty acid obtained from beef tallow; It is also within the scope of this invention to use other higher fatty acid mixtures of 10 to 20 carbon atoms or 12 to 18 carbon atoms containing fatty acids. Saturated fatty acids are preferred, and among these, a mixture of stearic acid and valmitic acid in a ratio of 1:1 to 2:1, preferably 1:1 to 1.3:1 is most preferred. A mixture containing about 45% stearic acid and about 55% valmitic acid is commercially available under the name "triple-pressed stearic acid."

In the detergent bar of the present invention, the proportions of monoglyceride sulfate, soap and higher fatty acids are usually 35 to 6, respectively.
5%, 8 to 25% and 15 to 40%, preferably 40 to 60%, IO to 20% and 20 to 35%, respectively, and 45 to 55%,
More preferably 12-18% and 22-28%, such as about 51% monoglyceride sulfate, 15% soap, and about 25% fatty acids.

Other components of the detergent bar of the present invention include various additive materials that impart certain desirable properties to the detergent bar. Such additives include blowing agents such as lower alkanolamides such as laurin myristic jetanolamide; pigments and dyes such as colorants such as titanium dioxide, chrome green, ultramarine blue and polar brilliant blue dyes; Optical brighteners such as stilbenes; antioxidants such as benzohydroxytoluene; binders such as starches and modified starches; enzymes such as proteases; excipients such as talc; fungicides, fungicides and fragrances. Considering the higher fatty acid content of the present detergent bar and the presence of some amount of water therein, the use of plasticizers such as higher aliphatic alcohols will not normally be desirable or necessary. The proportion of total additives present in the final detergent ring is small, usually in the range of 1 to 7%, preferably less than 5%, more preferably less than 3%.

Detergent rods often contain one or more accompanying materials in addition to their main components. Sodium monoglyceride sulfate detergents usually contain some amount of sodium WR acid and some amount of lower ether-soluble organic matter as impurities due to the manufacturing method. Contained as. Such organics include glycerol, free fatty acids and mono- and di-tri-glycerides. The content of sodium sulfate is usually between 2 and 10% based on the detergent rod (also based on the percentages of the other ingredients mentioned in this application).
The total amount of organic by-products in the manufacture of monoglyceride sulfate detergents is usually in the range of 1 to 8%, often in the range of 4 to 6%, such as about 5%. Monoglyceride sulfate detergents preferably used in the process of the present invention, often in the range of 5%, such as about 4%, are dissolved in the aqueous solvent extraction medium, usually with water present as well. The water content in I&F detergents is normally in the range of 0.2 to 5%, and 0.5 to 1.5%.
It may be desirable to add water to the amalgam stopper mixture to further improve its plasticity and improve its homogeneity, but usually the total water content will be less than the above. When using titanium dioxide as an additive, the percentage used will generally be within the range of 0.3 to 3%, such as 0.5 to 2%, such as about 1%.
Perfume is also normally present, preferably in a proportion of from 0.4 to 3%, preferably from 0.5 to 2%, such as about 1.5%.

In the process of the present invention, which results in a monoglyceride sulfate-soap-fatty acid mixture with improved homogeneity, from which a homogeneous, non-gritty detergent ring can be produced, the monoglyceride sulfate, soap and higher fatty acid are dissolved in a suitable solvent, followed by The solvent is removed from the solution, leaving a substantially dry, homogeneous solid (with some water present). The homogeneous form of such a preceding solution and solid mixture (or solid solution) results in a product with different properties than simply mixed components, and the solid "mixture" of the present invention is easier to process into bars. and soak the detergent ring in cold water (5 to 2
There is no roughness even when used for hand washing in water at a temperature of 5°C (for example, 15°C).

The preparation, extraction and final bar processing of the detergent of the present invention will be better understood with reference to the accompanying drawings.

FIG. 1 is a schematic diagram or flow sheet showing the method of the present invention.

In the figure, the first stage reactor 11 is a place for sulfating glycerol with fuming sulfuric acid at a temperature of about 35°C.

The obtained glycerol sulfuric acid is fed via line 13 to the second stage reactor 15 where glycerol tri[fi is transesterified with triglyceride at a temperature of about 50° C. to form monoesterified glycerol diFfL acid ( A so-called acid mixture (acid w+ix) is produced and passed via line 17 to a third reactor 19, in which
The glycerol di[4 monoester is neutralized with sodium hydroxide solution to produce monoglyceride Kn sodium. During the production of sodium monoglyceride sulfate, sodium sulfate and ether-soluble organic substances (impurities) are produced as by-products.

There you have it! These include fatty acid hydrolysis products of unreacted glycerol, unreacted diglycerides, and triglycerides. This material is fed via line 21 to extractor 23, to which water and impropatul are added. Inside the extractor, the contents separate into two phases: the aqueous lower phase dissolves and contains most of the sodium monoate, and the aqueous alcoholic upper phase contains monoglyceride sulfates and lipophilic substances, i.e., ether-soluble substances (impropatol). (also soluble in aqueous solution) and some amount of sodium sulfate. The solvent for the upper phase is a co-solvent solution of about l=l in-10panol and water, in a ratio of 2:
After removing the aqueous sodium sulfate phase, which is in the range of 1 to 1:2, preferably 3:2 to 2:3,
The remaining aqueous inpropatol phase containing the monoglyceride sulfate is passed via line 25 to a dissolution tank (mixing tank) 27, where it is fed at elevated temperature with kettle soap in a liquid state and fatty acids (which may be in a solid state).・Add.

Alternatively, the fatty acids may be first emulsified or dissolved in hot kettle soap and then the emulsion or solution dissolved in an extraction medium of an aqueous In-10 panol solution containing monoglyceride sulfate, the temperature of the dissolution bath typically being about in the range of 50 to 90°C, for example about 60°C, the components are completely soluble in each other and also in the aqueous isopropanol medium, and the total solids content is usually in the range of 45 to 65%, for example about 55%. The solution is then passed from the dissolution tank via line 29 to a film dryer or evaporator where the isopropanol and almost all of the water are removed and the remaining homogeneous mixture is used for film drying. When removed from a vessel (usually operated at elevated temperature and reduced pressure), it becomes a solid.

This homogeneous solid mixture is then transferred to an amalgamator 33, where suitable additives such as titanium dioxide and fragrances are mixed into the mixture, and then mill 35.
37, supply to cutter 39 and press 41 one after another,
If all these devices function properly, the properties such as foaming property, foaming property, solubility, volume, sloughness, hardness, non-irritation, texture and homogeneity will be good, making it suitable for washing in cold water. A homogeneous monoglyceride sulfate detergent bar with no surface roughness even when used is produced. It is also possible to discharge the material from the dryer as a liquid (at temperatures in the 60-90°C range), solidify it on chill rolls or other similar "chipping" equipment, and amalgamate the resulting chips. The key steps in the process described above are dissolving the soap, fatty acids and monoglyceride sulfates in an aqueous lower alkanol system, and then drying this solution to remove impropatul and most of the water. This is the process of removing. In the drying process, a wiped film evaporator (a wiped film*+ evaporaLor
) is used. The solvent is usually an aqueous solution of a lower alkanol of 3 or 4 carbon atoms, including in-10 panol, n-10 panol, n-butanol, secondary butanol and imbutanol.

Mixtures of any two or more of such lower alkanols may be used; ethanol may also be used as at least part of the alcohol component, but is less desirable for the process of the present invention due to its low boiling point. The temperature of the hydroalcoholic solvent and solution is usually in the range of 50 to 90°C, preferably 50 to 70°C; It may be at or near the reflux temperature of 0.
Drying of the solution in the M dryer is carried out at an elevated temperature, the temperature (
The temperature of the heat transfer surface of the dryer is 80°C or higher, and 9
In such an acceptable and suitable temperature range, which is often in the range of 0 to 210 degrees Celsius, and preferably in the range of ioo to 150 degrees Celsius, the components of the solution will not deteriorate, and moreover, the dryer process will be easier. The speed is sufficient.

A vacuum may be used to increase the drying rate, the degree of vacuum being in the range of 1 to 100 mm of absolute mercury, preferably 0.
The degree of vacuum is appropriate, such as 5 to 3 mm lg.

Solvents other than lower alkanols can be used to prepare the homogeneous solutions of the present invention from homogeneous "chips" of detergent compositions, and also lower alcohols such as isopropanol, especially aqueous lower alcohol solvent systems such as water. - monoglyceride sulfate in the hydroalcoholic extractant from the extractor in which the monoglyceride sulfate is already dissolved, although the ituburobanol solvent system can be used to dissolve the solid monoglyceride sulfate, soap and fatty acid components of the detergent bar of the present invention; It is highly preferred to use water and impropatol or other lower alcohols as common solvents for soap and fatty acids.

Soap is added to this extraction solution as a kettle soap and heat is supplied to the solution, and the action of the solvent on the fatty acid (usually added as a solid) (which may be preheated or pre-caulked in alcohol). Ideally, this would increase the concentration of the compound to facilitate dissolution into the final solvent system. Alternatively, such fatty acids may be emulsified or dissolved in the kettle soap and the emulsion or solution subsequently mixed with the monoglyceride sulfate extractant, i.e., the method of the present invention is suitable for monoglyceride sulfate drying and kettle soap drying. Skip the second drying process and use the heat of kettle soap,
And, the existing hydroalcoholic solvent medium is used as the solvent for the three main components of the detergent bar.

The fatty acids charged to the dissolution vessel are considered pure for purposes of the present invention. However, the kettle soap used is in a liquid state and may contain raw materials such as triglycerides in small to small amounts.
℃ range, often 65 to 85 degrees Celsius, this kettle soap usually contains small amounts of impurities such as sodium chloride, glycerol and unreacted or partially reacted triglycerides. . However, the presence of relatively small amounts of impurities in such materials does not significantly affect the described method or the final product and is therefore considered irrelevant to the present invention and is not discussed herein. Incidentally, there is no need to consider this in detail.
The term J refers to soaps made by the standard kettle process of reacting triglycerides with sodium hydroxide in salt water and separating the resulting soap phase from the aqueous salt solution phase; the use of such soaps is preferred. However, soaps made by other methods, such as by neutralization of fatty acids, can also be used in the present invention, and such soaps have a similar composition and can be present in single use with water at elevated temperatures. If so, the "kettle soap" preferably used in the method of the present invention is usually in the range of 25 to 35%, for example about 30%.
, and this water is added to the water in the monoglyceride sulfate extractant to form the hydroalcoholic solvent used in the dissolution tank to extract the monoglyceride sulfate,
Dissolves soaps and fatty acids.

This monoglyceride sulfate extractant is an extractor that is placed in a dissolution tank that will normally contain some amount of sodium sulfate and some amount of unreacted and by-product ether solubles, including various glycerides, free fatty acids, and glycerol. The monoglyceride sulfate content of the agent is usually in the range of 80 to 90%, for example about 85%, and the proportion of sodium sulfate and ether solubles is 6 to 10% and 5 to 9%, for example 8% and 7%, respectively. (based on solid content),
The ratio of in-10panol:water in the dissolution tank solution is usually 2
:l to l:2, preferably in the range of 3:2 to 2:3, for example about 3=4, the solids content of this solution is usually in the range of 45 to 65%, preferably is between 50 and 60%, most preferably about 55 or 56%.

In a coated film (or coated surface) dryer (or equivalent device), the solution from the dissolution tank dries very quickly to a very low water content, which typically ranges from 0.2 to 5%. within a few seconds, preferably between 0.5 and 1.5 or 2%, for example about 1%.
This can be done in 10 seconds to 10 seconds, especially when elevated temperature and vacuum are used. Because drying is so rapid, the individual components of the solution do not undergo undesirable crystallization (crystallization has a negative effect on homogeneity), and the resulting product is highly concentrated in all its various components. Homogeneous in the sense of being closely distributed. In fact, the properties of the dried product and the detergent bars made from it differ significantly in various respects from those expected from its individual components, and the differences are due to the fact that the components are uniformly distributed throughout. It can be attributed to being there. Another advantage of the coated film dryer is that the solution or resulting product remains in a hot location for a short period of time, thereby minimizing degradation of heat sensitive materials such as monoglyceride sulfates. This drying operation can be carried out using various film evaporators or driers such as Turba-Fi.
A device sold under the trade name Lm) can be used.

After draining the dried product from the applied film (or applied surface),
The product, which is normally in a liquid state upon discharge from the dryer, is converted to solid chips on chill rolls or otherwise solidified and subsequently processed in a soap amalgamator or other similar mixing vessel. Mixing the Additives The mixture is then ground, preferably in a four-way three-roll or five-roll soap grinder (eg, of the Lehman type), and then extruded into bars. The extruded bar is cut to length and pressed in a standard soap press.

The extrusion operation is preferably carried out in a twin-barrel (upper and lower) vacuum processor equipped with a fine sieve and heated nozzle plates, even when cooled during this operation due to the mechanical work of mixing. Regardless, the temperature is usually maintained within the 25-50°C range, often 30-40°C.
0 °C (temperature measured at the exit from the 10 tube), yet despite this mechanical work and the higher temperature of the "hot spot" of the extruded material mass, the fatty acid does not appear to liquefy or soften enough to cause the extruded mass to collapse; instead, the mass is homogeneous, apparently due to the tight distribution of fatty acids throughout. remains in the state. When crushed and extruded, a conventional amalgam stopper mixture made from the same fatty acids, monoglyceride sulfate and soap, but obtained by filling the dry powder into an amalgamator,
It is observed that the fatty acids separate and have poor extrudability, resulting in an unacceptable detergent bar with poor processability. Such unacceptable detergent bars, in extreme cases, become excessively plastic at common high processing temperatures due to separation of the liquefied fatty acids from the remaining components of the detergent bar acid. Such detergent rods do not press satisfactorily, and the press die is filled with separated sections of flashing and blanks, resulting in ribs that leave marks on the press. Even if the composition can be extruded and squeezed into a cookie shape, when washed in cold water with such a detergent bar, the surface will have a blotchy or rough appearance, and the detergent bar will have a rough texture. This property makes it unacceptable to discerning consumers. Although repeated grinding of the composition prior to extrusion can reduce the roughness of detergent bars made therefrom, such grinding is costly and time consuming and is therefore commercially disadvantageous. In addition, if the chips are repeatedly crushed, the flavor will also be lost, and the hardness of the crushed chips may vary due to uneven "drying" during the crushing process, which may cause new roughness to appear. .

The manufactured detergent rod has good foaming and foaming properties,
The solubility is also desirable and not excessive, does not cause excessive erosion during use, does not form a thick gel coating on its surface, and is satisfactory in consumer reviews when tested with a penetrometer. This detergent bar has a good hardness and does not irritate the skin in both in vivo (collagen) and in vitro tests.This detergent bar has a good feel and is very suitable for soaps that are the standard for a satisfactory feel when held in the hand. The texture is similar. As a result of observing the detergent bar visually and under a microscope and evaluating its various properties, it was found that the detergent bar of the present invention is a detergent with the same formulation, which is produced by mixing various solid components in an amalgamator and then using a conventional processing method. It is much more homogeneous than a bar.

As a variation of the above method, soap and fatty acids, usually in the form of chips (rather than kettle soap), may be added to the monoglyceride sulfate extract, in which the soap formulation also includes, for example, beef tallow; In addition to the 0 soap change being changed to 75:25, the composition of the monoglyceride sulfate is also changed. When the monoglyceride sulfate is a mixture of tallow and coco or palm and coco monoglyceride sulfate (sodium salt) in the range of 1:2 to 2:1, preferably about 1:1, the detergent made therefrom has anti-slough properties and Durability (slow use-up)
), but still foams satisfactorily. In another variant, the sodium monoglyceride sulfate detergent and stearic acid in the form of flakes are dissolved in kettle soap and the resulting melt is converted into chips and subsequently further processed as described above. In yet another variant, the fatty acid charge is prepared in situ.
5iLu) The soap is prepared by partial neutralization and the mixture obtained is mixed with monoglyceride sulfate in solid or solution form and then processed accordingly. Some evidence has been gathered that such in-situ detergent bars have lower sluffing properties than detergent bars produced by conventional amalgamation of powder components and subsequent extrusion. The partial neutralization is preferably carried out in the presence of the monoglyceride sulfate in the blended proportion, and the mixed fatty acids are neutralized to produce a mixed soap.

The detergent bars produced by Kenpo are homogeneous and remain stable even when heated. This property may not be observed in control detergent bars made from powder ingredients.

Examples are shown below, but these examples do not limit the present invention. Unless otherwise specified, all parts and percentages in the examples, other specifications, and claims are based on weight, and all temperatures are °C. It is a display.

Extract 176.5 in which sodium sulfate is separated from the "active ingredient" with an aqueous solution of Impropatol after neutralizing the product of transesterification of glyceryl tri-EiL acid with triglyceride based on "K Ship"1' with sodium hydroxide. 1 part, beef tallow: 21.4 parts of kettle soap of 85:15 and triple-pressed stearic acid (
25 parts of stearic acid (45%) and palmitic acid (55%) were mixed in a dissolution tank (mixing tank) (in the figure, the dissolution tank is indicated by the number 27) as shown in FIG. The aqueous extract of Impropatol monoglyceride sulfate contains approximately 34% solids, 33% water and 33% Impropatul. Approximately 8% of the solids are inorganic (substantially sodium sulfate), 7% are ether solubles (substantially glycerides, fatty acids and glycerol), and the remaining 8% is inorganic (substantially sodium sulfate);
5% was sodium 11-cocomoglyceride sulfate. The kettle soap was 70% solids, and the solids contained small amounts of sodium chloride, glycerol (retained in the soap), fatty acids, and glycerides. Fatty acids are solids when supplied.

The temperature of the extract and fatty acids is room temperature and the temperature of the kettle soap is about 70-75°C.

The mixture was heated to about 60 °C in a dissolution tank and stirred at that temperature for about 1/2 hour until the solution became clear.The solution was then heated to 1.8% absolute [Hg]. The coating surface was fed to a coating surface evaporator (or coating film dryer). In the evaporator, a heat transfer surface is constantly wiped to renew the thin film of solution for drying, the surface temperature of which is 60°C.
The temperature range is from 70°C to 70°C. The drying speed of the Turbafilm evaporator used in the manufacturing test was approximately 500.
hg/hour, which is about 15% higher than the drying rate for the extract alone. Instead of using a Turbafilm evaporator or other film dryer,
Although 4a zzon i) or ProcLorl Schwartz types may also be used, the product of the present invention is more homogeneous and has lower operating temperatures than those produced from other dryers; It is believed that monoglyceride sulfates and other heat sensitive materials are desirably maintained stable.

That is, by using a coated film dryer, a more homogeneous dried product with superior properties is produced.

The product on leaving the coated film dryer is in a molten state but is very easily solidified and the solid obtained by air cooling or surface contact cooling is amalgamated for additive addition before being processed into rod and cake form. directly into the evaporator. In some cases, it is preferred to direct the liquid product from the turber film evaporator to cooling rolls where it is cooled and solidified into thin sheets and ribbons, which are then cut into chips if desired; such chips are than a control product of the same formulation that was dry-blended (not dissolved in an aqueous solution of Improper Tool prior to film drying) or dried from an aqueous dispersion by conventional drying means (not film-based). It has been found that it is easy to transport in conventional material conveying equipment, such as screw conveyors or helix conveyors.

The product discharged from the coating film dryer contains approximately 51% tococomoglyceride sulfate, approximately 4% sodium sulfate,
Approximately 4% ether solubles (with monoglyceride sulfate), 15% soap, 25% mixture of stearic and palmitic acids, and 1% water were all contained in a homogeneous solid form.

Such a homogeneous product is referred to as a detergent bar base.

Fire'' 1 down 4 d Filtration ``1'' Detergent stick base (from Example 1) 97.5 Titanium dioxide (pigment) The ingredients are mixed in a soap amalgamator, ground in a three roll Lehlian mill, extruded in a dual barrel vacuum, cut to desired blank length, and
It was pressed into the final desired cake form in an automatic soap press. The mixing in the amalgamator is approximately room temperature (21”C).
) for about 10 minutes, and the chips were ground to a thickness of about 12 mm. Internal cooling water was used in the mill rolls and the temperature of the ribbon or chips exiting the mill was about 35-40°C. The resulting grinding ribbon was fed to a vacuum prorader, the composition temperature at the exit of which was approximately 40°C.

The detergent bar produced had a nice white appearance, felt very soap-like in the hand, and had a pleasant fragrance. The prepared detergent bars were subjected to foaming and foaming tests and showed satisfactory foaming and acceptable rich lathering.

The detergent bar was not excessively soluble in water and did not wear out too quickly, so its wear rate was acceptable. Although the sluff of the detergent bar was larger than that of the soap bar, the sluffing of the detergent bar of the present invention was lower than that of most detergent bars. The detergent bar thus manufactured has good hardness as evidenced by the needle scale test and is excellently non-irritating to human skin as confirmed by the collagen test and consumer response. there were. The detergent bar was homogeneous and exhibited no stickiness, stickiness, or grittiness after washing with cold water, as evidenced by microscopic examination.

The procedure of Examples 1 and 2 was repeated by replacing sodium coco tallow monoglyceride sulfate containing three parts of coco monoglyceride sulfate for one part of beef tallow monoglyceride sulfate with H-coco monoglyceride sulfate. . Preferably, both the acyls in the coco and tallow monoglyceride sulfates are hydrogenated and the detergent is saturated.

The resulting detergent bar had desirable properties similar to those reported for the detergent bar of Example 2, but with much less sloughing and better foaming and foaming. Ta. Fatty acids can act as plasticizers, especially at elevated temperatures, but as with the composition of Example 2, the composition could be processed without any difficulty despite the presence of fatty acids in the composition. It is believed that the detergent bars thus produced are homogeneous and many of the improved properties described can be attributed to this condition.

! ! By the same general method as described in JuLi Surprising Examples 1-3,
As shown below, by changing the proportions of the ingredients by ±lθ% and ±25% within the range shown in the specification, and by changing the ingredients themselves and the process steps, various other detergent bars belonging to the present invention can be prepared. was manufactured. The WA manufactured product was homogeneous and laboratory testing and consumer acceptance evaluation of the manufactured detergent bars had satisfactory results.

In the detergent bar of the previous example, the various components were present in a homogeneous relationship despite significant differences in their chemical properties. As a result, the composition of the detergent bar has been improved, its properties have been improved, and the drawbacks of previous synthetic detergent bars, which are based on the different and often contradictory properties of ingredients such as soap, synthetic detergents and fatty acids, have been improved. Averted.

In the claims and foregoing descriptions, when describing various compositions and methods, the words "consisting of, comprising, containing,
The word "comprise" is used to leave room for the inclusion of other materials within the scope of the claims. However, when some preferred embodiments of the invention are described as consisting essentially of (or consisting of) various steps and/or ingredients, this does not mean that such This means that the description and claims leave room for the inclusion of other ingredients that do not significantly alter the effects of the invention. Also, detergent compositions consisting of the ingredients and/or steps described. The wound rod and manufacturing method also belong to the present invention.The scope of the description and claims are narrow, and the scope of the patent is closed except for the addition of relatively small amounts of additives and various steps.

Although the present invention has been described with reference to examples, descriptions and embodiments thereof, these should not be construed as limiting the invention. This is because it is clear that products and equivalents can be used.

noon [1”l translated baby urine owl (4 other people)

Claims (1)

[Scope of Claims] 1. A method for producing a monoglyceride sulfate composition rod with improved homogeneity and less tendency to develop roughness even when washed in cold water, the method comprising: a water-soluble higher fatty acid monoglyceride sulfate; preparing a solvent solution of a higher fatty acid soap and a higher fatty acid, removing the solvent from the solution, recovering the resulting homogeneous solid composition, and extruding the composition into rod form. A method for producing a monoglyceride sulfate detergent composition stick. 2. The monoglyceride sulfate is higher fatty acid monoglyceride sodium sulfate having 12 to 18 carbon atoms in the higher aliphatic acyl group of the monoglyceride part; is a sodium soap of a fatty acid; the higher fatty acid is a mixture of higher fatty acids having a carbon atom range from 12 to 18; the solvent is a lower alkanol or a mixture of lower alkanols; The mutual solution of the components is removed; the homogeneous solid composition obtained by this drying is mixed with additives for the bar composition; and the resulting mixture is extruded into bar form and stamped into cake form. The method according to claim 1, characterized in that: 3. Higher fatty acid monoglyceride sodium sulfate may have its fatty acid monoglyceride portion derived from vegetable and/or animal oil and/or fat, and may be partially or fully hydrogenated; Soap may be derived from vegetable and/or animal oils and/or fats; / or mixtures of animal oils and/or fats, which may be partially or fully hydrogenated; higher fatty acids are mixtures of saturated higher fatty acids; alcohols are isopropanol, n
- propanol, n-butanol, secondary butanol or isobutanol, or a mixture of two or more thereof;
and is aqueous; drying of the solution is carried out in a membrane dryer at temperatures above 80°C; mixing is carried out in a soap amalgamator; the amalgamator mixture contains the dried solution solids, fines and contains divided pigments and fragrances; the extrusion is vacuum extrusion with an exit temperature in the range of 25 to 50°C; and
3. The method of claim 2, wherein the plodder rod is cut to cake size and stamped into a cake form. 4. The proportions of higher fatty acid monoglyceride sodium sulfate, higher fatty acid sodium soap and higher fatty acid in the monoglyceride sulfate detergent composition bar are within the range of 35 to 65%, 8 to 25% and 15 to 40%, respectively: High grade. The solution of sodium fatty acid monoglyceride sulfate, sodium soap and saturated higher fatty acids is in an aqueous isopropanol solution; the isopropanol:water ratio in such solution is in the range of 2:1 to 1:2. , the total proportion of normally solid materials (monoglyceride sulfates, soaps and free fatty acids) in the solution is 4
5 to 65%, and the solution temperature before charging into the membrane dryer is in the range of 50 to 90°C; drying is carried out in a coated film dryer or coated film evaporator; The temperature at the heat transfer surface is in the range of 90 to 210°C; the composition exiting the film dryer or evaporator contains 0.2 to 5% water and is substantially free of isopropanol; The amalgam mixture is ground or refined so that the additives are compositionally well dispersed;
4. A method as claimed in claim 3, characterized in that the extrusion is carried out in a vacuum plodder. 5. The proportions of higher fatty acid monoglyceride sodium sulfate, higher fatty acid sodium soap and higher fatty acid in the monoglyceride sulfate detergent composition bar are within the range of 40 to 60%, 10 to 20% and 20 to 35%, respectively; An aqueous isopropanol solution of sodium fatty acid monoglyceride sulfate, sodium soap, and saturated higher fatty acids is prepared in an isopropanol:water ratio of 3:2.
in the range of 2:3, the total proportion of normally solid materials in such solution being in the range of 50 to 60%, and in the film dryer or film evaporator. The solution temperature before charging is in the range of 50 to 70°C;
The temperature of the heat transfer surface of the coating film dryer or evaporator is 1
5. A process according to claim 4, characterized in that the temperature is in the range 00 to 150 DEG C.; and the composition exiting the coated film dryer or evaporator contains 0.5 to 2% water. 6. The higher fatty acid monoglyceride sodium sulfate is hydrogenated coco monoglyceride sodium sulfate; the higher fatty acid sodium soap is a tallow-coronodium soap containing 80 to 90 parts of beef tallow soap and 10 to 20 parts of coco soap;
The higher fatty acid consists of a mixture of stearic acid and palmitic acid; and the detergent composition bar is made of beef tallow with a ratio of 45 to 55% sodium H-cocomoglyceride sulfate and a beef tallow soap: coco soap ratio of about 85:15. sodium soap 1
2 to 18% and triple pressed stearic acid (about 45% stearic acid and about 55% palmitic acid) 22 to 28%,
Sodium sulfate 4 to 6%, organic by-product during H-cocomoglyceride sodium sulfate production 3 to 5%, water 0.5%
1.5% to 1.5%, fragrance 0.5 to 2%, titanium dioxide 0.
6. A method according to claim 5, characterized in that it contains from 5 to 2% and the remainder (if any) is an additive for the synthetic detergent composition bar. 7. Water-soluble higher fatty acid monoglyceride sulfate,
A water-soluble higher fatty acid soap and a solvent solution of higher fatty acids are
The soap and higher fatty acids are prepared by dissolving the soap and the higher fatty acids in an aqueous lower alcohol solution of higher fatty acid monoglyceride sulfate, which is an extracted solution of higher fatty acid monoglyceride sulfate neutralized product, thereby forming a mutual solution of said components of the detergent composition bar into an aqueous lower alcohol solution. 2. Process according to claim 1, characterized in that it is obtained in an alcoholic solvent. 8. Saturated higher fatty acids and kettle soap at a temperature within the range of 60 to 90°C are dissolved in an aqueous isopropanol extractant solution of higher fatty acid monoglyceride sodium sulfate, and the higher monoglyceride sodium sulfate, sodium soap and saturated An aqueous isopropanol solution of higher fatty acids is prepared, in which the isopropanol:water ratio in the aqueous isopropanol extractant is from 2:1 to 1:
2, the total proportion of the normally solid materials (monoglyceride sulfates, soaps and fatty acids) in the aqueous isopropanol solvent is in the range 45 to 65%, and the solution temperature is 50%. A method according to claim 4, characterized in that the temperature is in the range of 90 to 90°C. 9. Stearic acid and palmitic acid and tallow-cocosodium soap in kettle soap form at a temperature range of 65-85°C are dissolved in an aqueous isopropanol extractant solution of hydrogenated sodium coco-monoglyceride sulfate (sodium coco-monoglyceride sulfate). , an aqueous isopropanol solution of hydrogenated coconut monoglyceride sodium sulfate is prepared, the isopropanol:water ratio being in the range 3:2 to 2:3, and the normally solid material (
H-cocomoglyceride sodium sulfate, beef tallow-coconodium soap, stearic acid and palmitic acid) in the aqueous isopropanol solvent in a total proportion of 50 to 6.
within the range of 0℃ and the solution temperature is 50 to 7
A method according to claim 6, characterized in that the temperature is in the range of 0°C. 10. Foaming, foaming, solubility, abrasion, sloughness, hardness, made of water-soluble higher fatty acid monoglyceride sulfate, water-soluble higher fatty acid soap and higher fatty acid, and produced by the method according to claim 1. A monoglyceride sulfate detergent composition bar with good homogeneity and tactile properties. 11. Higher fatty acid monoglyceride sodium sulfate in which the monoglyceride portion is derived from vegetable and/or animal oil and/or fat and may be partially or fully hydrogenated; vegetable and/or animal oil and/or mixtures of fats, some or all of which may be hydrogenated; and some or all of which are derived from vegetable and/or animal oils and/or fats; foaming, foaming, consisting of a mixture of saturated higher fatty acids, which may be entirely hydrogenated, and which is the product of the process of claim 3;
A higher fatty acid monoglyceride sodium sulfate detergent composition bar having good properties such as solubility, abrasion, sloughness, hardness, homogeneity and feel. 12. Higher fatty acid monoglyceride sodium sulfate, in which the monoglyceride portion may be derived from vegetable and/or animal oils and/or fats, partially or fully hydrogenated; 40 to 60%; the higher fatty acid portion may be derived from vegetable oils and/or fats; 10 to 20% higher fatty acid sodium soap, which may be derived from a mixture of natural and/or animal oils and/or fats, which may be partially or fully hydrogenated; and vegetable and/or animal oils. and/or a saturated mixture of fatty acids having 12 to 18 carbon atoms, which may be derived from fats and partially or wholly hydrogenated, and which is produced by the method according to claim 4. A monoglyceride sulfate detergent composition rod having good properties such as elasticity, foamability, solubility, abrasion, sloughness, hardness, homogeneity and feel. 13. H-cocomoglyceride sodium sulfate 45-55%, beef tallow-coco sodium soap (however, the ratio of beef tallow soap: coco soap is about 85:15) 12-18%
, triple pressed stearic acid (stearic acid content approximately 45%)
and palmitic acid content (approximately 55%) 22 to 28%, sodium sulfate 4 to 6%, organic by-products from the production of H-cocomoglyceride sodium sulfate 3 to 5%, water 0.5 to 1.5%, fragrance 0. 5 to 2%, titanium dioxide 0.5 to 2%, the remainder (if any) being an additive for a synthetic detergent composition bar, produced by the method of claim 6; A monoglyceride sulfate detergent composition bar having good properties such as foamability, solubility, abrasion, sloughness, hardness, homogeneity and feel. 14. Higher fatty acid monoglyceride sodium sulfate, in which the monoglyceride portion may be derived from vegetable and/or animal oils and/or fats, partially or fully hydrogenated; 40 to 60%; higher fatty acid portion may be derived from vegetable oils and/or fats; 10 to 20% higher fatty acid sodium soap, which may be partially or fully hydrogenated, derived from a mixture of natural and/or animal oils and/or fats; and vegetable and/or animal oils. and/or a mixture of 20 to 35% saturated fatty acids of 12 to 18 carbon atoms, which may be partially or fully hydrogenated, derived from The various ingredients are so homogeneously distributed throughout the detergent bar that no roughness on the surface of the detergent bar can be detected when the detergent bar is washed with the detergent bar.It has excellent properties such as foaming property, foamability, solubility, abrasion, sloughness, hardness, and tactile feel. monoglyceride sulfate detergent composition bar. 15, H-cocomoglyceride sodium sulfate 45 to 55%, beef tallow-coco sodium soap 12 to 18% (however, the ratio of beef tallow soap to coco soap is about 85:15)
, triple pressed stearic acid (containing about 45% stearic acid and about 55% palmitic acid) 22-28%, sodium sulfate 4-6%, organic by-product from the production of H-cocomoglyceride sodium sulfate 3-5%, Water 0.5-1.5%, fragrance 0.5-2%, titanium dioxide 0.5
15. A monoglyceride sulfate detergent composition bar according to claim 14, wherein the monoglyceride sulfate detergent composition bar contains from 2% to 2%, with the remainder (if any) being an additive for a synthetic detergent composition bar.