CN101406817A - Betaine water-bearing liquid solution having solid content of at least 40% by weight - Google Patents
Betaine water-bearing liquid solution having solid content of at least 40% by weight Download PDFInfo
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- CN101406817A CN101406817A CNA200710180930XA CN200710180930A CN101406817A CN 101406817 A CN101406817 A CN 101406817A CN A200710180930X A CNA200710180930X A CN A200710180930XA CN 200710180930 A CN200710180930 A CN 200710180930A CN 101406817 A CN101406817 A CN 101406817A
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Abstract
The invention discloses a hydrous liquid state solution of betaine expressed by a general formula(I), wherein R represents alkyl of coconut oil fatty acid, alkyl of the optimized hydrogenated coconut oil fatty acid, or alkyl of a fatty acid mixture equal to the coconut oil fatty acid on an average; wherein the solid content of the solution is at least 40 weight percent, the pH value of the solution is between 5 and 8, and the amino amide content of the solution does not exceed 1 weight percent. The solution is characterized in that the solution contains 1 to 3 weight percent of one or more saturated fatty acids with the average carbon atom number of between 8 and18, or one or more unsaturated fatty acids with the average carbon atom number of between 8 and 24 based on the solution; and the solution contains 0 to 4 weight percent of glycerin based on the solution.
Description
Technical field
The present invention relates to the betaine water-bearing liquid solution of following general formula:
Wherein R is the alkyl of coco-nut oil fatty acid, the alkyl of the coco-nut oil fatty acid of preferred hydrogenation, or by average computation, the alkyl that is equivalent to the fatty acid mixt of coco-nut oil fatty acid, this solution solid content is at least 40 weight %, pH is 5 to 8, and amino amides (aminoamide) content is not higher than 1 weight %.
More particularly, the present invention relates to solid content and be at least 42 weight %, and especially be at least the above-mentioned type betaine water-bearing liquid solution of 45 weight %.Solid content is meant: under 105 ℃, in the measured weight after 2 hours of evaporation sample on the flat glass dish.
Background technology
As everyone knows, the alkali solution of beet of the above-mentioned type only is only liquid when being lower than certain specific total solid concentration, and this specific total solid concentration depends on aliphatic acid or fatty acid mixt used when preparing them.For example, solidify when the about 40 weight % of solid content by the alkali solution of beet of coco-nut oil fatty acid preparation.Therefore, obviously, by the cocoamidopropyl aqueous solution of coconut palm fat preparation, its total solid concentration is lower than 40 weight %, and in most of the cases, is about 35 weight % on the traditional commerce.Can keep the Cmax that alkali solution of beet still flows to reduce along with the increase of carbon number.If comprise the unrighted acid of higher proportion in the fatty acid mixt, then the Cmax that can reach usually is relatively higher than the Cmax that uses saturated fatty acid to reach.
Usually, the traditional commerce alkali solution of beet is composed as follows:
On this meaning, say the whole components beyond solid content has been represented and dewatered.According to following reaction equation, can determine the stoichiometry of reacting and the betaine that produces and the ratio of sodium chloride by fatty acid amide with uncle's amino (amino amides) and sodium chloroacetate:
Usually, because incomplete reaction can leave a spot of amino amides in the product.Yet, can be by adjusting the content that stoichiometry and reaction method reduce this part amino amides.Other typical component listed above derives from the building-up process of amino amides.If by aliphatic acid and 3-N, the N-dimethylaminopropylamine reacts and prepares amino amides, remaining aliphatic acid then still can occur.If with fat and 3-N, the N-dimethylaminopropylamine is that raw material comes the synthesizing amino acid amides, then partial fatty acid and glycerine can occur.
On physiology, amino amides is harmful to, and therefore, if any, should do everything possible that it is low-level that its content is remained on, and on the other hand, glycerine and aliphatic acid are supposed to use, and use often in the preparation of cosmetics.With regard to glycerine, the main flow skin nursing products that contain it are praised highly.Aliphatic acid is favourable for compound, for example, A.L.Hunting described among " cosmetic products and cosmetics " (Cosmetics and Toiletries) 97,53 (1982) aliphatic acid as shampoo in the purposes of thickener.By their use, particularly use with the form of their salt, can produce the effect that increases viscosity.
In the reality, people are attempting to produce the alkali solution of beet with higher concentration always.Yet only when using foreign compound or utilization specific process, this trial just can be successful, and still, these measures have all increased the cost of product.
For example, United States Patent (USP) 4,243, described such poured into aqueous compositions in 549, it comprises, for example: the betaine of 33.5 weight %, 33.5 the ethoxylated alkyl sulfate of weight %, the impurity of the sodium chloride of 9 weight % and 2 to 3 weight %, all the other are water.These mixtures exist with the form of so-called G phase.The flowability of this mixture is based on the mutually specific micellar structure of G, and this specific micellar structure only just can exist a narrow relatively concentration range.Yet for the compound of many use alkali solution of beet, the existence of the anionic surfactant of weight such as needed is not expected.Even add anionic surfactant for subsequently utilization, the user also needs decision to use which anionic surfactant.Because cationic surface active agent can interact with anionic surfactant, is inappropriate so contain the mixture of cationic surface active agent.
But Deutsche Bundespatent 36 13 944 relates to a kind of flowing and the preparation method of pumping solution of 70 weight % betaines that comprise at least.The synthetic method of this betaine is:
A) ammonium salt that uses halogenated carboxylic acid is as salt,
B) carry out quaternizedly in polar organic solvent, this polar organic solvent can not comprise the water greater than 20 weight %,
C) after quaternized, azeotropic distillation goes out whole water that contained and the ammonium halide of removing precipitation, then
D) distilling off solvent partly or completely, and
E) before distillation, simultaneously or afterwards, with the employed solvent of required application or the betaine concentration adjustment in the solvent mixture of being suitable for to desired value.
The fact shows that the shortcoming of this method is to need to use solvent, and need remove the ammonium chloride of precipitation by for example filtering.In addition,,, recommend to add the preferred aliphatic glycol of 2 to 15 weight % based on solution in order to obtain desired low viscosity, and the ethanol of 0.5 to 10 weight %.Equally, that the content of this glycol and/or ethanol may not be always desirable and acceptable.
The target of Deutsche Bundespatent 37 26 322 is methods of a kind of above-mentioned betaine of synthetic concentrated aqueous solution form.If necessary, can pass through transpiring moisture, to after quaternized, obtain, the concentration adjustment of the preferred still solution of heat is to desirable value, and in this solution, add inorganic acid, before the desirable value or afterwards, make the pH of this solution be adjusted to 1 to 4.5 by in this solution, adding inorganic acid with concentration adjustment.Yet, in storage, transportation and the use of this acidity alkali solution of beet, having produced etching problem, this makes and must use acid resisting material in basin, tank car or the like.
At last, with reference to Deutsche Bundespatent 38 26 654, according to this patent, the alkali solution of beet that can obtain concentrating: before the quaterisation or afterwards in reactant mixture by such method, the non-ionic water-soluble surfactant that perhaps in resulting alkali solution of beet, adds a certain amount, make the nonionic surface active agent that contains 3 to 20 weight % in the end product, thus after quaternized, do not need by adding alkaline solution the pH value of this solution to be adjusted to 〉=5 to 9.Equally, in this scheme, alkali solution of beet comprises external nonionic surface active agent, and in using in the later stage of this alkali solution of beet, the existence of this nonionic surface active agent is not perhaps expected.
Summary of the invention
The object of the present invention is to provide a kind of aqueous liquid alkali solution of beet that does not have external surfactant and organic solvent, the total solid content of this solution is at least 40 weight %, is preferably at least 42 weight %, and particularly 45 weight %, and pH value are 5 to 8.
Another object of the present invention provides a kind of method for preparing this liquid alkali solution of beet, and this method does not need other additional step of for example filtering.
The present invention also has another purpose, a kind of alkali solution of beet that does not have admixture and impurity promptly is provided, these admixtures and impurity are owing to the incomplete reaction of employed alkali solution of beet is stayed in the alkali solution of beet, owing to physiological reason, the residual volume of these materials is unwanted, especially impurity chloroacetate salt and aliphatic acid dimethylamino-propyl acid amides (" amino amides ").
Another free-revving engine of the present invention provides such alkali solution of beet: wherein the concentration of this alkali solution of beet makes does not need to preserve this solution so that antibacterium is decomposed with special method, and particularly solid content is at least about the alkali solution of beet of 40 weight %.
Surprisingly, having been found that can be by adjusting alkali solution of beet, makes it comprise a certain amount of free fatty and optional a small amount of glycerine is realized these and other purpose.
The present invention is a kind of moisture fluent solution of following general formula betaine:
Wherein, R is the alkyl (alkyl) of coco-nut oil fatty acid, the alkyl (alkyl) of the coco-nut oil fatty acid of preferred hydrogenation, or by average computation, the alkyl (alkyl) of the fatty acid mixt suitable with coco-nut oil fatty acid, this solution solid content is at least 40 weight %, pH is 5 to 8, and amino amides content is no more than 1 weight %, based on this solution, the average carbon atom number that comprises 1 to 3 weight % is that 8 to 18 one or more saturated fatty acids or average carbon atom number are one or more unrighted acids of 8 to 24, and, based on this solution, comprise the glycerine of 0 to 4 weight %.
The specific embodiment
As average carbon atom number is 8 to 18 saturated fatty acid, preferably uses natural acid and fatty acid mixt, and especially preferably using average carbon atom number is 8 to 12 aliphatic acid and fatty acid mixt.
As average carbon atom number is 8 to 24 unrighted acid, preferably uses natural unrighted acid and their mixture, for example oleic acid, castor oil acid and the aliphatic acid that obtains from fish oil.
Especially preferably use hydrogenation and unhydrided coco-nut oil fatty acid, laurate, oleic acid and castor oil acid.
In this respect, the aliphatic acid that exists with free form can be identical with the employed aliphatic acid RCOOH of preparation betaine.
Preferably, this creative alkali solution of beet is characterised in that it contains the aliphatic acid of 1.5 to 3 weight % and the glycerine of 1 to 2 weight %.
Those skilled in the art can both understand, and coco-nut oil fatty acid is the mixture of a kind of commercial hydrogenation that provides or non-hydrogenated fatty acid, and it obtains from coconut oil and has a following average composition:
The unhydrided hydrogenation of coco-nut oil fatty acid
Carbon number weight % weight %
6 0-1 0-1
8 5-10 5-10
10 3-10 5-10
12 43-53 43-53
14 15-22 15-22
16 7-14 7-14
18 2-8 4-12
18 monounsaturated 2-12 0-1
18 2 undersaturated 0-3 0
18 triunsaturated 0-3 0
In addition, can also contain other aliphatic acid of 0 to 3 weight % in the coco-nut oil fatty acid, for example castor oil acid or erucic acid.
According to the present invention, term " coco-nut oil fatty acid " is also chosen wantonly and is comprised optionally hydrogenated palm-kernel oil aliphatic acid.
The unhydrided hydrogenation of palm-kernel oil aliphatic acid
Carbon number weight % weight %
6 0-1 0-1
8 3-6 3-6
10 3-6 3-6
12 40-52 40-52
14 14-18 14-18
16 6-14 6-14
18 1-8 10-17
18 monounsaturated 9-16 0-2
18 2 undersaturated 1-3 0
18 triunsaturated 0-1 0
Just derive from the betaine of non-hydrogenated fatty acid,, be enough to obtain alkali solution of beet desired, that concentrate usually by adjustment to free fatty acid content and pH value.If use the coco-nut oil fatty acid or the palm-kernel oil aliphatic acid of hydrogenation, then need suitably to add the glycerine that is not more than 4 weight % usually.Preferred coco-nut oil fatty acid or the palm-kernel oil aliphatic acid that uses hydrogenation.
Below for the example of alkali solution of beet of the present invention:
Betaine betaine sodium chloride free-fat glycerine viscosity
Kind acid mPas,
25 ℃ of R-COOH (% represents with weight)
Coconut oil 36.8 6.2 1.06 0.89 85
Aliphatic acid
36.0 6.6 1.55 0.94 75 of hydrogenation
Coconut oil
Aliphatic acid
Palm kernel 36.7 6.2 1.78 0 90
The grease fat
Acid
According to a further aspect in the invention, by under heating up, prepare this creative alkali solution of beet with the compound of monoxone or the quaternary ammoniated following general formula of its salt:
Wherein, R as above defines, in the method, the fatty acid amino amide that will contain the general formula I I of required free fatty amount is used for this quaterisation, perhaps before quaterisation or among the aliphatic acid of aequum is joined in the reactant mixture, and choose wantonly in this reactant mixture and add glycerine.
Usually, " reaction temperature of rising " is defined as 80 ℃ to 180 ℃ temperature.Be higher than 100 ℃ temperature if use, then this reaction must be carried out in closed reactor.The preferred temperature of using 120 ℃ to 160 ℃, because in this temperature range, the viscosity of reaction medium is low especially, and reacts carry out very fast.
Suitably select the chloroacetic amount be used to react, so that amino amides is depleted when reaction finishes, its residual volume≤1 weight %.As Deutsche Bundespatent 29 26 479 is described,, more help reducing the content of amino amides by selecting a suitable alkaline pH.
As chloroacetate salt, preferably use sodium chloroacetate.It also can be by monoxone and sodium hydroxide solution form on the spot in reactant mixture.
Randomly, before reaction end temperature is reduced to room temperature, pH is adjusted to 5 to 8 with suitable acid.Preferred pH value scope is 5 to 7, especially 5.5 to 6.5.
For the preparation of alkali solution of beet of the present invention, if use the formula II amino amides that has comprised the aequum free fatty, in most of the cases, this free aliphatic acid is identical with the aliphatic acid RCOOH of amino amides.Thereby,, can consider the content of free fatty at the compound that is used for preparing amino amides.Yet also can to use acid number be 0 or be about 0 amino amides, and in this amino amides, add average carbon atom number be 8 to 24 one or more plant saturated fatty acids.
Add glycerine if desired, then can before the quaterisation or among add.Though can add glycerine after quaterisation, this is not favourable yet.
Alkali solution of beet of the present invention has realized not having the target of external surfactant and amino amides content≤1 weight %.In these schemes, must not add antimicrobial.In addition, depend on the average chain length of the fatty acid mixt that uses and the degree of unsaturation of these aliphatic acid, alkali solution of beet of the present invention is that solid content can be up to the liquid of about 48 weight %.
Further illustrate in the embodiments of the invention following, will describe the preparation of alkali solution of beet of the present invention in more detail, should be appreciated that following illustrative embodiment of giving is to be used to explain the present invention, rather than limitation of the present invention.
Embodiment
In following embodiment, the coco-nut oil fatty acid amino amides be by, for example, different fatty raw material and 3-N, N-dimethylaminopropylamine, and the chloroacetic acid sodium of conventional marketing quality prepares.
To A4, prepared non-alkali solution of beet of the present invention in embodiment A 1.In embodiment A 1 and A2, acid number is adjusted to outside the desired scope, and except that this point, among all similar embodiment of the invention B1 to B3 of others, has obtained containing the liquid alkali solution of beet of 45% solid.Do not contain glycerine in the embodiment A 3, although must contain glycerine for the product that obtains to flow.Except that this point, the embodiment of the invention B4 similar in others illustrated this point.In non-embodiments of the invention A4, pH is not adjusted to 5 to 8.
Being characterized as of the fatty acid amino amide that uses:
Fatty acid amino amide A:
Tertiary amine nitrogen content: 4.6%
Acid number: 2.1
Glycerol content: 3.0%
Fatty acid profile: caproic acid 0.5%
Sad 6.7%
Capric acid 6.5%
Laurate 48.0%
Myristic acid 17.5%
Palmitic acid 12.0%
Stearic acid 8.9%
Oleic acid-
Linoleic acid-
Fatty acid amino amide B:
Tertiary amine nitrogen content: 4.3%
Acid number: 4.1
Glycerol content :-
Fatty acid profile: caproic acid 1.0%
Sad 7.0%
Capric acid 6.0%
Laurate 48.0%
Myristic acid 19.0%
Palmitic acid 9.0%
Stearic acid 10.0%
Oleic acid-
Linoleic acid-
Fatty acid amino amide C:
Tertiary amine nitrogen content: 4.42%
Acid number: 4.3
Glycerol content :-
Fatty acid profile: caproic acid 1.0%
Sad 7.0%
Capric acid 6.0%
Laurate 48.0%
Myristic acid 19.0%
Palmitic acid 9.0%
Stearic acid 2.0%
Oleic acid 7.0%
Linoleic acid 1.0%
Fatty acid amino amide D:
Tertiary amine nitrogen content: 4.2%
Acid number: 2.1
Glycerol content: 2.9%
Fatty acid profile: caproic acid-
Sad 7.0%
Capric acid 6.0%
Laurate 48.0%
Myristic acid 17.0%
Palmitic acid 7.0%
Stearic acid 3.0%
Oleic acid 11.0%
Linoleic acid 1.0%
Fatty acid amino amide E:
Tertiary amine nitrogen content: 4.2%
Acid number: 1.8
Glycerol content: 3.3%
Fatty acid profile: caproic acid-
Sad 3.0%
Capric acid 3.0%
Laurate 50.0%
Myristic acid 17.0%
Palmitic acid 12.0%
Stearic acid 5.0%
Oleic acid 10.0%
Linoleic acid-
Fatty acid amino amide F:
Tertiary amine nitrogen content: 4.42%
Acid number: 4.3
Glycerol content: 2.9%
Fatty acid profile: caproic acid 1.0%
Sad 7.0%
Capric acid 12.0%
Laurate 40.0%
Myristic acid 19.0%
Palmitic acid 12.0%
Stearic acid 9.0%
Oleic acid-
Linoleic acid-
Fatty acid amino amide G:
Tertiary amine nitrogen content: 4.6%
Acid number: 18
Glycerol content :-
Fatty acid profile: caproic acid 1.0%
Sad 7.0%
Capric acid 6.0%
Laurate 48.0%
Myristic acid 19.0%
Palmitic acid 9.0%
Stearic acid 2.0%
Oleic acid 7.0%
Linoleic acid 1.0%
A) non-embodiments of the invention
Embodiment A 1
With coco-nut oil fatty acid amino amides A (305g) and 1.1g acid number is that 290 coco-nut oil fatty acid mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 3; In laurate, this is equivalent to 0.36% aliphatic acid.This mixture is joined in the solution of 131g 98% chloroacetic acid sodium (1.1 moles) in 534g water, and be heated with stirring to 98 ℃.During reaction, by adding several (about 1.5mL) 40%NaOH the pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduced, the aqueous hydrochloric acid solution with 10% was adjusted to 6 with the pH value.Thus, formed the non-current product of a kind of glue, it is characterized by following numerical value:
Solid content: 45%
Betaine: 37.2%
NaCl： 6.7％
Aliphatic acid: 0.1%
Glycerine: 0.97%
Amino amides:＜0.3%
PH： 6.0
Embodiment A 2
With coco-nut oil fatty acid amino amides A (305g) and 39g acid number is that 290 coco-nut oil fatty acid mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 35; In laurate, this is equivalent to 11.3% aliphatic acid.This mixture is joined in the solution of 131g 98% chloroacetic acid sodium (1.1 moles) in 581g water, and be heated with stirring to 98 ℃.During reaction, by adding several (about 1.5mL) 40%NaOH the pH value is maintained between 8 and 9.Between this stage of reaction, the viscosity of reactant mixture improves widely and stirs very difficult.Stop reaction after 8 hours.Before temperature reduced, the aqueous hydrochloric acid solution with 10% was adjusted to 6 with the pH value.Thus, formed the non-current product of a kind of muddiness, thickness, pasty state, it is characterized by following numerical value:
Solid content: 45%
Betaine: 34.1%
NaCl： 6.2％
Aliphatic acid: 3.8%
Glycerine: 0.98%
Amino amides: 0.5%
PH： 6.0
Embodiment A 3
With coco-nut oil fatty acid amino amides B (326g) and 16.7g acid number is that 290 laurate mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 18; In laurate, this is equivalent to 4.9% aliphatic acid.This mixture is joined in the solution of 131g98% chloroacetic acid sodium (1.1 moles) in 579g water, and be heated with stirring to 98 ℃.During reaction, by adding several (about 1.5mL) 40%NaOH the pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduced, the aqueous hydrochloric acid solution with 10% was adjusted to 6 with the pH value.Thus, formed the non-current product of a kind of gel, it is characterized by following numerical value:
Solid content: 45%
Betaine: 36.7%
NaCl： 6.2％
Aliphatic acid: 1.56%
Glycerine :-
Amino amides:＜0.3%
PH： 6.0
Embodiment A 4
With coco-nut oil fatty acid amino amides A (305g) and 17.5g acid number is that 290 laurate mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 18; In laurate, this is equivalent to 5.4% aliphatic acid.This mixture is joined in the solution of 131g98% chloroacetic acid sodium (1.1 moles) in 554g water, and be heated with stirring to 120 ℃.During reaction, by adding several (about 1.5mL) 40%NaOH the pH value is maintained between 8 and 9.Stop reaction after 8 hours.Subsequently, do not add acid and change change pH values.Thus, formed a kind of solid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 35.2%
NaCl： 6.5％
Aliphatic acid: 1.78%
Glycerine: 1.0%
Amino amides:＜0.3%
PH： 8.6
B) embodiments of the invention
Embodiment B 1
With coco-nut oil fatty acid amino amides A (305g) and 11g acid number is that 290 coco-nut oil fatty acid mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 12; In laurate, this is equivalent to 3.8% aliphatic acid.This mixture is joined in the solution of 131g98% chloroacetic acid sodium (1.1 moles) in 546g water, and be heated with stirring to 98 ℃.By adding several (about 1.5mL) 40%NaOH reaction pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduces, the pH value is adjusted to 5.5 with hydrochloric acid.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 36%
NaCl： 6.6％
Aliphatic acid: 1.1%
Glycerine: 0.94%
Amino amides:＜0.3%
PH： 5.5
Viscosity: 90mPas
Embodiment B 2
With coco-nut oil fatty acid amino amides A (305g) and 17.5g acid number is that 290 coco-nut oil fatty acid mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 18; In laurate, this is equivalent to 5.7% aliphatic acid.This mixture is joined in the solution of 131g 98% chloroacetic acid sodium (1.1 moles) in 554g water, and be heated with stirring to 98 ℃.By adding several (about 1.5mL) 40%NaOH this reaction pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduces, the pH value is adjusted to 5 with 10% aqueous hydrochloric acid solution.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 35.8%
NaCl： 6.5％
Aliphatic acid: 1.8%
Glycerine: 0.93%
Amino amides:＜0.3%
PH： 5.0
Viscosity: 90mPas
Embodiment B 3
With coco-nut oil fatty acid amino amides A (305g) and 29g acid number is that 290 coco-nut oil fatty acid mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 27; In laurate, this is equivalent to 8.7% aliphatic acid.This mixture is joined in the solution of 131g98% chloroacetic acid sodium (1.1 moles) in 568g water, and be heated with stirring to 98 ℃.By adding several (about 1.5mL) 40%NaOH this reaction pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduced, the aqueous hydrochloric acid solution with 10% was adjusted to 6 with the pH value.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 34.5%
NaCl： 6.3％
Aliphatic acid: 2.9%
Glycerine: 0.9%
Amino amides:＜0.3%
PH： 6.0
Viscosity: 110mPas
Embodiment B 4
With coco-nut oil fatty acid amino amides B (326g) and 17.5g acid number is that 290 coco-nut oil fatty acid and 10.6g glycerine mix.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid and glycerine is 18, in laurate, is equivalent to 5.4% aliphatic acid, and glycerol content is 3%.This mixture is joined in the solution of 131g 98% chloroacetic acid sodium (1.1 moles) in 593g water, and be heated with stirring to 98 ℃.Stop reaction after 8 hours.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 35.5%
NaCl： 6.1％
Aliphatic acid: 1.78%
Glycerine: 0.93%
Amino amides: 0.7%
PH： 5.5
Viscosity: 85mPas
Embodiment B 5
With coco-nut oil fatty acid amino amides A (305g) and 17.5g acid number is that 290 laurate mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 18; In laurate, this is equivalent to 5.4% aliphatic acid.This mixture is joined in the solution of 143g98% chloroacetic acid sodium (1.2 moles) in 569g water, and in autoclave, be stirred and heated to 140 ℃, make pressure rise to 3.5bar.It is favourable carrying out this reaction under heating up, because under such reaction temperature, has reduced the viscosity of reaction medium, and has shortened the reaction time.Stop reaction after 4 hours.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 34.6%
NaCl： 6.9％
Aliphatic acid: 1.78%
Glycerine: 0.93%
Amino amides: 0.5%
PH： 5.3
Viscosity: 90mPas
Embodiment B 6
With coco-nut oil fatty acid amino amides C (317g) and 17.1g acid number is that 278 non-hydrogenation coco-nut oil fatty acid mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 18; In laurate, this is equivalent to 5.2 aliphatic acid.This mixture is joined in the solution of 131g 98% chloroacetic acid sodium (1.1 moles) in 504g water, and be heated with stirring to 98 ℃.By adding several (about 1.5mL) 40%NaOH this reaction pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduces, the pH value is adjusted to 5.5 with several hydrochloric acid.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 48%
Betaine: 39%
NaCl： 6.7％
Aliphatic acid: 1.8%
Glycerine :-
Amino amides: 0.5%
PH： 5.5
Viscosity: 120mPas
Embodiment B 7
With coco-nut oil fatty acid amino amides D (333g) and 11g acid number is that 290 laurate mixes.The acid number of resulting coco-nut oil fatty acid amino amides and fatty acid mixt is 12; In laurate, this is equivalent to 3.2% aliphatic acid.This mixture is joined in the solution of 131g 98% chloroacetic acid sodium (1.1 moles) in 581g water, and be heated with stirring to 98 ℃.By adding several (about 1.5mL) 40%NaOH this reaction pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduces, the pH value is adjusted to 7.5 with several 10% hydrochloric acid.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 36.8%
NaCl： 6.2％
Aliphatic acid: 1.06%
Glycerine: 0.89%
Amino amides:＜0.3%
PH： 7.5
Viscosity: 75mPas
Embodiment B 8
Coco-nut oil fatty acid amino amides B (326g) is mixed with 10.9g glycerine; This is equivalent to 3.2% glycerol content.This mixture is joined in the solution of 131g 98% chloroacetic acid sodium (1.1 moles) in 646g water, and be heated with stirring to 98 ℃.By adding several (about 1.5mL) 40%NaOH this reaction pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduces, the pH value is adjusted to 7 with several 10% hydrochloric acid.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 42%
Betaine: 33.3%
NaCl： 5.9％
Aliphatic acid: 1.8%
Glycerine: 1.0%
Amino amides:＜0.3%
PH： 7.0
Viscosity: 75mPas
Embodiment B 9
With coco-nut oil fatty acid amino amides E (317g) and 24.3g acid number is that 200 oleic acid mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 18; In laurate, this is equivalent to 7.1% aliphatic acid.This mixture is joined in the solution of 131g98% chloroacetic acid sodium (1.1 moles) in 577g water, and be heated with stirring to 98 ℃.Stop reaction after 8 hours.Thus, formed a kind of liquid product of clarification, the pH value of this product is 7.5, and it is characterized by following numerical value:
Solid content: 45%
Betaine: 36.7%
NaCl： 6.2％
Aliphatic acid: 1.78%
Glycerine :-
Amino amides: 0.3%
PH： 7.5
Viscosity: 90mPas
Embodiment B 10
With coco-nut oil fatty acid amino amides F (316g) and 16.5g acid number is that 290 laurate mixes.The acid number of the mixture of resulting coco-nut oil fatty acid amino amides and aliphatic acid is 18; In laurate, this is equivalent to 5.4% aliphatic acid.This mixture is joined in the solution of 131g98% chloroacetic acid sodium (1.1 moles) in 567g water, and be heated with stirring to 98 ℃.During reaction, by adding several (about 1.5mL) 40%NaOH the pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduces, the pH value is adjusted to 5.5 with hydrochloric acid.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 36.7%
NaCl： 6.3％
Aliphatic acid: 1.1%
Glycerine: 0.94%
Amino amides:＜0.3%
PH： 5.5
Viscosity: 85mPas
Embodiment B 11
Coco-nut oil fatty acid amino amides G (329g) is joined in the solution of 131g 98% chloroacetic acid sodium (1.1 moles) in 562g water, and be stirred and heated to 98 ℃.During reaction, by adding several (about 1.5mL) 40%NaOH the pH value is maintained between 8 and 9.Stop reaction after 8 hours.Before temperature reduced, the aqueous hydrochloric acid solution with 10% was adjusted to 6 with the pH value.Thus, formed a kind of liquid product of clarification, it is characterized by following numerical value:
Solid content: 45%
Betaine: 36.4%
NaCl： 6.4％
Aliphatic acid: 1.78%
Glycerine: 0.97%
Amino amides: 0.4%
PH： 6.0
Viscosity: 95mPas
C) anticorrosion carrying capacity test
Embodiment C
" Praxis der Sterilisation; Desinfektion; Konservierung; Keimidentifizierung; Betriebshygiene " (" sterilization, sterilization, preservation, microbial identification and factory hygiene are put into practice ") third edition according to Karl Heinz Mallhaeusser, Georg Thieme publishes, the Stuttgart, 1984, the 336th page and subsequent content, to implementing the alkali solution of beet of B7 preparation, and solid content is that 40% and 35% water dilution carries out microbial load test (anticorrosion carrying capacity test).These samples (10mL) are separately by about 105 microorganisms of the following type of inoculation:
Staphylococcus aureus
Escherichia coli
Pseudomonas aeruginosa
Candida albicans
Aspergillus niger
Candida lipolytica
After 1,24 and 72 hour and 7 days, measure bacterial number.Resulting result is summarised in the following form.
Table 1-solid content is 35% alkali solution of beet
The bacterial population of microorganism after the following time of test
1 hour 24 hours 72 hours 7 days
Staphylococcus aureus 1.4 * 10
3＜10＜10＜10
Escherichia coli 1.4 * 10
51.5 * 10
4＜10＜10
Pseudomonas aeruginosa 2.6 * 10
41.0 * 10
21.0 * 10
1＜10
Candida albicans 1.0 * 10
11.0 * 10
1＜10＜10
Aspergillus niger 2.0 * 10
51.0 * 10
57.0 * 10
32.0 * 10
3
Candida lipolytica 1.1 * 10
52.9 * 10
43.8 * 10
33.9 * 10
3
Table 2-solid content is 40% alkali solution of beet
The bacterial population of microorganism after the following time of test
1 hour 24 hours 72 hours 7 days
Staphylococcus aureus 2.7 * 10
3＜10＜10＜10
Escherichia coli 4.9 * 10
42.3 * 10
3＜10＜10
Pseudomonas aeruginosa 1.3 * 10
43.0 * 10
2＜10＜10
Candida albicans 1.0 * 10
1＜10＜10＜10
Aspergillus niger 1.7 * 10
51.2 * 10
51.2 * 10
31.0 * 10
2
Candida lipolytica 1.2 * 10
52.2 * 10
42.0 * 10
35.0 * 10
1
Table 3-solid content is 45% alkali solution of beet
The bacterial population of microorganism after the following time of test
1 hour 24 hours 72 hours 7 days
Staphylococcus aureus 1.0 * 10
2＜10＜10＜10
Escherichia coli 4.1 * 10
4＜10＜10＜10
Pseudomonas aeruginosa 8.0 * 10
34.0 * 10
1＜10＜10
Candida albicans＜10＜10＜10＜10
Aspergillus niger 2.3 * 10
51.7 * 10
52.0 * 10
21.0 * 10
1
Candida lipolytica 4.3 * 10
42.2 * 10
3＜10＜10
According to Wallhaeusser, " if in the time that was less than for three weeks, the bacterium that is inoculated is reduced to and is lower than every milliliter of 100 microorganisms " thinks that then antisepsis is enough.Solid content is that 45% alkali solution of beet has reached this requirement best.Solid content is that 40% alkali solution of beet still can satisfy this requirement, does not demonstrate enough microorganism resistances but solid content is 35% alkali solution of beet.
Claims (11)
1. water-bearing liquid solution with betaine of following general formula:
Wherein R be coco-nut oil fatty acid alkyl, hydrogenation coco-nut oil fatty acid alkyl or by average computation, the alkyl of the fatty acid mixt suitable with coco-nut oil fatty acid, wherein, the solid content of this solution is at least 40 weight %, pH is 5 to 8, and amino amides content is no more than 1 weight %, and based on this solution, the average carbon atom number that comprises at least 1 to 3 weight % is that 8 to 18 one or more saturated fatty acids or average carbon atom number are one or more unrighted acids of 8 to 24, and, comprise the glycerine of 0 to 4 weight % based on this solution.
2. alkali solution of beet as claimed in claim 1, it comprises the described saturated or unrighted acid of 1.5 to 3 weight %.
3. alkali solution of beet as claimed in claim 1, its compound that comprises formula RCOOH is as described saturated or unrighted acid, and wherein R as above defines.
4. alkali solution of beet as claimed in claim 2, its compound that comprises formula RCOOH is as described saturated or unrighted acid, and wherein R as above defines.
5. alkali solution of beet as claimed in claim 1, its comprise be selected from laurate, oleic acid, castor oil acid, coco-nut oil fatty acid and hydrogenated coconut fatty acid oil compound as described saturated or unrighted acid.
6. alkali solution of beet as claimed in claim 2, its comprise be selected from laurate, oleic acid, castor oil acid, coco-nut oil fatty acid and hydrogenated coconut fatty acid oil compound as described saturated or unrighted acid.
7. alkali solution of beet as claimed in claim 1, it comprises the glycerine of 1 to 2 weight %.
8. alkali solution of beet as claimed in claim 2, it comprises the glycerine of 1 to 2 weight %.
9. alkali solution of beet as claimed in claim 3, it comprises the glycerine of 1 to 2 weight %.
10. alkali solution of beet as claimed in claim 4, it comprises the glycerine of 1 to 2 weight %.
11. one kind is used to prepare the method for alkali solution of beet according to claim 1, it comprises: under heating up, use the compound of monoxone or the quaternized following formula of its salt:
Wherein R as above defines,
For this quaterisation, wherein, the fatty acid amino amide of use formula II, its described saturated or unrighted acid that contains aequum is as free fatty, perhaps before this quaterisation or among, the described saturated or unrighted acid of aequum is joined in the reactant mixture, and randomly, in this reactant mixture, add glycerine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710180930XA CN101406817A (en) | 2007-10-09 | 2007-10-09 | Betaine water-bearing liquid solution having solid content of at least 40% by weight |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710180930XA CN101406817A (en) | 2007-10-09 | 2007-10-09 | Betaine water-bearing liquid solution having solid content of at least 40% by weight |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101406817A true CN101406817A (en) | 2009-04-15 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200710180930XA Pending CN101406817A (en) | 2007-10-09 | 2007-10-09 | Betaine water-bearing liquid solution having solid content of at least 40% by weight |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106619232A (en) * | 2017-02-13 | 2017-05-10 | 武汉中博绿亚生物科技有限公司 | Infantile frothy leave-on hand sanitizer containing edible sterilizing components and preparation method thereof |
| US11214763B2 (en) | 2018-01-26 | 2022-01-04 | Ecolab Usa Inc. | Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a carrier |
| US11377628B2 (en) | 2018-01-26 | 2022-07-05 | Ecolab Usa Inc. | Solidifying liquid anionic surfactants |
| US11655436B2 (en) | 2018-01-26 | 2023-05-23 | Ecolab Usa Inc. | Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a binder and optional carrier |
-
2007
- 2007-10-09 CN CNA200710180930XA patent/CN101406817A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106619232A (en) * | 2017-02-13 | 2017-05-10 | 武汉中博绿亚生物科技有限公司 | Infantile frothy leave-on hand sanitizer containing edible sterilizing components and preparation method thereof |
| US11214763B2 (en) | 2018-01-26 | 2022-01-04 | Ecolab Usa Inc. | Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a carrier |
| US11377628B2 (en) | 2018-01-26 | 2022-07-05 | Ecolab Usa Inc. | Solidifying liquid anionic surfactants |
| US11655436B2 (en) | 2018-01-26 | 2023-05-23 | Ecolab Usa Inc. | Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a binder and optional carrier |
| US11834628B2 (en) | 2018-01-26 | 2023-12-05 | Ecolab Usa Inc. | Solidifying liquid anionic surfactants |
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