JP3414493B2 - Hairdressing base - Google Patents

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a base for hair styling agents. More specifically, it has excellent affinity with hair, has a strong setting power under high humidity, has excellent detergency despite little flaking, and has little deterioration in these physical properties even when an anionic electrolyte is added. The present invention relates to a base for hairdressing agents.

[0002]

2. Description of the Related Art Bases for hair styling agents are used for fixing and maintaining hair in any desired hairstyle. Among them, vinyl acetate or dimethylaminoethyl methacrylate and vinylpyrrolidone are partially or completely quaternary. Modified copolymers are widely used.

However, such a hair styling agent base absorbs water at high humidity and develops adhesiveness, which causes problems such as sticky hair and weak setting power at high humidity. There was a point.

A polymer disclosed in Japanese Patent Laid-Open No. 21263/1992 is known as a base for a hairdressing agent that solves the above problems. However, the polymer has a compatibility with liquefied petroleum gas and a setting force. Although excellent, it is not satisfactory in terms of stiffness, squeaky feeling and detergency. Further, as a base for a hair styling agent that solves the above-mentioned problems, Japanese Patent Application Laid-Open No. HEI 2
The cationic polymer disclosed in JP-A-180911 is also known. The polymer is an excellent polymer that does not have a stiff or squeaky feel, has a smooth feel, and has moisture resistance and detergency, but is used after neutralizing the amino group of the polymer side chain with an organic acid or an inorganic acid. Therefore, if an anionic electrolyte or an amine compound is added, it may become unstable in the state of an aqueous solution and may be aggregated and deposited.Therefore, in the case of aqueous formulations such as set lotion, gel, mist spray, and mousse, It may not be possible to apply it uniformly.

[0005]

DISCLOSURE OF THE INVENTION The present invention has been made in view of the above-mentioned prior art, and is excellent in compatibility with water and a hydrophilic solvent, excellent affinity for hair, and glossiness, and It is an object to provide a base for a hair styling agent which has a strong setting power under high humidity.

[0006]

That is, the present invention has the general formula (I):

[0007]

[Chemical 4]

(In the formula, X is an imino group or an oxygen atom, R is
¹ is a hydrogen atom or a methyl group, R ² is an alkylene group having 1 to 3 carbon atoms, and R ³ , R ⁴ , R ⁵ and R ⁶ are each independently a methyl group or an ethyl group) (meta) 15-40% by weight of acrylic monomer (A),
General formula (II):

[0009]

[Chemical 5]

(Wherein R ¹ is a hydrogen atom or a methyl group,
R ⁷ represents an alkyl group having 2 to 8 carbon atoms) (meth) acrylamide derivative monomer (B) 25 to 5
5% by weight and general formula (III):

[0011]

[Chemical 6]

(Wherein R ¹ is a hydrogen atom or a methyl group,
R ⁸ represents an alkyl group having 1 to 18 carbon atoms) (meth) acrylic acid alkyl ester monomer (C)
The present invention relates to a hair styling base material obtained by polymerizing a monomer component containing 5 to 60% by weight.

[0013]

Actions and Examples As described above, the base of the present invention for the hairdressing composition has the general formula (I):

[0014]

[Chemical 7]

(Wherein X is an imino group or an oxygen atom, R is
¹ is a hydrogen atom or a methyl group, R ² is an alkylene group having 1 to 3 carbon atoms, and R ³ , R ⁴ , R ⁵ and R ⁶ are each independently a methyl group or an ethyl group) (meta) 15-40% by weight of acrylic monomer (A),
General formula (II):

[0016]

[Chemical 8]

(Wherein R ¹ is a hydrogen atom or a methyl group,
R ⁷ represents an alkyl group having 2 to 8 carbon atoms) (meth) acrylamide derivative monomer (B) 25 to 5
5% by weight and general formula (III):

[0018]

[Chemical 9]

(Wherein R ¹ is a hydrogen atom or a methyl group,
R ⁸ represents an alkyl group having 1 to 18 carbon atoms) (meth) acrylic acid alkyl ester monomer (C)
It is obtained by polymerizing a monomer component containing 5 to 60% by weight.

A major feature of the present invention is that the (meth) acrylic monomer (A) represented by the general formula (I) (hereinafter referred to as the monomer (A)) is used. The base for hairdressing preparation obtained by using is a water-soluble base, has a high affinity for hair, and has no flaking, and is therefore an effective component for the base for hairdressing preparation.

Specific examples of the monomer (A) include N- (meth) acryloxyethyl-N-ethyl-
N, N-dimethylammonium ethyl sulfate, N
-(Meth) acryloxyethyl-N, N, N-trimethylammoniummethylsulfate, N- (meth) acryloxyethyl-N, N, N-triethylammoniumethylsulfate, N- (meth) acryloxyethyl-N, N-diethyl-N-methylammonium methylsulfate, N- (meth) acryloxypropyl-N-
Ethyl-N, N-dimethylammonium ethyl sulfate, N- (meth) acryloxypropyl-N, N, N
-Trimethylammonium methyl sulfate, N-
(Meth) acrylamidopropyl-N-ethyl-N, N
-Dimethylammoniumethylsulfate, N- (meth) acrylamidopropyl-N, N, N-trimethylammoniummethylsulfate and the like can be mentioned, and these can be used alone or in admixture of two or more.

The amount of the monomer (A) used is 15% by weight or more, preferably 17% by weight or more, more preferably 20% by weight or more, based on the monomer component used for the polymerization. If such usage is too low,
The film formed of the obtained hair styling base material exhibits poor water solubility, and the cleaning property tends to decrease. The amount of the monomer (A) used is 40% by weight or less, preferably 35% by weight or less, and more preferably 30% by weight or less, based on the monomer components used for the polymerization. If the amount used is too large, the obtained hair styling agent base material tends to have high hygroscopicity, resulting in stickiness and weak setting force.

Another feature of the present invention is that the (meth) acrylamide derivative monomer (B) represented by the general formula (II) (hereinafter referred to as the monomer (B)) is used. The film formed on the hair with the base for hair styling obtained by using B) has appropriate hardness and moisture resistance, has a high affinity for hair, has no flaking, and has a natural luster and high humidity. Since it has a strong setting power in, it is an effective ingredient for the base for hairdressing preparation.

In the above general formula (II), R ⁷ is an alkyl group having 2 to 8 carbon atoms. When the alkyl group has 1 carbon atom, it is formed on the hair by the base for hair styling agent. The moisture resistance of the film is reduced, and it becomes sticky.
There is a tendency for the setting power to drop under high humidity. Further, when the number of carbon atoms exceeds 8, the film formed on the hair by the base for hairdressing agent exhibits poor water solubility,
It becomes difficult to wash and remove hair.

Specific examples of the monomer (B) include N-ethylacrylamide, N-ethylmethacrylamide, Nn-butylacrylamide, Nn-butylmethacrylamide, Nt-butylacrylamide, N-. Examples thereof include t-butyl methacrylamide, Nn-octyl acrylamide, Nn-octyl methacrylamide, Nt-octyl acrylamide, and Nt-octyl methacrylamide, and these components may be used alone or in combination of two or more. Used as a mixture.

The amount of the above-mentioned monomer (B) used is 25% by weight or more based on the monomer components used for the polymerization, and 2
It is preferably 7% by weight or more, more preferably 30% by weight or more. If the amount used is too small, the hardness and moisture resistance of the film formed from the obtained hair styling base will deteriorate, and the setting force under high humidity will tend to be weak or sticky. is there. Further, the monomer (B)
The amount used is 5 with respect to the monomer component used for the polymerization.
The amount is 5% by weight or less, preferably 53% by weight or less, and more preferably 50% by weight or less. If the amount used is too large, the film formed on the hair by the obtained hair styling base material exhibits poor water solubility, and it tends to be difficult to remove the film by washing the hair.

In the present invention, the (meth) acrylic acid alkyl ester monomer (C) represented by the general formula (III) (hereinafter referred to as the monomer (C)) is used as a monomer component. The film formed on the hair by the base for hair styling agent obtained by using the monomer (C) exhibits water resistance and flexibility.

In the above-mentioned general formula (III), R ⁸ is an alkyl group having 1 to 18 carbon atoms. When the alkyl group has more than 18 carbon atoms, it is formed from the obtained hair styling base material. The resulting film tends to be poorly water-soluble, which makes it difficult to wash hair and remove unwanted side reactions such as transesterification when alcohols are used as a hydrophilic solvent during copolymerization. Easier to do.

Specific examples of the monomer (C) include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate and t-butyl. (Meth) acrylate, hexyl (meth) acrylate, octyl (meth) acrylate, 2
-Ethylhexyl (meth) acrylate, lauryl (meth) acrylate, tridecyl (meth) acrylate,
Examples include cetyl (meth) acrylate and stearyl (meth) acrylate. These components may be used alone or in admixture of two or more.

The amount of the above-mentioned monomer (C) used is 5% by weight or more, preferably 12% by weight or more, more preferably 20% by weight or more, based on the monomer components used for the polymerization. If the amount used is too small, the flexibility and water resistance of the film formed from the obtained hairdressing base will decrease, and the setting force will become weak under high humidity or flaking will occur. There is a tendency to The amount of the monomer (C) used is 60% by weight or less based on the monomer components used for the polymerization,
It is preferably not more than 50% by weight, more preferably not more than 50% by weight. If the amount used is too large, the film formed from the obtained hair styling base material exhibits poor water solubility and tends to aggregate and precipitate in an aqueous formulation such as mist or gel.

In the present invention, in order to change the feel and feel of the film formed by the obtained hair styling base, and when used in the form of an aerosol, a propellant for an aerosol or a hydrophilic solvent used for an aerosol. An ethylenically unsaturated monomer (D) (hereinafter referred to as a monomer (D)) may be used, if necessary, in order to further improve the compatibility with.

Specific examples of the monomer (D) include (meth) acrylic acid, maleic acid, itaconic acid,
Hydroxyethyl (meth) acrylate, hydroxypropyl (meth) acrylate, hydroxybutyl (meth) acrylate, methoxyethyl (meth) acrylate, ethoxyethyl (meth) acrylate, polyethylene glycol mono (meth) acrylate, methoxy polyethylene glycol mono (meth) Examples thereof include acrylate, polypropylene glycol mono (meth) acrylate, methoxy polypropylene glycol mono (meth) acrylate, vinylpyrrolidone, (meth) acrylamide, diacetone acrylamide, vinyl acetate and styrene. These components may be used alone or in admixture of two or more.

The amount of the monomer (D) used is 1% by weight or more, preferably 3% by weight or more, and more preferably 5% by weight or more, based on the monomer component used for the polymerization. If the amount used is too small, it becomes difficult to change the obtained hair styling base material to a desired texture and feel. The amount of the monomer (D) used is 30% by weight or less, preferably 25% by weight or less, and more preferably 2% by weight based on the monomer components used for the polymerization.
It is 0% by weight or less. If the amount used is too large, the resulting hair styling base material may be impaired in physical properties such as setting power under high humidity, moisture resistance and water resistance.

The hair styling base material of the present invention is prepared by adjusting the desired amount of the above-mentioned monomers (A) to (C) and, if necessary, the monomer (D), and copolymerizing in a hydrophilic solvent. available.

The hydrophilic solvent as used herein means an organic solvent having a solubility in water of 10 g / 100 g of water (25 ° C.) or more. Specific examples of the hydrophilic solvent include aliphatic 1-4 hydric alcohols having 1 to 4 carbon atoms, ethyl cellosolve, butyl cellosolve, dioxane, methyl acetate, dimethylformamide, tetrahydrofuran and the like. Group 1 to dihydric alcohols are particularly preferable for handling as a cosmetic raw material.

Specific examples of the aliphatic monohydric alcohol include methanol, ethanol, n-propyl alcohol, isopropyl alcohol, n-butyl alcohol, s-butyl alcohol and t-butyl alcohol. Specific examples of the aliphatic dihydric alcohol include ethylene glycol, propylene glycol, diethylene glycol and the like. Specific examples of the aliphatic trihydric alcohol include glycerin and trimethylolpropane. Specific examples of the aliphatic tetrahydric alcohol include pentaerythritol and the like.

Further, since the hair styling base material of the present invention may adhere to the skin of the human body, in consideration of such safety, among the hydrophilic solvents, ethanol, isopropyl alcohol and n-butyl are used. Alcohol is particularly preferred.

The above-mentioned polymerization is carried out by the above-mentioned monomers (A) to (C).
And, if necessary, a monomer component consisting of the monomer (D) is dissolved in the hydrophilic solvent, and a polymerization initiator is added,
For example, it is performed by stirring while heating in an inert gas atmosphere such as nitrogen gas.

The polymerization initiator is not particularly limited as long as it is generally used, and specific examples thereof include benzoyl peroxide, lauroyl peroxide, di-t-butyl peroxide and t-.
Butyl cumyl peroxide, t-butyl peroxyneodecanate, t-hexyl peroxyneodecanate, t-butyl peroxyisopropyl carbonate and other peroxides, azobisisobutyronitrile, azobisdimethylvaleronitrile, dimethyl Examples thereof include azo compounds such as azobisisobutyrate and azobis-2-methylbutyronitrile.

In the polymerization, it is preferable to adjust the hydrophilic solvent so that the concentration of all the monomer components used in the copolymerization is about 30 to 70% by weight. When the concentration of the monomer component exceeds 50% by weight, it is preferable to divide the monomer component and perform the polymerization while gradually adding it to avoid a sudden heat of polymerization and to perform the polymerization safely. It is preferable to carry out.

The polymerization temperature cannot be unconditionally determined because it depends on the type of polymerization initiator used, etc., but it is usually preferable to set it as the 10-hour half-life temperature of the polymerization initiator, especially the reflux temperature of the hydrophilic solvent used. It is preferable that they are close to each other, because highly reproducible polymerization can be carried out.

Polymerization time is 8 hours or more, especially 12
~ 36 hours is preferred. If it is less than 8 hours,
Polymerization may be incomplete and unreacted monomers may remain.

Whether or not the residual monomer is present is determined by
This can be confirmed by confirming whether or not the double bond exists by a general method such as the PSDB method.

The thus obtained base for hair styling agent of the present invention can be used as a hair styling agent in the state of a polymer solution or in the state of removing the solvent.

When the hair styling agent base of the present invention is used as an aerosol, for example, the hair styling agent base is dissolved in the hydrophilic solvent used as a polymerization solvent, and an aerosol such as natural gas or dimethyl ether is used. A propellant for injection, other additives, auxiliary agents, etc. may be pressurized and filled in the aerosol container and sealed. In this case, it is desirable that the blending ratio of various components to be filled in the aerosol container is usually adjusted appropriately according to the intended use.

Next, the hair styling base material of the present invention will be explained in more detail based on examples, but the present invention is not limited to such examples.

Example 1 A five-necked flask equipped with a reflux condenser, a dropping funnel, a thermometer, a nitrogen introducing tube, and a stirring device was used, and an N concentration of 85% by weight was obtained.
-Acryloxyethyl-N-ethyl-N, N-dimethylammonium ethyl sulfate ethanol solution 2
9.4 parts (parts by weight, the same applies hereinafter), 40 parts of t-butyl acrylamide, 35 parts of ethyl acrylate and 95.6 parts of absolute ethanol were added and heated to 80 ° C. in a nitrogen stream while stirring. When reflux started, 0.1 part of 2,2'-azobisisobutyronitrile was added to initiate polymerization. After 6 hours, 0.1 part of 2,2'-azobisisobutyronitrile was added, and the reaction was completed by further polymerizing for 12 hours.

The obtained hairdressing base was an ethanol solution having a concentration of 50% by weight, and the viscosity average molecular weight of the hairdressing base was 65,000.

Next, the physical properties, water solubility and compatibility with ethanol of the obtained hair styling base material were examined based on the following methods. The results are shown in Table 1.

(A) Appearance An ethanol solution containing 30% by weight of the obtained hair styling base was prepared, and the appearance (color tone) was visually observed.

(B) Water-soluble An ethanol solution containing 30% by weight of the obtained hair styling base was prepared, and water was added while maintaining the liquid temperature at 25 ° C.,
Water solubility was evaluated based on the following evaluation criteria.

(Evaluation criteria) ○: Infinitely diluted. X: Polymer is aggregated and precipitated when water is added.

(C) Stability of aqueous solution An aqueous solution was prepared by adding 20 g of water to 10 g of an ethanol solution containing 30% by weight of the obtained hairdressing base. 5 g of an aqueous solution containing 10% by weight of triethanolamine was added to the aqueous solution, and the state of the aqueous solution was evaluated based on the following evaluation criteria.

(Evaluation criteria) ◯: No change is observed in the aqueous solution. Δ: Turbidity occurs in the aqueous solution. X: Polymer is precipitated.

(D) An ethanol solution containing 10% by weight of a hair styling base material compatible with ethanol was prepared, the liquid temperature was kept at 10 to 20 ° C., and the state of the ethanol solution was evaluated as follows. It evaluated based on the standard.

(Evaluation criteria) ◯: No change is recognized. Δ: Turbidity occurs. X: The polymer aggregates and precipitates.

[0057]

[Table 1]

Examples 2 to 20 and Comparative Example 1 In Example 1, the blended monomer component and the amount used
In the same manner as in Example 1 except that is changed as shown in Table 2.
As a result, a base for hairdressing agent was obtained. However, in Comparative Example 2,
50 weight of lactic acid to the ethanol solution of the prepared hairdressing base
23.1 parts of an ethanol solution containing 1% to neutralize
It was

[0059]

[Table 2]

The viscosity-average molecular weight and physical properties of the obtained hair styling base material were examined in the same manner as in Example 1. The results are shown in Table 1.

The abbreviations in the table mean the following components.

DMADS: N-acryloxyethyl-N
-Ethyl-N, N-dimethylammonium ethyl sulf
Mate DMAPADS: N-acrylamidopropyl-N-E
Chill-N, N-dimethylammonium ethyl sulfite
To DMDS: N-methacryloxyethyl-N-ethyl-
N, N-dimethylammonium ethyl sulfate t-BuAAm: Nt-butylacrylamide N-OAAm: Nt-octyl acrylamide NVP: N-vinylpyrrolidone EA: Ethyl acrylate IBA: isobutyl acrylate TBA: t-butyl acrylate BA: n-butyl acrylamide LA: lauryl acrylate STA: Stearyl acrylate EMA: ethyl methacrylate TBMA: t-butyl methacrylate EHMA: 2-ethylhexyl methacrylate LMA: Lauryl methacrylate IBMA: isobutyl methacrylate MTA: 2-methoxyethyl acrylate HPA: hydroxypropyl acrylate MAA: methacrylic acid DAAM: Diacetone acrylamide ETMA: 2-ethoxyethyl methacrylate From the results shown in Table 1, the results obtained in Examples 1 to 20
All bases for hair agents are appearance, water solubility, and stability in aqueous solution.
Excellent compatibility with ethanol
I understand.

Formulation Examples 1 to 20 and Comparative Formulation Example 1 Examples 1 to 20 and Comparative ExampleIn 1Obtained base for hair dressing
10 g of an ethanol solution containing 10% by weight of the resin component of
And 10g of liquefied petroleum gas as a propellant
Fill a container (80 ml full volume) and attach it to the valve.
Then, an aerosol product for hair styling was prepared.

Next, using the obtained aerosol product, the setting power of the hair styling agent under high humidity and the physical properties of the film were examined based on the following methods. The results are shown in Table 3.

(A) Setting power under high humidity 2 g of hair having a length of 25 cm was sprayed with the hair styling agent from a distance of 20 cm for 10 seconds, and then the hair had an outer diameter of 1.2 c.
Wrap around a curler of m and dry with warm air of 40 ° C for 60 minutes, then remove the hair from the curler and set the temperature to 3
The length (L ₁ cm) immediately after hanging vertically in an atmosphere of 0 ° C. and 80% relative humidity and the length (L ₂ cm) after standing for 2 hours were measured, and the curl retention was calculated by the following formula:

[0066]

[Equation 1]

Calculated from

A curl retention of 60% or more was passed (indicated by ◯ in the table), and a curl retention of less than 60% was rejected (indicated by x in the table).

(B) Physical properties of film (i) Detergency After spraying the above hair styling agent on a glass plate having a length of 2.5 cm and a width of 7.5 cm from a distance of 20 cm for 5 seconds, the mixture was kept at 20 ° C. for 3 minutes.
Air dried for hours to form a film. 4 this glass plate
The film was dipped in warm water containing 0.2% shampoo at 0 ° C., and the time-dependent change in the dissolved state of the film was examined, and evaluated based on the following evaluation criteria.

(Evaluation criteria) ◯: Completely dissolved within 10 minutes. (Triangle | delta): It melt | dissolves completely within 15 minutes. X: The film remains after 15 minutes.

(Ii) Blocking resistance The above hair styling agent was sprayed onto 2 g of hair having a length of 25 cm for 10 seconds from a distance of 20 cm and applied uniformly. 40 this hair
It was dried for 60 minutes with warm air at 0 ° C., and the state of combing was evaluated using a commercially available comb based on the following evaluation criteria.

(Evaluation criteria) ○: The comb passes smoothly without getting caught. Δ: There is a catch, but the comb can be passed through. X: The comb does not pass.

(Iii) Smoothness A glass plate having a length of 2.5 cm and a width of 7.5 cm was sprayed with the hair styling agent from a distance of 20 cm for 5 seconds, and then at 20 ° C. for 3 minutes.
Air dried for hours to form a film. Next, the feel of the formed film surface was examined with a finger, and the smoothness was evaluated based on the following evaluation criteria.

(Evaluation criteria) ○: It is completely smooth. Δ: Somewhat rough. X: Very rough.

(Iv) Transparency After spraying the above hair styling agent on a glass plate having a length of 2.5 cm and a width of 7.5 cm from a distance of 20 cm for 5 seconds, the mixture was heated at 20 ° C. for 3 hours
Air dried for hours to form a film. Next, the state of the formed film was visually observed and evaluated based on the following evaluation criteria.

(Evaluation criteria) ◯: Completely transparent. Δ: Partly whitened. X: The entire surface is whitened.

(V) Glossiness 2 g of hair having a length of 25 cm was sprayed with the hair styling agent from a distance of 20 cm for 5 seconds and applied uniformly. This hair was dried with warm air at 40 ° C. for 60 minutes, the glossiness was visually observed, and evaluated based on the following evaluation criteria.

(Evaluation criteria) ◯: Very glossy. Δ: Somewhat glossy X: There is no gloss.

[0079]

[Table 3]

From the results shown in Table 3, Formulation Examples 1 to 20
The obtained hair styling products all have the setting power under high humidity necessary for the hair styling agent, the washing property, the blocking resistance, the smoothness, the transparency and the glossiness at the same time. By comparison, it can be seen that the setting force and smoothness are particularly excellent.

[0081]

EFFECT OF THE INVENTION The base of the present invention for hair styling has excellent affinity with hair, imparts beautiful luster, can be retained for a long time on any hairstyle, and has a feeling of stiffness and flaking. The effect that there is no.

Further, the base of the present invention for hair styling has excellent compatibility with water and hydrophilic organic solvents, and while being cationic, the hair styling agent can be prepared by adding an anionic electrolyte or an amine compound. When used in mist sprays, gels, mousses, etc. of aqueous formulations, the physical properties of the hairdressing base are small, so that the hairdressing base does not aggregate and deposit in the spray container or the injection nozzle, which is a waste. There is an effect that it can be used uniformly until the end.

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Claims (2)

(57) [Claims] 1. A compound represented by the general formula (I): (In the formula, X is an imino group or an oxygen atom, R ¹ is a hydrogen atom or a methyl group, R ² is an alkylene group having 1 to 3 carbon atoms,
R ³ , R ⁴ , R ⁵ and R ⁶ each independently represent a methyl group or an ethyl group) 15 to 40% by weight of the (meth) acrylic monomer (A) represented by the general formula (I
I): (In the formula, R ¹ represents a hydrogen atom or a methyl group, and R ⁷ represents an alkyl group having 2 to 8 carbon atoms) (meth) acrylamide derivative monomer (B) 25 to 55% by weight and general formula (III) : [Chemical 3] (In the formula, R ¹ represents a hydrogen atom or a methyl group, and R ⁸ represents an alkyl group having 1 to 18 carbon atoms.) A monomer containing (meth) acrylic acid alkyl ester monomer (C) in an amount of 5 to 60% by weight. A base for hair styling products obtained by polymerizing the ingredients. 2. An ethylenically unsaturated monomer whose monomer component is copolymerizable with a (meth) acrylic monomer (A), a (meth) acrylamide derivative monomer (B) and a (meth) acrylic acid alkyl ester monomer (C). The base for hairdressing composition according to claim 1, which contains 1 to 30% by weight of (D).