CN109602642A - A kind of semipermanent colored hair dye preparation method - Google Patents
A kind of semipermanent colored hair dye preparation method Download PDFInfo
- Publication number
- CN109602642A CN109602642A CN201910023735.9A CN201910023735A CN109602642A CN 109602642 A CN109602642 A CN 109602642A CN 201910023735 A CN201910023735 A CN 201910023735A CN 109602642 A CN109602642 A CN 109602642A
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- China
- Prior art keywords
- hair dye
- semipermanent
- hair
- preparation
- dyestuff
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/042—Gels
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/58—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
- A61K8/585—Organosilicon compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/896—Polysiloxanes containing atoms other than silicon, carbon, oxygen and hydrogen, e.g. dimethicone copolyol phosphate
- A61K8/898—Polysiloxanes containing atoms other than silicon, carbon, oxygen and hydrogen, e.g. dimethicone copolyol phosphate containing nitrogen, e.g. amodimethicone, trimethyl silyl amodimethicone or dimethicone propyl PG-betaine
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/10—Preparations for permanently dyeing the hair
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3855—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/42—Colour properties
- A61K2800/43—Pigments; Dyes
- A61K2800/432—Direct dyes
Abstract
The invention discloses a kind of semipermanent colored hair dye preparation methods, are related to technical field of fine.Preparation method includes the following steps: (1) the preparation of the small molecule dyes with organosilan property: being keyed colored reactive dye monomer using diisocyanate and organosiloxane prepares hair dye dyestuff；Step 2, hair dye preparation: organosilane-modified hair dye is hydrolyzed with dyestuff, and hydrolysate is from coupling gel.The present invention is by synthesizing a kind of semipermanent small molecule hair dye dyestuff, it can be handed over from connection after acting on hair and form macromolecular structure, form macromolecular dyestuff hair dye, this hair dye has the characteristic of macromolecular, human body cell cannot absorb, and have the advantages that safe and non-toxic, lasting, washable, easy to operate.
Description
Technical field
The invention belongs to technical field of fine, more particularly to a kind of semipermanent colored hair dye preparation method.
Background technique
With the raising of living standards of the people, hair dye as a kind of daily cosmetics for changing color development gradually
Common people is come into, modern's self-expression is become and pursues the declaration of individual character.On the one hand, hair dye can be such that color development returns certainly
So, some inadequate natural endowments or posteriori sorry are made up；On the other hand, as individual character and it is fashionable intersperse, many people require to change
Oneself single hair color, to pursue colorful color development.In recent years, hair dyeing had become the wind direction mark of fashion.In recent years
Come, the global hair dye market demand is powerful, has become and develops product the most active in cosmetic field.However it is contaminated in tradition
It sends out in agent, the case of allergy is caused to happen occasionally.With people's health consciousness step up and beauty science be constantly progressive,
There is an urgent need to hair dye that is safe and non-toxic, will not causing skin allergy, macromolecular hair dyes to be increasingly becoming the following hair dyeing by people
The development trend in agent market.
Traditional semipermanent hair dye, mostly uses some molecules small, with the stronger alkalinity of hair affinity, disperse dyes
Etc..It due to the easy permeability of small molecule dyes, can rapidly be penetrated into inside hair after acting on hair, to make color
The a few days can be retained on hair and the flushing being resistant to for several times is just faded.But the easy permeability of traditional small molecule hair dye
Skin can also be penetrated into, pruitus, allergy or serious lesion are caused.
Summary of the invention
It is a kind of semipermanent small by synthesizing the purpose of the present invention is to provide a kind of semipermanent colored hair dye preparation method
Molecule hair dye dyestuff can be handed over from connection after acting on hair and form macromolecular structure, form macromolecular dyestuff hair dye,
This hair dye has the characteristic of macromolecular, and human body cell cannot absorb, with safe and non-toxic, lasting, washable, easy to operate excellent
Point.
In order to solve the above technical problems, the present invention is achieved by the following technical solutions:
The present invention is 1, the semipermanent colored hair dye preparation method of one kind, which is characterized in that comprising steps of
The preparation of step 1, small molecule dyes with organosilan property, specifically includes:
(1), the addition reaction of reactive dye monomer and diisocyanate one end, reaction equation are as follows:
(2), the condensation reaction of organosilan and the diisocyanate other end, reaction equation are as follows:
Step 2, hair dye preparation, specifically include:
(1), organosilane-modified hair dye is hydrolyzed with dyestuff, hydrolysis equation are as follows:
(2), hydrolysate is from coupling gel, reaction equation are as follows:
Further, the step 1 specifically includes: it takes reactive dye monomer to be added to acetone and stirs to Quan Rong, it is small with 2-3
When be slowly dropped into diisocyanate system, organosilan is added after reacting 4-5 hours under conditions of 50-55 DEG C；Exist again
Reaction product is transferred to Rotary Evaporators after reacting 4-5 hours under conditions of 65-70 DEG C, 40-50 DEG C, vacuum degree -0.01~-
Acetone is sloughed under 0.05MP condition of negative pressure to get to organosilane-modified hair dye dyestuff；
The mass ratio of the reactive dye monomer and acetone is 1:5-10；The diisocyanate and reactive dye monomer
Molar ratio be 1:1；The molar ratio of the organosilan and reactive dye monomer is 1:1.
Further, the reactive dye monomer is one or more in structural formula DYE1-DYE4:
Further, the diisocyanate is selected from toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate
(MDI), one of isophorone diisocyanate (IPDI) or hexamethylene diisocyanate (HDI) or a variety of.
Further, the organo silane coupling agent is that KH550, KH560, KH551 contain amino or the silane of hydroxyl is even
Join the one or more of agent.
Further, the step 2 specifically includes: the organosilane-modified hair dye dyestuff for taking step 1 to be prepared
It is soluble in water and auxiliary agent is added is made into aqueous solution, 10-25 DEG C at a temperature of hydrolyze 5-10 minutes；Then uniformly it is applied to hair
On silk, after being acted on 10-20 minutes under room temperature, firmly hair is wrapped up from gel, color is fixed on hair, is formed
Hair dye.
Further, the auxiliary agent includes table grapes saccharic acid calcium, edible essence, moisturizer, glycerol, thickener；
The mass concentration of auxiliary agent is 10-20% in the aqueous solution；Organosilane-modified hair dye is used in the aqueous solution
The mass concentration of dyestuff is 0.05-0.5%；
Wherein, table grapes saccharic acid calcium in the aqueous solution, edible essence, moisturizer, glycerol, the quality between thickener
Than for 0.8-1.2:1-1.5:1-2:5-10:1-3.
The invention has the following advantages:
1, the present invention can be handed over by synthesizing a kind of semipermanent small molecule hair dye dyestuff after acting on hair from connection
Macromolecular structure is formed, the characteristics of high molecular dye is difficult to through cell membrane can be played, improves the safety of hair dye, is formed big
Molecular dye hair dye, this hair dye have the characteristic of macromolecular, and human body cell cannot absorb, and have safe and non-toxic, lasting, resistance to
It washes, easy to operate advantage.
2, the colored macromolecular dyestuff hair dye of the method for the present invention preparation makes to contaminate due to the characteristic with organosilan gel
The hair time is more longlasting, and gel time is short, and faster, the skin covering of the surface of gel-forming makes hair more beautiful to hair dyeing speed.
3, the colored macromolecular dyestuff hair dye of the method for the present invention preparation has the effect of moisturizing sizing to hair.
4, the colored macromolecular dyestuff hair dye of the method for the present invention preparation, the film that gel generates are wrapped in hair surface, more
Hair can be protected to reduce hair impaired.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
Specific embodiment
Prepare embodiment
Dyestuff prepares embodiment 1
First claim toluene di-isocyanate(TDI) (TDI) 0.33g, opens stirring and be warming up to 50-55 DEG C, take blue active dye monomer
(DYE1) 1.05g be added in the acetone of 10g be dispersed with stirring uniformly after, be slowly added into toluene di-isocyanate(TDI) within 2-3 hours
(TDI) in, reaction 4-5 hours is added, KH550 0.42g is added, is warming up to 65-70 DEG C within about 10 minutes, insulation reaction 4-5 is small
When, reaction terminates, and is transferred to Rotary Evaporators, sloughs acetone under 40-50 DEG C, 0.01MPa condition of negative pressure to get organosilan is arrived
Modified blue hair dye dyestuff, number 1#.
Dyestuff prepares embodiment 2
Dyestuff is prepared into the blue active dye monomer (DYE1) in embodiment 1 and replaces with Yellow active dye (DYE4),
Simultaneously with isophorone diisocyanate (IPDI) replacement toluene di-isocyanate(TDI) (TDI), organosilane-modified yellow dye is obtained
Send out agent dyestuff, number 2#.
Dyestuff prepares embodiment 3
Dyestuff is prepared into the blue active dye monomer (DYE1) in embodiment 1 and replaces with black and active dye (DYE3),
Toluene di-isocyanate(TDI) (TDI) is replaced with isophorone diisocyanate (IPDI) simultaneously, and replaces KH550 with KH551, is obtained
To organosilane-modified black hair dye dyestuff, number 3#.
Dyestuff prepares embodiment 4
Dyestuff is prepared into the blue active dye monomer (DYE1) in embodiment 1 and replaces with red reactive dyes (DYE2),
KH550 is replaced with KH551 simultaneously, obtains organosilane-modified red hair dye dyestuff, number 4#.
Application Example
Embodiment 1
Blue dyes hair dye preparation method: by table grapes saccharic acid calcium 1g, edible essence 1.2g, moisturizer 1.5g are sweet
The above-mentioned blue dyes of oily 8.0g, thickener 2.0g, 0.2g is added sequentially to stir evenly in 86.1g deionized water, room temperature
After five minutes, blue hair dye preparation is completed.
Embodiment 2
Cudbear hair dye preparation method: by table grapes saccharic acid calcium 1g, edible essence 1.2g, moisturizer 1.5g are sweet
Oily 8.0g, thickener 2.0g, 0.1g blue dyes 1#, 0.1g orchil 4#, is added sequentially to stir in 86.1g deionized water
Uniformly, after five minutes, is completed in the preparation of purple hair dye to room temperature
Embodiment 3
Black dyes hair dye preparation method: by table grapes saccharic acid calcium 1g, edible essence 1.2g, moisturizer 1.5g are sweet
Oily 8.0g, thickener 2.0g, 0.2g black dyes 3#, it is added sequentially to stir evenly in 86.1g deionized water, room temperature 5
After minute, black hair dye preparation is completed.
It is arranged in pairs or groups by different color dyes, the hair dye of available different color
Hair is washed the moisture wiped to the greatest extent on the end hair when use, then uniformly smears embodiment by the application method of coloring agent
1 or the hair dye for preparing of embodiment 2 on hair, kept for 10-15 minutes at room temperature, it is clean with warm water washing.
Comparative example:
Comparative test is the hair dye for preparing embodiment 1 prepared by the present invention and embodiment 2 and market blue and purple
Color hair dye is applied on white hair topknot according to identical amount and dyes, and then washes and is washed with shampoo, is then dried, dyeing hair
Beam is used as dyeing capacity compared with the white hair topknot of untreated people, with the naked eye carries out judgement scoring, score value 0-5 by 20 people of professional person
Point, the more big then dyeing capacity of score value is better.Small different with buy on the market 2 of sample obtained in test above-described embodiment 1
Molecular dye sample, specific steps are as follows:
White hair 2g is taken, equivalent smears above-mentioned 4 kinds of hair dyes, wherein embodiment 1 and the method smeared of embodiment 2, room temperature
Then 25 DEG C of dyeing place 10 minutes for 25 DEG C of room temperature, wash and washed with shampoo, then 25 DEG C of room temperature dry dyeing.With commercially available
Shampoo washs 1 minute, and water is dry after cleaning, and repeats this operation 5 times, 10 time, 20 times, topknot dyes before washing rear topknot and washing
It compares, judgement scoring is with the naked eye carried out by 20 people of professional person, score value 0-5 points, the more big then color fastness to washing of score value is better.Experiment
As a result it see the table below 1.
Table 1: contrast and experiment
Compared by table 1 it will be seen that embodiment 1 not only has with better dyeing capacity, dye it is full more evenly, and
And color fastness to washing is higher, more difficult decoloration, dyeing guarantor is more longlasting, and effect is very satisfied.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (7)
1. a kind of semipermanent colored hair dye preparation method, which is characterized in that comprising steps of
The preparation of step 1, small molecule dyes with organosilan property, specifically includes:
(1), the addition reaction of reactive dye monomer and diisocyanate one end, reaction equation are as follows:
(2), the condensation reaction of organosilan and the diisocyanate other end, reaction equation are as follows:
Step 2, hair dye preparation, specifically include:
(1), organosilane-modified hair dye is hydrolyzed with dyestuff, hydrolysis equation are as follows:
(2), hydrolysate is from coupling gel, reaction equation are as follows:
2. the semipermanent colored hair dye preparation method of one kind according to claim 1, which is characterized in that step 1 tool
Body includes: to take reactive dye monomer to be added to acetone to stir to Quan Rong, is slowly dropped into diisocyanate system with 2-3 hours
In, organosilan is added after reacting 4-5 hours under conditions of 50-55 DEG C；It is reacted 4-5 hours under conditions of 65-70 DEG C again
Reaction product is transferred to Rotary Evaporators afterwards, sloughs acetone under 40-50 DEG C, vacuum degree -0.01~-0.05MP condition of negative pressure,
Obtain organosilane-modified hair dye dyestuff；
Wherein, the mass ratio of the reactive dye monomer and acetone is 1:5-10；
Wherein, the molar ratio of the diisocyanate and reactive dye monomer is 1:1；
Wherein, the molar ratio of the organosilan and reactive dye monomer is 1:1.
3. the semipermanent colored hair dye preparation method of one kind according to claim 1 or 2, which is characterized in that the activity
Dye monomer is one or more in structural formula DYE1-DYE4:
4. the semipermanent colored hair dye preparation method of one kind according to claim 1 or 2, which is characterized in that described two is different
Cyanate is selected from toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate (MDI), isophorone diisocyanate
(IPDI) or one of hexamethylene diisocyanate (HDI) or a variety of.
5. the semipermanent colored hair dye preparation method of one kind according to claim 1 or 2, which is characterized in that described organic
Silane coupling agent is the one or more for the silane coupling agent that KH550, KH560, KH551 contain amino or hydroxyl.
6. the semipermanent colored hair dye preparation method of one kind according to claim 1, which is characterized in that step 2 tool
Body includes: that the organosilane-modified hair dye dyestuff that takes step 1 to be prepared is soluble in water and auxiliary agent is added is made into aqueous solution,
10-25 DEG C at a temperature of hydrolyze 5-10 minutes；Then it is uniformly applied on hair, after being acted on 10-20 minutes under room temperature, from
Color is fixed on hair by gel to firmly wrap up hair, forms hair dye.
7. the semipermanent colored hair dye preparation method of one kind according to claim 6, which is characterized in that the auxiliary agent includes
Table grapes saccharic acid calcium, edible essence, moisturizer, glycerol, thickener；
The mass concentration of auxiliary agent is 10-20% in the aqueous solution；Organosilane-modified hair dye dyestuff in the aqueous solution
Mass concentration be 0.05-0.5%；
Wherein, table grapes saccharic acid calcium in the aqueous solution, edible essence, moisturizer, glycerol, the mass ratio between thickener are
0.8-1.2:1-1.5:1-2:5-10:1-3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910023735.9A CN109602642A (en) | 2019-01-10 | 2019-01-10 | A kind of semipermanent colored hair dye preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910023735.9A CN109602642A (en) | 2019-01-10 | 2019-01-10 | A kind of semipermanent colored hair dye preparation method |
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| CN109602642A true CN109602642A (en) | 2019-04-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114404323A (en) * | 2022-01-28 | 2022-04-29 | 浙江材华科技有限公司 | Permanent or semi-permanent macromolecular hair dye |
-
2019
- 2019-01-10 CN CN201910023735.9A patent/CN109602642A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114404323A (en) * | 2022-01-28 | 2022-04-29 | 浙江材华科技有限公司 | Permanent or semi-permanent macromolecular hair dye |
| CN114404323B (en) * | 2022-01-28 | 2023-11-10 | 浙江材华科技有限公司 | Permanent or semi-permanent macromolecular hair dye |
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Application publication date: 20190412 |