CN105434190A - Organic silicone surfactant, preparation method thereof and application thereof to cosmetics - Google Patents
Organic silicone surfactant, preparation method thereof and application thereof to cosmetics Download PDFInfo
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- CN105434190A CN105434190A CN201511033865.9A CN201511033865A CN105434190A CN 105434190 A CN105434190 A CN 105434190A CN 201511033865 A CN201511033865 A CN 201511033865A CN 105434190 A CN105434190 A CN 105434190A
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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
- A61K8/18—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
- A61K8/899—Polysiloxanes containing atoms other than silicon, carbon, oxygen and hydrogen, e.g. dimethicone copolyol phosphate containing sulfur, e.g. sodium PG-propyldimethicone thiosulfate copolyol
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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
- A61K8/18—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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
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- 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
- A61Q5/02—Preparations for cleaning the hair
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- 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
- A61K2800/59—Mixtures
- A61K2800/596—Mixtures of surface active compounds
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Abstract
The invention belongs to the field of fine chemical engineering, and discloses an organic silicone surfactant, a preparation method thereof and application thereof to cosmetics. The organic silicone surfactant has a structural formula as shown in the formula (1) (shown in the description); the preparation method of the organic silicone surfactant comprises the following steps: in N2 atmosphere, adding hydrogen-containing silicone oil, increasing the temperature until the reaction temperature reaches 20-90 DEG C, adding a catalyst, dropwise adding allyl epoxy ether with the dropping time being 30-120 min, controlling the temperature to be 40-120 DEG C after the temperature is increased and becomes stable, and carrying out thermal reaction for 60-240 min to remove low-boiling-point substances, so as to obtain an intermediate; adding a reactant B and a solvent into a flask, increasing the temperature until the reaction temperature reaches 30-100 DEG C, dropwise adding a silicone intermediate for 20-120 min, carrying out thermal reaction for 60-240 min, increasing the temperature to be 40-100 DEG C, and carrying out thermal reaction for 30-90 min, so as to obtain the product. The organic silicone surfactant can be used as a moisturizer, conditioner or auxiliary surface active agent in personal care products.
Description
Technical field
The invention belongs to field of fine chemical, particularly a kind of organic silicon surfactant and preparation method thereof and at personal care articles, the application in bath gel, shampoo and moisturiser.
Background technology
Polydimethylsiloxane has many properties such as hydrophobicity, interfacial activity, heat stability, and is widely used in commercial production, such as polyurethane foam stabilizer, emulsifying agent, defoamer, releasing agent etc.But polydimethylsiloxane is insoluble in organic solvent and water, because which limit the application of polydimethylsiloxane.By organically-modified polydimethylsiloxane, in the polysiloxanes end of the chain or/and two ends or/and side introduce oil-soluble/or and water miscible organic group, then effectively can address this problem, make the purposes of polydimethylsiloxane more extensive.Such as, by the polyether silicone oil after these technological improvements, alkyl-silicone oil, Silica hydrogel, amido silicon oil is widely used as emulsifying agent, emollient, hair conditioner etc. at cosmetic field.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, primary and foremost purpose of the present invention is to provide a kind of organic silicon surfactant.
Another object of the present invention is to the preparation method that above-mentioned organic silicon surfactant is provided.
Another object of the present invention is to provide the application of above-mentioned organic silicon surfactant in cosmetics.
Object of the present invention is realized by following technical proposals:
A kind of organic silicon surfactant, this organic silicon surfactant has such as formula the structure shown in (1):
Wherein, R has such as formula the structure shown in (2):
Wherein, n=0 ~ 100, are preferably 0 ~ 20;
Q has such as formula the structure shown in (3):
R
1, R
2, R
3, R
4or R
5for-CH
3or-CH
2cH
2oH; R
1, R
2and R
3can not be-CH simultaneously
3, R
4and R
5can not be-CH simultaneously
3; A is Cl or Ac.
The preparation method of above-mentioned organic silicon surfactant, comprises following operating procedure:
(1) silicone intermediate preparation:
N
2under atmosphere, in the four-hole boiling flask with backflow and agitating device, add containing hydrogen silicone oil, be warming up to reaction temperature T
1, add catalyst, drip pi-allyl ether epoxy, time for adding t
1, temperature rises, and after temperature stabilization, controls reaction temperature T
2, insulation reaction; Reaction end is the process of sample thief sodium hydroxide solution, no longer produces hydrogen, cessation reaction, then opens vacuum pump, deviate from low-boiling-point substance, obtain silicone intermediate;
(2) preparation of organic silicon surfactant:
To in the four-hole boiling flask with backflow and agitating device, add reactant B and solvent, be warming up to reaction temperature T
3; Drip step (1) gained silicone intermediate, time for adding t
2, drip rear insulation reaction t
3; Be warming up to reaction temperature T
4, insulation reaction t
4; Obtain organic silicon surfactant product.
Step (2) described reactant B is secondary amine, sodium sulfite solution, hydroxyl tertiary amine hydrochlorate or hydroxyl tertiary amine acetate containing hydroxyl, has such as formula the structure described in (4):
Wherein, R
1, R
2or R
3for H or-CH
3or-CH
2cH
2oH, and R
1, R
2and R
3in have two at least respectively containing H and-CH
2cH
2oH; R
6, R
7or R
8for-CH
3or-CH
2cH
2oH, and R
6, R
7or R
8in have one at least containing-CH
2cH
2oH; A is Cl or Ac.
Step (2) described reactant B is preferably methyl monoethanolamine, diethanolamine, triethanolamine hydrochloride, triethanolamine acetate, dimethyl ethanol amine hydrochlorate or triethanolamine acetate.
Step (1) described containing hydrogen silicone oil is heptamethyltrisiloxane;
The mol ratio of described containing hydrogen silicone oil and pi-allyl ether epoxy is 1.2 ~ 0.9:1;
Described reaction temperature T
1it is 20 ~ 90 DEG C;
Described catalyst is platinum catalyst, has high activity under low temperature;
Described pi-allyl ether epoxy has the structure described in formula (5):
Wherein, n is 0 ~ 100, is preferably 0 ~ 20;
Described t
1be 30 ~ 120min;
Described T
2it is 40 ~ 120 DEG C;
The time of described insulation reaction is 60 ~ 240min;
Described deviate from low-boiling-point substance be adopt following condition: vacuum 0.08 ~ 0.095MPa, temperature is 90 ~ 120 DEG C, and the time is 30 ~ 120min;
The mol ratio of step (2) described silicone intermediate and reactant B is 1.1 ~ 0.9:1;
Described reaction temperature T
3it is 30 ~ 100 DEG C;
The time for adding t of described silicone intermediate
2be 20 ~ 120min;
Described insulation reaction t
3be 60 ~ 240min;
Described reaction temperature T
4it is 40 ~ 100 DEG C;
Described insulation reaction time t
4be 30 ~ 90min;
Described solvent is water.
When described reactant B is the secondary amine containing hydroxyl, in step (2) described insulation reaction t
4further comprising the steps of afterwards: dropwise reaction thing C, then at T
4, insulation reaction t
5after obtain organic silicon surfactant product;
Described reactant C is the sodium chloroacetate solution of mass percent 70%;
In described reactant B and reactant C, the mol ratio of sodium chloroacetate is 1.05 ~ 0.95:1;
Described t
5be 60 ~ 240min.
The application of above-mentioned organic silicon surfactant in preparation personal care product, the mass percent concentration of described organic silicon surfactant in personal care product is 0.05 ~ 10.0%, is preferably 1.0 ~ 5.0%.Coldly to join, heat joins.
Principle of the present invention: the invention provides that a kind of synthesis technique is simple, the organic silicon surfactant of small-molecular-weight, find in application that this organic silicon surfactant has certain short bubble property, its distinctive polyhydroxy cation structure makes it have hydrophilic, water absorption, adsorptivity simultaneously, while the siloxane structure of short chain makes it have breathability, avoid the too fast loss of moisture content, embody very excellent performance of keeping humidity, spreadability.Have at least a kind of organic silicon surfactant to be excellent personal nursing wetting agent raw material, conditioner in embodiment disclosed in this patent, surface modifier etc., can not only provide the effect of long-acting moisturizing, can also bring that silicone oil with low viscosity is salubrious, the skinfeel of non-greasy.
Hinge structure of the present invention, has following advantage and beneficial effect:
(1) the organic silicon surfactant technique of the present invention's synthesis is simple, easy to operate.
(2) organic silicon surfactant of the present invention's synthesis has the effect of moisturizing, conditioning personal care product, also can be used as cosurfactant and is applied to compound surfactant product.
(3) organic silicon surfactant of the present invention's synthesis is gentle, can with the skinfeel of water profit and softness.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
The raw material (hydrogen containing siloxane and alkenes compounds) that the embodiment of the present invention uses all can be buied from commercially available product.
Below by way of specific embodiment, the present invention is further elaborated.
Pi-allyl ether epoxy used in embodiment has following structure:
The structure of pi-allyl ether epoxy is:
wherein, n=0 ~ 20.
Embodiment 1
N
2under atmosphere, to in the four-hole boiling flask with backflow and agitating device, add 1.2mol heptamethyltrisiloxane, be warming up to reaction temperature 40 DEG C, add catalyst, drip 1.0mol pi-allyl ether epoxy (n=0), time for adding 60min, temperature can obviously rise, after temperature stabilization, control to reaction temperature 80 DEG C, insulation reaction 180min.Reaction end is the process of sample sodium hydroxide solution, not at generation hydrogen.Open vacuum pump, control vacuum 0.09MPa, temperature is 100 DEG C, continues evacuation 90min, deviates from low-boiling-point substance, obtain intermediate.
Embodiment 2
N
2under atmosphere, to in the four-hole boiling flask with backflow and agitating device, add 1.0mol heptamethyltrisiloxane, be warming up to reaction temperature 20 DEG C, add catalyst, drip 1.0mol pi-allyl ether epoxy (n=8), time for adding 30min, temperature can obviously rise, after temperature stabilization, control to reaction temperature 60 DEG C, insulation reaction 240min.Reaction end is the process of sample sodium hydroxide solution, not at generation hydrogen.Open vacuum pump, control vacuum 0.08MPa, temperature is 90 DEG C, continues evacuation 120min, deviates from low-boiling-point substance, obtain intermediate.
Embodiment 3
N
2under atmosphere, to in the four-hole boiling flask with backflow and agitating device, add 0.95mol heptamethyltrisiloxane, be warming up to reaction temperature 80 DEG C, add catalyst, drip 1.0mol pi-allyl ether epoxy (n=20), time for adding 120min, temperature can obviously rise, after temperature stabilization, control to reaction temperature 100 DEG C, insulation reaction 90min.Reaction end is the process of sample sodium hydroxide solution, not at generation hydrogen.Open vacuum pump, control vacuum 0.09MPa, temperature is 100 DEG C, continues evacuation 90min, deviates from low-boiling-point substance, obtain intermediate.
Embodiment 4
N
2under atmosphere, to in the four-hole boiling flask with backflow and agitating device, add 1.05mol heptamethyltrisiloxane, be warming up to reaction temperature 90 DEG C, add catalyst, drip 1.0mol pi-allyl ether epoxy (n=4), time for adding 40min, temperature can obviously rise, after temperature stabilization, control to reaction temperature 120, insulation reaction 60min.Reaction end is the process of sample sodium hydroxide solution, not at generation hydrogen.Open vacuum pump, control vacuum 0.095MPa, temperature is 120 DEG C, and lasting evacuation is 30min, deviates from low-boiling-point substance, obtains intermediate.
Embodiment 5
N
2under atmosphere, to in the four-hole boiling flask with backflow and agitating device, add 0.9mol heptamethyltrisiloxane, be warming up to reaction temperature 30 DEG C, add catalyst, drip 1.0mol pi-allyl ether epoxy (n=12), time for adding 90min, temperature can obviously rise, after temperature stabilization, control to reaction temperature 40 DEG C, insulation reaction 200min.Reaction end is the process of sample sodium hydroxide solution, not at generation hydrogen.Open vacuum pump, control vacuum 0.08MPa, temperature is 90 DEG C, continues evacuation 60min, deviates from low-boiling-point substance, obtain intermediate.
Embodiment 6
To in the four-hole boiling flask with backflow and agitating device, add 1.0mol dimethyl ethanol amide hydrochloride (mass fraction is 30%), be warming up to reaction temperature 50 DEG C; Drip intermediate 1.05mol, time for adding 60min described in embodiment 1, drip rear insulation reaction 60min; Be warming up to reaction temperature 80 DEG C, insulation reaction 90min; Obtain product.
Embodiment 7
To in the four-hole boiling flask with backflow and agitating device, add 1.0mol dimethylethanolamine Acetate Solution (mass fraction is 30%), be warming up to reaction temperature 30 DEG C; Drip intermediate 1.0mol, time for adding 100min described in embodiment 4, drip rear insulation reaction 90min; Be warming up to reaction temperature 100 DEG C, insulation reaction 90min; Obtain product.
Embodiment 8
To in the four-hole boiling flask with backflow and agitating device, add 1.0mol sodium sulfite solution (mass fraction is 30%), be warming up to reaction temperature 100 DEG C; Drip intermediate 0.9mol, time for adding 20min described in embodiment 3, drip rear insulation reaction 120min; Be warming up to reaction temperature 100 DEG C, insulation reaction 30min; Obtain product.
Embodiment 9
To in the four-hole boiling flask with backflow and agitating device, add 1.0mol methyl monoethanolamine solution (mass fraction is 30%), be warming up to reaction temperature 50 DEG C; Drip intermediate 1.1mol, time for adding 120min described in embodiment 5, drip rear insulation reaction 240min; Be warming up to reaction temperature 90 DEG C, insulation reaction 30min; Drip 0.95mol sodium chloroacetate solution (mass fraction is 70%), then at 90 DEG C of insulation reaction 120min, obtain product.
Embodiment 10
To in the four-hole boiling flask with backflow and agitating device, add 0.95mol diethanolamine solution (mass fraction is 30%), be warming up to reaction temperature 60 DEG C; Drip intermediate 1.0mol, time for adding 50min described in embodiment 1, drip rear insulation reaction 180min; Be warming up to reaction temperature 85 DEG C, insulation reaction 90min; Drip 0.95mol sodium chloroacetate solution (mass fraction is 70%), then at 85 DEG C of insulation reaction 120min, obtain product.
Embodiment 11
To in the four-hole boiling flask with backflow and agitating device, add 1.0mol triethanolamine hydrochloride (mass fraction is 30%), be warming up to reaction temperature 30 DEG C; Drip intermediate 1.0mol, time for adding 100min described in embodiment 1, drip rear insulation reaction 180min; Be warming up to reaction temperature 65 DEG C, insulation reaction 80min, obtains product.
Embodiment 12
To in the four-hole boiling flask with backflow and agitating device, add 1.1mol sodium sulfite solution (mass fraction is 30%), be warming up to reaction temperature 85 DEG C; Drip intermediate 1.0mol, time for adding 90min described in embodiment 1, drip rear insulation reaction 120min; Be warming up to reaction temperature 95 DEG C, insulation reaction 90min; Obtain product.
Embodiment 13
To in the four-hole boiling flask with backflow and agitating device, add 1.0mol triethanolamine Acetate Solution (mass fraction is 30%), be warming up to reaction temperature 55 DEG C; Drip intermediate 1.0mol, time for adding 100min described in embodiment 4, drip rear insulation reaction 120min; Be warming up to reaction temperature 90 DEG C, insulation reaction 90min, obtains product.
Embodiment 14
To in the four-hole boiling flask with backflow and agitating device, add 1.05mol sodium sulfite (mass fraction is 30%), be warming up to reaction temperature 75 DEG C; Drip intermediate 1.0mol, time for adding 120min described in embodiment 3, drip rear insulation reaction 100min; Be warming up to reaction temperature 100 DEG C, insulation reaction 40min, obtains product.
Embodiment 15
To in the four-hole boiling flask with backflow and agitating device, add 0.95mol diethanolamine solution (mass fraction is 30%), be warming up to reaction temperature 60 DEG C; Drip intermediate 1.0mol, time for adding 90min described in embodiment 2, drip rear insulation reaction 120min; Be warming up to reaction temperature 90 DEG C, insulation reaction 90min; Drip 0.95mol sodium chloroacetate solution (mass fraction is 70%), then at 90 DEG C of insulation reaction 110min, obtain product.
Application Example 1
The preparation of gentleness, anti-acne facial milk cleanser, its formula is as shown in table 1:
Table 1: gentle, anti-acne facial milk cleanser formula
Its preparation method is, water is heated to 55-60 DEG C, adds HANSHENGJIAO, rapid stirring, make it to dissolve completely, under stirring, add remaining ingredient (before adding next component, guaranteeing that last component stirs) successively, until become homogeneous mixture, add essence and antiseptic, stir, obtain milky white thick shape facial milk cleanser.
Application Example 2
The preparation of water profit repair cream, its formula is as shown in table 2:
Table 2: water profit repair cream formula
Its preparation method is: add suitable quantity of water and beaker, adds hydroxyethyl-cellulose under stirring, is heated to 55 ~ 60 DEG C, adds surplus component, stirs, and is heated to 65 ~ 70 DEG C, is stirred to 60min.Be cooled to 40 ~ 45 DEG C, adjust pH to 4.5 ~ 5.0.Add pigment, essence and antiseptic, stir, cool and obtain milky white water profit repair cream.
Application Example 3
The preparation of skin lotion, its formula is as shown in table 3:
Table 3: skin lotion formula
Its preparation method is: components I and compositionⅱ are heated to 65 ~ 70 DEG C respectively, and then under Keep agitation and heating, be distributed to gradually in components I by compositionⅱ, abundant dispersed with stirring is even.Limit is stirred change and is cooled to 40 ~ 45 DEG C, adds essence, antiseptic, obtains the low sticky lotion of water white transparency.
Application Example 4
The preparation of transparent shampoo, its formula is as shown in table 4:
Table 4: transparent shampoo formula
Its preparation method is: be added to the water by I part material and be heated with stirring to about 80 DEG C, insulated and stirred evenly forms transparence, it is good that II part is heated to 75 DEG C of complete hydrations, add I system and stir cooling, add remaining III component successively stir when temperature is reduced to about 40 DEG C, obtain clear viscous shampoo.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. an organic silicon surfactant, is characterized in that: this organic silicon surfactant has such as formula the structure shown in (1):
Wherein, R has such as formula the structure shown in (2):
Wherein, n=0 ~ 100;
Q has such as formula the structure shown in (3):
R
1, R
2, R
3, R
4or R
5for-CH
3or-CH
2cH
2oH; R
1, R
2and R
3can not be-CH simultaneously
3, R
4and R
5can not be-CH simultaneously
3; A is Cl or Ac.
2. a kind of silicon surface active agent according to claim 1, is characterized in that: described n is 0 ~ 20.
3. the preparation method of organic silicon surfactant according to claim 1, is characterized in that comprising following operating procedure:
(1) silicone intermediate preparation:
N
2under atmosphere, in the four-hole boiling flask with backflow and agitating device, add containing hydrogen silicone oil, be warming up to reaction temperature T
1, add catalyst, drip pi-allyl ether epoxy, time for adding t
1, temperature rises, and after temperature stabilization, controls reaction temperature T
2, insulation reaction; Reaction end is the process of sample thief sodium hydroxide solution, no longer produces hydrogen, cessation reaction, then opens vacuum pump, deviate from low-boiling-point substance, obtain silicone intermediate;
(2) preparation of organic silicon surfactant:
To in the four-hole boiling flask with backflow and agitating device, add reactant B and solvent, be warming up to reaction temperature T
3; Drip step (1) gained silicone intermediate, time for adding t
2, drip rear insulation reaction t
3; Be warming up to reaction temperature T
4, insulation reaction t
4; Obtain organic silicon surfactant product.
4. preparation method according to claim 3, it is characterized in that: step (2) described reactant B is secondary amine, sodium sulfite solution, hydroxyl tertiary amine hydrochlorate or hydroxyl tertiary amine acetate containing hydroxyl, have such as formula the structure described in (4):
Wherein, R
1, R
2or R
3for H or-CH
3or-CH
2cH
2oH, and R
1, R
2and R
3in have two at least respectively containing H and-CH
2cH
2oH; R
6, R
7or R
8for-CH
3or-CH
2cH
2oH, and R
6, R
7or R
8in have one at least containing-CH
2cH
2oH; A is Cl or Ac.
5. preparation method according to claim 3, is characterized in that: step (2) described reactant B is methyl monoethanolamine, diethanolamine, triethanolamine hydrochloride, triethanolamine acetate, dimethyl ethanol amine hydrochlorate or triethanolamine acetate.
6. preparation method according to claim 3, is characterized in that: step (1) described containing hydrogen silicone oil is heptamethyltrisiloxane;
The mol ratio of described containing hydrogen silicone oil and pi-allyl ether epoxy is 1.2 ~ 0.9:1;
Described reaction temperature T
1it is 20 ~ 90 DEG C;
Described catalyst is platinum catalyst;
Described pi-allyl ether epoxy has the structure described in formula (5):
Wherein, n is 0 ~ 100;
Described t
1be 30 ~ 120min;
Described T
2it is 40 ~ 120 DEG C;
The time of described insulation reaction is 60 ~ 240min;
Described deviate from low-boiling-point substance be adopt following condition: vacuum 0.08 ~ 0.095MPa, temperature is 90 ~ 120 DEG C, and the time is 30 ~ 120min;
The mol ratio of step (2) described silicone intermediate and reactant B is 1.1 ~ 0.9:1;
Described reaction temperature T
3it is 30 ~ 100 DEG C;
The time for adding t of described silicone intermediate
2be 20 ~ 120min;
Described insulation reaction t
3be 60 ~ 240min;
Described reaction temperature T
4it is 40 ~ 100 DEG C;
Described insulation reaction time t
4be 30 ~ 90min;
Described solvent is water.
7. preparation method according to claim 6, is characterized in that: described n is 0 ~ 20.
8. preparation method according to claim 3, is characterized in that: when described reactant B is the secondary amine containing hydroxyl, in step (2) described insulation reaction t
4further comprising the steps of afterwards: dropwise reaction thing C, then at T
4, insulation reaction t
5after obtain organic silicon surfactant product;
Described reactant C is the sodium chloroacetate solution of mass percent 70%;
In described reactant B and reactant C, the mol ratio of sodium chloroacetate is 1.05 ~ 0.95:1;
Described t
5be 60 ~ 240min.
9. the application of organic silicon surfactant according to claim 1 in preparation personal care product, is characterized in that: the mass percent concentration of described organic silicon surfactant in personal care product is 0.05 ~ 10.0%.
10. application according to claim 1, is characterized in that: the mass percent concentration of described organic silicon surfactant in personal care product is 1.0 ~ 5.0%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942821A (en) * | 2019-03-26 | 2019-06-28 | 吉林乾仁新材料有限公司 | Preparation method of hydroxylamino-modified silicone oil cation emulsion and products thereof and application |
| CN111004396A (en) * | 2019-12-27 | 2020-04-14 | 江苏美思德化学股份有限公司 | Tertiary amino modified organic silicon polyether copolymer and preparation method and application thereof |
| CN112876684A (en) * | 2021-03-18 | 2021-06-01 | 新辉（中国）新材料有限公司 | Micron-level high-crosslinking-degree organic silicon polymer microspheres with controllable particle sizes and preparation method thereof |
| CN114907442A (en) * | 2022-06-08 | 2022-08-16 | 常熟理工学院 | Organic silicon modified copper peptide and preparation method thereof |
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| CN112876684B (en) * | 2021-03-18 | 2023-03-14 | 新辉（中国）新材料有限公司 | Micron-level high-crosslinking-degree organic silicon polymer microspheres with controllable particle sizes and preparation method thereof |
| CN114907442A (en) * | 2022-06-08 | 2022-08-16 | 常熟理工学院 | Organic silicon modified copper peptide and preparation method thereof |
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