CN110974715A - APG (ammonium polyphosphate) modified MBBT (MBBT) composite material and preparation method of aqueous slurry thereof - Google Patents
APG (ammonium polyphosphate) modified MBBT (MBBT) composite material and preparation method of aqueous slurry thereof Download PDFInfo
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/60—Sugars; Derivatives thereof
- A61K8/602—Glycosides, e.g. rutin
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
- A61K8/496—Triazoles or their condensed derivatives, e.g. benzotriazoles
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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
- A61K8/85—Polyesters
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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
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
- A61K8/893—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by an alkoxy or aryloxy group, e.g. behenoxy dimethicone or stearoxy dimethicone
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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
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
- A61K8/894—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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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
- 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
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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Abstract
The invention discloses an APG modified MBBT composite material and a preparation method of aqueous slurry thereof, and specifically, MBBT is added into an APG aqueous solution, the temperature of the heating system is 50-100 ℃, reflux reaction is carried out for 2-8 hours, and the APG modified MBBT composite material is prepared after spray drying. Adding the APG modified MBBT composite material into deionized water, adding a dispersing agent in batches, performing dispersion grinding through a sanding dispersion stirring multi-purpose machine, adding a preservative, and performing grinding for 1-3 hours through the sanding dispersion stirring multi-purpose machine to obtain the aqueous slurry of the APG modified MBBT composite material. The method adopts APG to modify MBBT, so that the composite slurry has better moisture retention and better application in the formula of cosmetics; and the MBBT particles and the dispersing agent can be better combined, so that the dispersing effect is better, and the prepared aqueous slurry has better stability and sun protection index.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to an APG (ammonium polyphosphate) modified MBBT (sodium buna-butyl-buna-methyl) composite material and a preparation method of aqueous slurry thereof.
Background
With the remarkable increase of skin diseases caused by sunlight irradiation in the global scope, the development and research of various sunscreen cosmetics for protecting the skin from the damage of ultraviolet rays in the sunlight become difficult problems which are urgently needed to be solved by cosmetic enterprises. Ultraviolet rays which can cause damage to skin in sunlight mainly comprise UVA wave bands with the wavelength of 320-400 nm and UVB wave bands with the wavelength of 280-320 nm. The purpose of scientific and effective combination can be achieved only by accurately measuring the ultraviolet absorption of the sunscreen agent in UVA and UVB wave bands.
Methylene bis-benzotriazolyl tetramethyl butyl phenol (MBBT) is a broad-spectrum organic sunscreen agent with good application prospect, and has the capability of shielding ultraviolet rays in both UVA and UVB wave bands. The MBBT molecular structure contains chromophoric groups for absorbing ultraviolet rays, and ultraviolet shielding is realized through scattering and absorption. However, since MBBT is easily agglomerated in an aqueous solution, the uv absorption effect is poor, and the application in the field of sun protection is limited. And in the use process of the MBBT, dust cannot escape, so that the MBBT is harmful to the physical health of operators and the environmental protection.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to solve the problems of particle agglomeration phenomenon, difficult push-away, dust pollution and the like of MBBT in the using process of cosmetics, the invention provides an APG (alkyl glycoside) modified MBBT composite material and a preparation method of aqueous slurry thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: an APG modified MBBT composite material is prepared by the following method: adding MBBT into an APG aqueous solution, heating the system to 50-100 ℃, carrying out reflux reaction for 2-8 hours, and carrying out spray drying on the obtained dispersion liquid to obtain the APG modified MBBT composite material; the mass ratio of the MBBT to the APG is 3-8: 1. Further, the APG is any one or a combination of more than one of APG0810, APG1214, APG 0814 or APG 1216. The APG is a safe modifier, can be stored for a long time in a larger temperature range, has the function of humidification, completely meets the performance requirements of active components for cosmetics, and has high reliability.
A preparation method of aqueous slurry of an APG modified MBBT composite material comprises the following steps: and uniformly dispersing the APG modified MBBT composite material in deionized water under the action of a dispersing agent to prepare the aqueous slurry of the APG modified MBBT composite material.
Further, the method comprises the following specific steps:
adding the APG modified MBBT composite material into deionized water, dispersing by using a dispersion disc of a sanding dispersion stirring multipurpose machine, dropwise adding a part of dispersing agent into the composite material, switching to a grinding wheel, and dropwise adding the rest dispersing agent while grinding, wherein the weight part of the deionized water is 30-80, the weight part of the APG modified MBBT composite material is 20-70, and the weight part of the dispersing agent is 1-15; and then adding 0.1-5 parts by weight of preservative, and grinding for 1-3 hours by using a sanding, dispersing and stirring multi-purpose machine to obtain the aqueous slurry of the APG modified MBBT compound.
Preferably, the dispersing agent is any one or a combination of several of methyl ether dimethicone (6011), polyhydroxystearic acid (300R) and lauryl polyglycerol-3 polydimethylsiloxyethyl dimethicone (6105).
Preferably, the preservative is any one or a combination of more of phenoxyethanol, caprylyl glycol, 1,2 pentanediol or 1,2 hexanediol.
The invention has the beneficial effects that:
1. the method adopts APG to modify MBBT, so that the composite slurry has better moisture retention and better application in the formula of cosmetics; the MBBT particles and the dispersing agent can be better combined, so that the dispersing effect is better;
2. the method adopts a sand grinding, dispersing and stirring multi-purpose machine for dispersing, and breaks the dispersed and agglomerated MBBT particles; the dispersant is utilized to better disperse and wet MBBT particles, so that the MBBT particles are stably and uniformly dispersed in an aqueous phase medium to form a stable composite system, and the sun protection index of the product is greatly improved.
Drawings
Fig. 1 shows the results of absorbance measurements on aqueous slurries of APG-modified MBBT composites prepared in examples of the present invention and comparative examples.
Detailed description of the preferred embodiments
The present invention will be described in more detail below with reference to examples, but the scope of the present invention is not limited to these examples. In the following examples, APG is produced by Shanghai Kai chemical Co., Ltd, and MBBT is produced by Meifeng chemical Co., Huangshi, Hubei province.
Example 1
A preparation method of aqueous slurry of an APG modified MBBT composite material comprises the following specific steps:
1. firstly, 20g of APG 0814 aqueous solution is added into a flask with mechanical stirring, the water bath temperature is 97 ℃, then 100g of MBBT is added into the flask to be stirred and is subjected to heat preservation and reflux reaction for 2 hours, and finally, the obtained APG modified MBBT dispersion is subjected to spray drying, so that the APG modified MBBT composite material is obtained.
2. And weighing deionized water and the APG modified MBBT composite material prepared in the step 1, adding the deionized water and the APG modified MBBT composite material into a sanding cylinder of a sanding dispersion and stirring multi-purpose machine, dropwise adding a part of 6011 dispersing agent after a dispersion disc is pre-dispersed for 10min at the rotating speed of 2000r/min, and dropwise adding the rest 6011 dispersing agent again at the rotating speed of 4000r/min by changing a grinding wheel, wherein the aim is to prevent a large amount of bubbles possibly generated by adding the dispersing agent at one time and influence the use of slurry, adding phenoxyethanol, and grinding for 1h to obtain the aqueous slurry of the APG modified MBBT composite material, namely the dispersed slurry 1. The dispersing slurry 1 for short comprises the following components in percentage by mass: 50% of APG modified MBBT composite material, 10% of 6011 dispersant, 3% of phenoxyethanol and deionized water until the total mass of the dispersed slurry is 100%. The 6011 dispersant added twice in this example is of the same mass.
Example 2
Preparing an APG modified MBBT composite material: adding 20g of APG0810 aqueous solution into a flask with mechanical stirring, controlling the water bath temperature to be 80 ℃, then adding 140g of MBBT into the flask, stirring, preserving heat, refluxing and reacting for 5 hours, and finally, carrying out spray drying on the obtained APG modified MBBT dispersion liquid to obtain the APG modified MBBT composite material;
the aqueous slurry of the APG modified MBBT composite material contains the following components (in percentage by mass): 40% of APG modified MBBT composite material, 4% of 300R dispersant, 3% of octyl glycol and the balance of deionized water. The preparation method comprises the following steps:
weighing deionized water and the APG modified MBBT composite material, adding the deionized water and the APG modified MBBT composite material into a sanding charging barrel of a sanding dispersion and stirring multi-purpose machine, dropwise adding a 300R dispersing agent with the formula amount of 5/8 after a dispersion disc is pre-dispersed for 10min at the rotating speed of 2000R/min, dropwise adding the rest 300R at the rotating speed of 4000R/min by changing a grinding wheel, adding caprylyl glycol, and grinding for 1h to obtain the aqueous slurry of the APG modified MBBT composite material, namely the dispersion slurry 2.
Example 3
Preparing an APG modified MBBT composite material: adding 50g of APG 1216 aqueous solution into a flask with mechanical stirring, wherein the water bath temperature is 50 ℃, then adding 150g of MBBT into the flask, stirring, preserving heat, refluxing and reacting for 4 hours, and finally, carrying out spray drying on the obtained APG modified MBBT dispersion liquid to obtain the APG modified MBBT composite material;
aqueous slurry of APG-modified MBBT composite 3: comprises the following components (by mass percent): 30% of APG modified MBBT composite material, 4% of 6011 dispersant, 5% of 1,2 pentanediol, and the balance of deionized water.
Weighing deionized water and the compound, adding the deionized water and the compound into a sand grinding cylinder, pre-dispersing for 10min by a dispersion disc at the rotating speed of 2000r/min, dropwise adding a 6011 dispersing agent with the formula amount of 5/8, replacing a grinding wheel, dropwise adding the rest 6011 at the rotating speed of 4000r/min, adding 1,2 pentanediol, and grinding for 1h to obtain the aqueous slurry of the APG modified MBBT composite material, which is referred to as dispersed slurry 3 for short.
Example 4
Preparing an APG modified MBBT composite material: adding 30g of APG1214 water solution into a flask with mechanical stirring, wherein the water bath temperature is 70 ℃, then adding 240g of MBBT into the flask, stirring, preserving heat, refluxing and reacting for 8 hours, and finally, carrying out spray drying on the obtained APG modified MBBT dispersion liquid to obtain the APG modified MBBT composite material;
the aqueous slurry 4 of the APG modified MBBT composite material comprises the following components in percentage by mass: 35% of APG modified MBBT composite material, 10% of 6015 dispersing agent, 1% of 1,2 pentanediol, and the balance of deionized water. The preparation method comprises the following steps:
weighing deionized water and the compound, adding the deionized water and the compound into a sand grinding cylinder, pre-dispersing for 10min by a dispersion disc at the rotating speed of 2000r/min, dropwise adding a 6015 dispersing agent with the formula amount of 1/4, replacing a grinding wheel, dropwise adding the rest 6015 dispersing agent at the rotating speed of 4000r/min, adding 1,2 pentanediol, and grinding for 1h to obtain the aqueous slurry of the APG modified MBBT composite material, namely the dispersed slurry 4 for short.
Comparative example 1
The step of APG modification of MBBT in the following 1 is removed, and the specific operation is as follows:
the aqueous slurry of the APG modified MBBT composite material comprises the following components in parts by weight: 50% of MBBT, 10% of 6011 dispersant, 3% of phenoxyethanol and the balance of deionized water. The preparation method comprises the following steps:
weighing deionized water and MBBT, adding the deionized water and the MBBT into a sand grinding cylinder, pre-dispersing for 10min by a dispersion disc at the rotating speed of 2000r/min, then adding a 6011 dispersing agent with the formula amount of 1/2, grinding by a grinding wheel, adding the rest 6011 at the rotating speed of 4000r/min under the condition, adding phenoxyethanol, and grinding for 1h to obtain the aqueous slurry of the APG modified MBBT composite material, which is called as dispersing slurry 5 for short.
The application effect test of the slurry obtained by the invention comprises the following steps:
the aqueous slurries of APG-modified MBBT composite materials prepared in examples 1 to 4 and comparative example 1 were added with deionized water, respectively, to prepare 50ppm dispersions, and after further ultrasonic dispersion for 30 minutes, the absorbances of light were measured on an ultraviolet-visible near-infrared spectrophotometer (UV3600, shimadzu corporation, japan) using a quartz cuvette having a light path of 1cm and deionized water as a reference, respectively. The experimental results are shown in FIG. 1. As can be seen from the figure, the dispersion slurry prepared by the invention has excellent full-wave band ultraviolet blocking effect and strong shielding capability on UVA and UVB.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and their concepts should be equivalent or changed within the technical scope of the present invention.
Claims (6)
1. An APG modified MBBT composite material, which is characterized in that: is prepared by the following steps: adding MBBT into an APG aqueous solution, heating the system to 50-100 ℃, carrying out reflux reaction for 2-8 hours, and carrying out spray drying on the obtained dispersion liquid to obtain the APG modified MBBT composite material; the mass ratio of the MBBT to the APG is 3-8: 1.
2. The APG-modified MBBT composite of claim 1, wherein: the APG is any one or the combination of more than one of APG0810, APG1214, APG 0814 or APG 1216.
3. A preparation method of aqueous slurry of an APG modified MBBT composite material is characterized by comprising the following steps: the method comprises the following steps: uniformly dispersing the APG modified MBBT composite material in deionized water by the action of a dispersing agent to prepare the aqueous slurry of the APG modified MBBT composite material according to the claim 1 or 2.
4. The method of preparing an aqueous slurry of an APG-modified MBBT composite according to claim 3, characterized in that: the method comprises the following specific steps:
adding the APG modified MBBT composite material into deionized water, dispersing by using a dispersion disc of a sanding dispersion stirring multipurpose machine, dropwise adding a part of dispersing agent into the composite material, switching to a grinding wheel, and dropwise adding the rest dispersing agent while grinding, wherein the weight part of the deionized water is 30-80, the weight part of the APG modified MBBT composite material is 20-70, and the weight part of the dispersing agent is 1-15; and then adding 0.1-5 parts by weight of preservative, and then grinding for 1-3 hours by using a grinding wheel of a sanding dispersion stirring multipurpose machine to prepare the aqueous slurry of the APG modified MBBT compound.
5. The method of preparing an aqueous slurry of an APG-modified MBBT composite according to claim 3, characterized in that: the dispersing agent is any one or a combination of several of methyl ether dimethicone, polyhydroxy stearic acid and lauryl polyglycerol-3 polydimethylsiloxyethyl polydimethylsiloxane.
6. The method of preparing an aqueous slurry of an APG-modified MBBT composite according to claim 3, characterized in that: the preservative is any one or a combination of more of phenoxyethanol, caprylyl glycol, 1,2 pentanediol or 1,2 hexanediol.
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