CN110974715B - APG modified MBBT composite material and preparation method of aqueous slurry thereof - Google Patents

APG modified MBBT composite material and preparation method of aqueous slurry thereof Download PDF

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Publication number
CN110974715B
CN110974715B CN201911369156.6A CN201911369156A CN110974715B CN 110974715 B CN110974715 B CN 110974715B CN 201911369156 A CN201911369156 A CN 201911369156A CN 110974715 B CN110974715 B CN 110974715B
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mbbt
apg
modified
composite material
dispersing
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CN110974715A (en
Inventor
姚超
季金金
左士祥
严向玉
李霞章
刘文杰
吴凤芹
王灿
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Changzhou Nano Materials S&t Co ltd
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Changzhou Nano Materials S&t Co ltd
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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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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

Abstract

The invention discloses an APG modified MBBT composite material and a preparation method of aqueous slurry thereof, and specifically relates to a preparation method of the APG modified MBBT composite material by adding MBBT into APG aqueous solution, heating the system to 50-100 ℃, carrying out reflux reaction for 2-8 hours, and spray drying. Adding the APG modified MBBT composite material into deionized water, adding a dispersing agent in batches, performing dispersion grinding through a sand grinding dispersing and stirring multipurpose machine, adding a preservative, and performing grinding through the sand grinding dispersing and stirring multipurpose machine for 1-3 hours to obtain the aqueous slurry of the APG modified MBBT composite. The method adopts APG to modify MBBT, so that the composite slurry has better moisture retention and better application in cosmetic formulas; but also can better combine MBBT particles with dispersing agents, so that the dispersing effect is better, and the prepared aqueous slurry has better stability and sun protection index.

Description

APG modified MBBT composite material and preparation method of aqueous slurry thereof
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to an APG modified MBBT 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, development and research of various sun-screening cosmetics have become a difficult problem to be solved urgently by cosmetic enterprises in order to protect skin from ultraviolet rays in sunlight. Ultraviolet rays in sunlight which can cause damage to skin are mainly a UVA wave band with the wavelength of 320-400 nm and a UVB wave band 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 sun-screening agent in UVA and UVB wave bands.
Methylene bis-benzotriazole 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 a chromophoric group for absorbing ultraviolet, and ultraviolet shielding is realized by scattering and absorption modes. However, MBBT has poor uv absorption due to its tendency to aggregate in aqueous solutions, and has limited application in the sun protection field. In addition, in the using process of the MBBT, dust is inevitably flying, and the MBBT is harmful to the health of operators and the environmental protection.
Disclosure of Invention
The invention aims to solve the technical problems that: in order to solve the problems of particle agglomeration phenomenon, difficult pushing away, dust pollution and the like of MBBT in the use 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 for solving the technical problems is as follows: an APG modified MBBT composite material is prepared by the following steps: adding MBBT into APG water 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 APG 0810, APG 1214, APG 0814 and APG 1216. The APG is a safe modifier, can be stored for a long time in a larger temperature range, has a moisturizing function, completely meets the performance requirements of active components for cosmetics, and the prepared APG modified MBBT compound has high reliability.
A preparation method of an 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 specific steps are as follows:
adding the APG modified MBBT composite material into deionized water, then dispersing by using a dispersing disc of a sanding dispersing and stirring multipurpose machine, then dripping part of dispersing agent into the dispersing disc, switching to a grinding wheel, and dripping 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; then adding 0.1-5 parts by weight of preservative, and grinding for 1-3 hours by using a sand grinding dispersing and stirring multipurpose machine to prepare the aqueous slurry of the APG modified MBBT compound.
Preferably, the dispersing agent is any one or a combination of several of methyl ethyl ether dimethicone (6011), polyhydroxystearic acid (300R) and lauryl polyglycerol-3-polydimethylsiloxane ethyl polydimethylsiloxane (6105).
Preferably, the preservative is any one or a combination of more than one of phenoxyethanol, octylglycol, 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 cosmetic formulas; but also can better combine MBBT particles with dispersing agent, so that the dispersing effect is better;
2. the method adopts a sand grinding, dispersing and stirring multi-purpose machine to disperse and break up the MBBT particles which are agglomerated by dispersion; the MBBT particles are better dispersed and wetted by the dispersing agent, so that the MBBT particles are stably and uniformly dispersed in the aqueous medium to form a stable composite system, and the sun protection index of the product is greatly improved.
Drawings
FIG. 1 shows the absorbance test results of aqueous slurries of APG-modified MBBT composite materials prepared in examples and comparative examples of the present invention.
Detailed description of the preferred embodiments
The invention will be described in more detail below with reference to examples, but the scope of the invention is not limited to these examples. In the following examples, APG is produced by Shanghai Kaiki chemical Co., ltd, and MBBT is produced by Hubei province Huang Danshi Meifeng chemical industry.
Example 1
The preparation method of the aqueous slurry of the APG modified MBBT composite material comprises the following specific steps:
1. firstly, adding 20g of APG 0814 aqueous solution into a mechanically stirred flask, wherein the water bath temperature is 97 ℃, then adding 100g of MBBT into the flask, stirring and carrying out heat preservation reflux reaction for 2 hours, and finally, carrying out spray drying on the obtained dispersion liquid of the APG modified MBBT, thus obtaining the APG modified MBBT composite material.
2. And then 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 charging barrel of a sanding dispersing and stirring multipurpose machine, pre-dispersing a dispersing disc for 10min at the rotating speed of 2000r/min, dropwise adding part 6011 dispersing agent, and dropwise adding the rest 6011 dispersing agent after the rotating speed of 4000r/min by changing a grinding wheel, so as to prevent a large amount of bubbles possibly generated when the dispersing agent is added at one time, influence the use of slurry, add phenoxyethanol, and grind for 1h, thereby obtaining the aqueous slurry of the APG modified MBBT composite material, namely the dispersing slurry 1. The mass content of each component in the dispersion slurry 1 for short is as follows: 50% of APG modified MBBT composite material, 10% of 6011 dispersing agent, 3% of phenoxyethanol and 100% of deionized water. The quality of 6011 dispersant added in this example was the same for both runs.
Example 2
Preparation of APG modified MBBT composite material: adding 20g of APG 0810 aqueous solution into a flask with mechanical stirring, wherein the water bath temperature is 80 ℃, then adding 140g of MBBT into the flask, stirring, preserving heat and refluxing for reaction for 5 hours, and finally, carrying out spray drying on the obtained dispersion liquid of the APG modified MBBT to obtain the APG modified MBBT composite material;
the aqueous slurry of the APG modified MBBT composite material comprises the following components in percentage by mass: 40% of APG modified MBBT composite material, 4% of 300R dispersing agent, 3% of octyl glycol and the balance of deionized water. The preparation method comprises the following steps:
the deionized water and the APG modified MBBT composite material are weighed and added into a sanding charging barrel of a sanding, dispersing and stirring multipurpose machine, after the dispersion disc is pre-dispersed for 10min at the rotating speed of 2000R/min, 300R dispersing agent with the formula amount of 5/8 is dropwise added, the rest 300R is dropwise added into a grinding wheel at the rotating speed of 4000R/min, octanediol is added, and then the grinding is carried out for 1h, so that the aqueous slurry of the APG modified MBBT composite material, namely the dispersing slurry 2 for short, is obtained.
Example 3
Preparation of APG modified MBBT composite material: 50g of APG 1216 aqueous solution is added into a flask with mechanical stirring, the water bath temperature is 50 ℃, then 150g of MBBT is added into the flask, stirring and heat preservation reflux reaction are carried out for 4 hours, finally, the obtained dispersion liquid of the APG modified MBBT is subjected to spray drying, and the APG modified MBBT composite material is prepared;
aqueous slurry 3 of APG modified MBBT composite: the composition comprises the following components in percentage by mass: 30% of APG modified MBBT composite material, 4% of 6011 dispersing agent, 5% of 1,2 pentanediol and the balance of deionized water.
Deionized water and the compound are weighed and added into a sand milling charging barrel, after the dispersion disc is pre-dispersed for 10min at the rotating speed of 2000r/min, 6011 dispersing agent with the formula amount of 5/8 is dropwise added, the rest 6011 is dropwise added into a grinding wheel at the rotating speed of 4000r/min, 1,2 pentanediol is added, and then the grinding is carried out for 1h, so that the aqueous slurry of the APG modified MBBT composite material, namely the dispersed slurry 3 for short, is obtained.
Example 4
Preparation of APG modified MBBT composite material: adding 30g of APG 1214 aqueous solution into a mechanically stirred flask, 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 dispersion liquid of the APG modified MBBT 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:
deionized water and the compound are weighed and added into a sanding charging barrel, after the dispersion disc is pre-dispersed for 10min at the rotating speed of 2000r/min, 6015 dispersing agent with the formula amount of 1/4 is dropwise added, the grinding wheel is replaced, the rest 6015 dispersing agent is dropwise added at the rotating speed of 4000r/min, 1,2 pentanediol is added, and then the mixture is ground for 1h, so that the aqueous slurry of the APG modified MBBT composite material, namely the dispersed slurry 4 for short, is obtained.
Comparative example 1
The steps for removing the APG modified MBBT of example 1 are as follows:
the aqueous slurry of the APG modified MBBT composite material comprises the following components in parts by weight: MBBT 50%,6011 dispersant 10%, phenoxyethanol 3% and the balance deionized water. The preparation method comprises the following steps:
adding deionized water and MBBT into a sanding charging barrel, pre-dispersing for 10min by a dispersing disc at the rotating speed of 2000r/min, adding 6011 dispersing agent with the formula amount of 1/2, replacing a grinding wheel for grinding, adding the rest 6011 under the condition that the rotating speed is 4000r/min, adding phenoxyethanol, and grinding for 1h to obtain the aqueous slurry of the APG modified MBBT composite material, namely the dispersing slurry 5 for short.
The application effect test of the slurry obtained by the invention:
the aqueous slurries of the APG-modified MBBT composites prepared in examples 1 to 4 and comparative example 1 were respectively added with deionized water to prepare 50ppm dispersions, and after ultrasonic dispersion for 30 minutes, the absorbance of light was measured on an ultraviolet-visible near infrared spectrophotometer (UV 3600, shimadzu corporation) with a 1cm quartz cuvette as a reference with deionized water. The experimental results are shown in fig. 1. As can be seen from the graph, the dispersion slurry prepared by the invention has excellent full-wave band ultraviolet blocking effect and strong shielding capability on UVA and UVB.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme and the concept of the present invention, and should be covered by the scope of the present invention.

Claims (2)

  1. The preparation method of the aqueous slurry of the APG modified MBBT composite material is characterized by comprising the following steps of: the method comprises the following specific steps:
    adding the APG modified MBBT composite material into deionized water, then dispersing by using a dispersing disc of a sand grinding dispersing and stirring multipurpose machine, then dripping part 6011 dispersing agent into the dispersing disc, switching to a grinding wheel, and dripping the rest 6011 dispersing agent while grinding; then adding a preservative, and grinding for 1-3 hours by using a grinding wheel of a sand grinding, dispersing and stirring multipurpose machine to prepare aqueous slurry of the APG modified MBBT compound, wherein the mass content of each component in the slurry is as follows: 50% of APG modified MBBT composite material, 10% of 6011 dispersing agent, 3% of preservative and the balance of deionized water;
    the APG modified MBBT composite material is prepared by the following method: adding MBBT into APG water solution, heating the system to 97 ℃, carrying out reflux reaction for 2 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 5:1;
    the APG is selected as APG 0814.
  2. 2. The method for preparing the aqueous slurry of the APG modified MBBT composite material according to claim 1, characterized in that: the preservative is any one or the combination of more of phenoxyethanol, octylglycol, 1, 2-pentanediol or 1, 2-hexanediol.
CN201911369156.6A 2019-12-26 2019-12-26 APG modified MBBT composite material and preparation method of aqueous slurry thereof Active CN110974715B (en)

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CN108464947A (en) * 2018-04-12 2018-08-31 苏州绿叶日用品有限公司 Include the cosmetic composition and preparation method thereof of film forming agent and microsphere particle
CN109453064A (en) * 2018-12-10 2019-03-12 苏州绿叶日用品有限公司 The frangible cosmetic composition and preparation method thereof removed of the anti-sweat warm water of waterproof
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