CN113768817A - Preparation method of nano-diamond makeup product - Google Patents

Preparation method of nano-diamond makeup product Download PDF

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Publication number
CN113768817A
CN113768817A CN202111163508.XA CN202111163508A CN113768817A CN 113768817 A CN113768817 A CN 113768817A CN 202111163508 A CN202111163508 A CN 202111163508A CN 113768817 A CN113768817 A CN 113768817A
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Prior art keywords
diamond
nano
beaker
atmosphere
temperature
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CN202111163508.XA
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Inventor
栗正新
张鹏
陈冰威
黄雷波
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Henan University of Technology
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Henan University of Technology
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Priority to CN202111163508.XA priority Critical patent/CN113768817A/en
Publication of CN113768817A publication Critical patent/CN113768817A/en
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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
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • 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
    • A61K8/67—Vitamins
    • A61K8/676—Ascorbic acid, i.e. vitamin C
    • 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
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/25—Diamond
    • C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
    • 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
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/413—Nanosized, i.e. having sizes below 100 nm
    • 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
    • A61K2800/592—Mixtures of compounds complementing their respective functions

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Veterinary Medicine (AREA)
  • Nanotechnology (AREA)
  • Public Health (AREA)
  • Epidemiology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Dermatology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Birds (AREA)
  • Composite Materials (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Cosmetics (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a preparation method of a nano-diamond makeup product, belonging to the field of diamond application. The main process comprises the steps of strong acid treatment of the nano-diamond and N2The method comprises four parts of atmosphere vacuum heat treatment, surface functionalization treatment of the nano-diamond and combination of the nano-diamond and vitamin C. The invention has simple operation, and the product has low toxicity, biocompatibility and chemical inertnessThe nano diamond can be combined with the skin surface, reduce the water loss through skin, influence the functions of the water and lipid skin surface and protect the skin from aging.

Description

Preparation method of nano-diamond makeup product
Technical Field
The invention relates to the field of diamond application, in particular to a preparation method of a nano-diamond makeup product.
Background
The development of diamond has been greatly improved from the discovery of diamond use to the synthesis of synthetic diamond, especially the artificial synthesis of diamond in our country, and many synthetic methods of diamond have provided a solid foundation for the application and research of diamond in the past for a long time. The nano-diamond is distinguished from other materials by virtue of excellent properties such as low toxicity, biocompatibility, larger specific surface area and the like, attracts the attention of many researchers, carries out deep research on the nano-diamond, carries out surface modification and modification on the nano-diamond, and further gradually carries out research combined with biomacromolecules.
Currently, nanodiamonds are widely used in the field of fine chemical engineering by virtue of their excellent physicochemical properties, and in particular, in skin care products, nanodiamonds are gradually used by researchers due to low toxicity and biocompatibility. Currently, there are hundreds of cosmetic products containing nanodiamond. However, as the research progresses, some problems are exposed, for example, the nano-diamond has a high specific surface energy, a large specific surface area, and is in a thermodynamically unstable state, and in addition, the surface activity of the nano-diamond is also large, and thus the agglomeration phenomenon between particles often occurs. Therefore, it is a major focus of current research on how to solve the agglomeration of the nano-diamond particles and effectively treat the surfaces of the nano-diamond particles to exert the excellent properties of the nano-diamond. Because the nano-diamond has incomparably excellent performances of other materials, the nano-diamond has a wide application prospect, particularly in the aspect of biomedicine, in recent years, the nano-diamond is considered to be a suitable carrier of a medicament for improving skin diseases, and various functional groups on the surface of the nano-diamond can be combined in a chemical bond mode for cancer diagnosis and treatment medicaments, and the nano-diamond becomes one of the main targets of the current cancer medicament research. In addition, the nano-diamond can improve the durability and stability of the drug and disperse the drug which is not dissolved in water. Also, since nanodiamonds have a large surface area, particles are loaded with a large amount of therapeutic agents, and thus, nanodiamonds are gradually applied to the field of fine chemical engineering, particularly in cosmetics and health products.
In the field of nano-diamond impregnated cosmetics, because of its good absorption properties, it can be formulated into a variety of skin care products, such as face washes, soaps, etc. There are now hundreds of cosmetic products on the market that contain nanodiamonds. Moreover, experiments show that the nano diamond can be combined with the skin surface, reduce the water loss in the skin, influence the functions of the water and lipid skin surface and protect the skin from aging. The nano-diamond has great potential in the aspect of ultraviolet protection, namely sunscreen cream due to unique optical properties. Therefore, nanodiamonds have been widely popular in cosmetics due to the properties of biocompatibility and low toxicity.
Disclosure of Invention
The invention aims to: the nano-diamond is subjected to strong acid treatment by adopting a water bath heating mode, so that the nano-diamond can be uniformly heated, and the nano-diamond can be subjected to dispersion treatment to a certain degree. And N is2The heat treatment is carried out under high temperature and vacuum, the dispersibility of the nano-diamond can be improved, and the nano-diamond is N2Under the protection of atmosphere, the nano-diamond can isolate water molecules in the air, and meanwhile impurities are prevented from being generated, but the biggest effect of the nano-diamond is to remove hydroxyl groups and other groups on the surface of the nano-diamond. The nano-diamond treated by strong acid has good effect when being combined with vitamin C, and has certain effect on whitening.
Technical scheme
In order to realize the purpose of the invention, the following technical scheme is adopted for realizing the purpose:
a. the strong acid treatment of the nano-diamond comprises the following specific steps: uniformly mixing the nano-diamond with concentrated nitric acid, carrying out strong acid treatment, and washing and drying the treated nano-diamond for later use;
b. the N2 atmosphere vacuum heat treatment comprises the following specific steps: putting the treated nano-diamond into a crucible, putting the crucible into a vacuum tube furnace, vacuumizing, filling nitrogen atmosphere, and performing heat treatment: heating at a heating rate of 10 ℃/min to 20 ℃/min, keeping the temperature constant for 2 hours when the temperature reaches 600 ℃ to 800 ℃, cooling to 200 ℃ without closing the atmosphere after keeping the temperature, opening the vacuum tube furnace, closing the atmosphere, and naturally cooling to room temperature;
c. the surface functionalization treatment of the nano diamond comprises the following specific processes: adding the nano-diamond subjected to high-temperature nitrogen heat treatment into a small dry clean beaker, adding concentrated hydrochloric acid, completely immersing the nano-diamond by the addition of the concentrated acid in the beaker, uniformly stirring, standing for 24h to 26h, pouring the upper layer acid solution into a waste liquid barrel, leaving the lower layer of nano-diamond powder, cleaning with deionized water until the pH value is about 7, repeating the operation for more than three times, and drying the obtained nano-diamond in a drying oven;
d. the specific process of combining the nano-diamond with the vitamin C is as follows: placing the nano-diamond with the functionalized surface in a dry and clean beaker, adding vitamin C liquid into the beaker, completely soaking the nano-diamond, uniformly mixing, standing for 2 to 4 hours, cleaning with deionized water, then placing the lower layer nano-diamond powder layer in a drying oven, drying at 110 ℃ for 2 to 4 hours, and taking out.
The preferred process of strong acid treatment in step a of the present invention is: 1.5g of nano-diamond is taken, and 10ml to 20ml of concentrated HNO is taken3Slowly pouring into a beaker, uniformly mixing, and heating for 2 to 4 hours at a temperature of between 80 and 100 ℃.
The preferable washing and drying process in the step a of the invention comprises the following steps: and pouring the supernatant in the beaker into a waste liquid barrel, placing the beaker containing the nano-diamond sediments in a ventilated place, cooling to room temperature, and standing for 18-24 h.
The invention has the beneficial effects that:
1. the nano-diamond is subjected to strong acid treatment in a water bath heating mode, so that the nano-diamond can be uniformly heated, and the nano-diamond can be subjected to dispersion treatment to a certain degree;
2. and N is2The heat treatment is carried out under high temperature and vacuum, the dispersibility of the nano-diamond can be improved, and the nano-diamond is N2Under the protection of atmosphere, the nano-diamond can isolate water molecules in the air and simultaneously avoid the generation of impurities, but the maximum effect of the nano-diamond is to remove hydroxyl groups and other groups on the surface of the nano-diamond;
3. the nano-diamond treated by strong acid has good effect when being combined with vitamin C, and has certain effect on whitening.
Detailed Description
The invention is further described below with reference to specific examples:
example 1:
a. 1.5g of nano-diamond is taken, and 10ml of concentrated HNO is taken3Slowly pouring into a beaker, uniformly mixing, heating at 80 ℃ for 2h, pouring supernatant in the beaker into a waste liquid barrel, placing the beaker containing the nano-diamond sediments in a ventilated place, cooling to room temperature, and standing for 18 h;
b. putting the treated nano-diamond into a crucible, putting the crucible into a vacuum tube furnace, vacuumizing, filling nitrogen atmosphere, and performing heat treatment: heating at a heating rate of 10 ℃/min, keeping the temperature at 600 ℃ for 2h, cooling to 200 ℃ without closing the atmosphere after keeping the temperature, opening the vacuum tube furnace, closing the atmosphere, and naturally cooling to room temperature;
c. adding the nano-diamond subjected to high-temperature nitrogen heat treatment into a small dry clean beaker, adding concentrated hydrochloric acid, completely immersing the nano-diamond by the addition of the concentrated acid in the beaker, uniformly stirring, standing for 24h, pouring the upper layer acid solution into a waste liquid barrel, leaving the lower layer of nano-diamond powder, cleaning with deionized water until the pH value is about 7, repeating the operation for more than three times, and drying the obtained nano-diamond in a drying oven;
d. placing the surface-functionalized nano-diamond in a dry and clean beaker, adding 5ml of vitamin C liquid into the beaker, completely soaking the nano-diamond, uniformly mixing, standing for 2 hours, cleaning with deionized water, then placing the lower nano-diamond powder layer in a drying oven, drying at 110 ℃ for 2 hours, and taking out.
Example 2:
a. taking 1.5g of nano-diamond and taking 15ml of concentrated HNO3Slowly pouring into a beaker, uniformly mixing, heating at 90 ℃ for 3h, pouring supernatant in the beaker into a waste liquid barrel, placing the beaker containing the nano-diamond sediments in a ventilated place, cooling to room temperature, and standing for 20 h;
b. putting the treated nano-diamond into a crucible, putting the crucible into a vacuum tube furnace, vacuumizing, filling nitrogen atmosphere, and performing heat treatment: heating at a heating rate of 15 ℃/min, keeping the temperature at 700 ℃ for 2h, cooling to 200 ℃ without closing the atmosphere after keeping the temperature, opening the vacuum tube furnace, closing the atmosphere, and naturally cooling to room temperature;
c. adding the nano-diamond subjected to high-temperature nitrogen heat treatment into a small dry clean beaker, adding concentrated hydrochloric acid, completely immersing the nano-diamond in the amount of the concentrated acid in the beaker, uniformly stirring, standing for 25h, pouring the upper layer acid solution into a waste liquid barrel, leaving the lower layer of nano-diamond powder, cleaning with deionized water until the pH value is about 7, repeating the operation for more than three times, and drying the obtained nano-diamond in a drying oven;
d. placing the surface-functionalized nano-diamond in a dry and clean beaker, adding 10ml of vitamin C liquid into the beaker, completely soaking the nano-diamond, uniformly mixing, standing for 3 hours, cleaning with deionized water, then placing the lower nano-diamond powder layer into a drying oven, drying at 110 ℃ for 3 hours, and taking out.
Example 3:
a. 1.5g of nano-diamond is taken, and 20ml of concentrated HNO is taken3Slowly pouring into a beaker, uniformly mixing, heating at 100 ℃ for 4h, pouring supernatant in the beaker into a waste liquid barrel, placing the beaker containing the nano-diamond sediments in a ventilated place, cooling to room temperature, and standing for 24 h;
b. putting the treated nano-diamond into a crucible, putting the crucible into a vacuum tube furnace, vacuumizing, filling nitrogen atmosphere, and performing heat treatment: heating at a heating rate of 20 ℃/min, keeping the temperature at 800 ℃ for 2h, cooling to 200 ℃ without closing the atmosphere after keeping the temperature, opening the vacuum tube furnace, closing the atmosphere, and naturally cooling to room temperature;
c. adding the nano-diamond subjected to high-temperature nitrogen heat treatment into a small dry clean beaker, adding concentrated hydrochloric acid, completely immersing the nano-diamond in the amount of the concentrated acid in the beaker, uniformly stirring, standing for 26h, pouring the upper layer acid solution into a waste liquid barrel, leaving the lower layer of nano-diamond powder, cleaning with deionized water until the pH value is about 7, repeating the operation for more than three times, and drying the obtained nano-diamond in a drying oven;
d. placing the surface-functionalized nano-diamond in a dry and clean beaker, adding 15ml of vitamin C liquid into the beaker, completely soaking the nano-diamond, uniformly mixing, standing for 4 hours, cleaning with deionized water, then placing the lower nano-diamond powder layer in a drying oven, drying at 110 ℃ for 4 hours, and taking out.

Claims (2)

1. A method for etching a diamond monocrystal is characterized by comprising the following steps:
a. the strong acid treatment of the nano-diamond comprises the following specific steps: uniformly mixing the nano-diamond with concentrated nitric acid, carrying out strong acid treatment, and washing and drying the treated nano-diamond for later use;
b. the N2 atmosphere vacuum heat treatment comprises the following specific steps: putting the treated nano-diamond into a crucible, putting the crucible into a vacuum tube furnace, vacuumizing, filling nitrogen atmosphere, and performing heat treatment: heating at a heating rate of 10 ℃/min to 20 ℃/min, keeping the temperature constant for 2 hours when the temperature reaches 600 ℃ to 800 ℃, cooling to 200 ℃ without closing the atmosphere after keeping the temperature, opening the vacuum tube furnace, closing the atmosphere, and naturally cooling to room temperature;
c. the surface functionalization treatment of the nano diamond comprises the following specific processes: adding the nano-diamond subjected to high-temperature nitrogen heat treatment into a small dry clean beaker, adding concentrated hydrochloric acid, completely immersing the nano-diamond by the addition of the concentrated acid in the beaker, uniformly stirring, standing for 24h to 26h, pouring the upper layer acid solution into a waste liquid barrel, leaving the lower layer of nano-diamond powder, cleaning with deionized water until the pH value is about 7, repeating the operation for more than three times, and drying the obtained nano-diamond in a drying oven;
d. the specific process of combining the nano-diamond with the vitamin C is as follows: placing the nano-diamond with the functionalized surface in a dry and clean beaker, adding vitamin C liquid into the beaker, completely soaking the nano-diamond, uniformly mixing, standing for 2 to 4 hours, cleaning with deionized water, then placing the lower layer nano-diamond powder layer in a drying oven, drying at 110 ℃ for 2 to 4 hours, and taking out.
2. The production method according to claim 1, characterized in that: the specific step in the step a is to take 1.5g sodiumTaking 10ml to 20ml of concentrated HNO3Slowly pouring into a beaker, uniformly mixing, heating at 80-100 ℃ for 2-4 h, pouring supernatant in the beaker into a waste liquid barrel, placing the beaker containing the nano-diamond sediments in a ventilated place, cooling to room temperature, and standing for 18-24 h.
CN202111163508.XA 2021-09-30 2021-09-30 Preparation method of nano-diamond makeup product Pending CN113768817A (en)

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Application Number Priority Date Filing Date Title
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101821196A (en) * 2007-10-13 2010-09-01 纳米金刚石有限公司 Nanodiamond compounds synthesized by surface functionalization
CN103146230A (en) * 2013-02-08 2013-06-12 浣石 Nanodiamond derivative having hydroxy groups as terminal groups, and preparation method and use thereof
CN104529527A (en) * 2014-12-15 2015-04-22 湖南大学 Method for increasing surface roughness of man-made diamond single crystal
CN107929242A (en) * 2017-11-26 2018-04-20 郑州大学 Pharmaceutical carrier, drug composite based on Nano diamond and its preparation method and application
CN111778718A (en) * 2020-07-28 2020-10-16 河北工业大学 Preparation method of nano-diamond modified carbon fiber

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101821196A (en) * 2007-10-13 2010-09-01 纳米金刚石有限公司 Nanodiamond compounds synthesized by surface functionalization
CN103146230A (en) * 2013-02-08 2013-06-12 浣石 Nanodiamond derivative having hydroxy groups as terminal groups, and preparation method and use thereof
CN104529527A (en) * 2014-12-15 2015-04-22 湖南大学 Method for increasing surface roughness of man-made diamond single crystal
CN107929242A (en) * 2017-11-26 2018-04-20 郑州大学 Pharmaceutical carrier, drug composite based on Nano diamond and its preparation method and application
CN111778718A (en) * 2020-07-28 2020-10-16 河北工业大学 Preparation method of nano-diamond modified carbon fiber

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
孙陶利等: "纳米金刚石材料在生物医药领域中的应用", 《中国生物医学工程学报》 *
王芬芬等: "纳米金刚石表面修饰工艺研究", 《超硬材料工程》 *
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邓福铭等: "纳米金刚石表面改性处理及表面结构表征", 《金刚石与磨料磨具工程》 *

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