CN111003714B - Modification method of attapulgite clay for cosmetics - Google Patents
Modification method of attapulgite clay for cosmetics Download PDFInfo
- Publication number
- CN111003714B CN111003714B CN201911416417.5A CN201911416417A CN111003714B CN 111003714 B CN111003714 B CN 111003714B CN 201911416417 A CN201911416417 A CN 201911416417A CN 111003714 B CN111003714 B CN 111003714B
- Authority
- CN
- China
- Prior art keywords
- attapulgite
- slurry
- cosmetics
- purified
- stirring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- 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
- A61K8/25—Silicon; Compounds thereof
-
- 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
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Dermatology (AREA)
- Dispersion Chemistry (AREA)
- Cosmetics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a modification method of attapulgite clay for cosmetics, which comprises the steps of crushing and drying attapulgite raw ores, preparing dry particles into slurry with the mass fraction of 5-20%, stirring, ultrasonic dispersing, sieving with a 1200-mesh sieve for separation, and concentrating filtrate to obtain slurry with the water content of 50-75%; adding egg white into the slurry, stirring for 15-40 min at 2-10 ℃, and introducing ammonia gas to float the foam containing the attapulgite; collecting floating foam, adding citric acid to defoam, centrifuging, and washing to obtain purified attapulgite; and (3) uniformly mixing the purified attapulgite and D-glucuronic acid in water, refluxing for 15-30 hours at 60-100 ℃, centrifuging, washing and drying to obtain the modified attapulgite. The attapulgite modified by D-glucuronic acid is stable, has good adsorption and moisture retention properties, can effectively reduce the content of preservative in cosmetics, increase the content of trace elements in cosmetics, improve air permeability and has universality in the field of cosmetics.
Description
Technical Field
The invention relates to a modification method of attapulgite clay, in particular to a modification method of attapulgite clay for cosmetics, and belongs to the technical field of material treatment.
Background
Attapulgite, also known as palygorskite, has the name of "Qianzhen Wang" and "Universal soil" and has special application in industry and other various industries. Because attapulgite is found early, the attapulgite is widely used in various fields of agriculture, medicine, petrochemical industry, drilling, construction, nuclear industry, food, environmental protection, silicate industry and other departments. The method is mainly produced in three provinces of Su, anhui and Gansu, and finds out that the palygorskite resource amount reaches 6000 ten thousand tons for nine production areas of Su and Anhui by the end of 2001. Gansu, inner Mongolia, hebei, qinghai, sichuan, shanxi, xinjiang, guizhou and other provinces are distributed, and Gansu is the region with the most concentrated northwest reserves.
However, most of attapulgite ores in Gansu province are low-grade minerals with the content of less than 30%, which brings great difficulty to the application of the attapulgite, besides the attapulgite, quartz in Gansu province has the content of more than 50%, calcium carbonate has the content of more than 15%, and a large amount of ferric oxide, montmorillonite and the like are also present. If only products with low added values such as soil conditioner, cat litter, haydite and the like are prepared, the waste of the rare resources is caused, but if the products are not subjected to fine purification, the products can not be used in the fields with high added values such as medicines, cosmetics, foods and the like. Therefore, the method is particularly important for purifying the low-grade attapulgite clay mineral.
Among the applications, the application of attapulgite to cosmetics is one of the very promising fields, and not only has large demand but also has considerable price. In the cosmetics, the purity of the attapulgite is required to be at least more than 99.5%, the surface of the attapulgite serving as an inorganic substance is required to be organically modified, and the modified material is not only harmless to the body, but also is better fused with other substances in the cosmetics, thereby being beneficial to the skin.
Disclosure of Invention
The invention aims to provide a modification method of attapulgite clay for cosmetics.
1. Modification of attapulgite clay for cosmetics
The modification method of the attapulgite clay for cosmetics comprises the following process steps:
(1) Crushing attapulgite raw ore into small particles with the size of 2-5 cm, naturally airing or manually heating and dehydrating to constant weight;
(2) Preparing the dry particles obtained in the step (1) into slurry with the mass fraction of 5-20%, stirring, performing ultrasonic dispersion, sieving with a 1200-mesh sieve, separating, and concentrating the filtrate to obtain slurry with the water content of 50-75%. Wherein the stirring time is 20-60 min; the ultrasonic dispersion time is 15-45 min;
(3) Adding egg white into the slurry obtained in the step (2), stirring for 15-40 min at 2-10 ℃, and introducing ammonia gas to float the foam containing the attapulgite; the addition amount of egg white is 5-20% of the mass of the slurry;
(4) Collecting the floating foam obtained in the step (3), adding citric acid to defoam, centrifuging, and washing to obtain purified attapulgite; the addition amount of the citric acid is 1-10% of the mass of the slurry;
(5) And (3) uniformly mixing the purified attapulgite and D-glucuronic acid (DGA) in water, refluxing for 15-30 hours at 60-100 ℃, centrifuging, washing and drying to obtain the modified attapulgite, wherein the modified attapulgite is marked as DGA-ATG. The mass ratio of the purified attapulgite to the DGA is 1:0.1-1:1;
2. structural Properties of attapulgite clay for cosmetic
FIG. 1 is an XRD profile of purified attapulgite. The purity of the purified attapulgite is higher than 92.5 percent. As can be seen from FIG. 1, the purified attapulgite contains negligible amounts of other substances, and all of the substances are absorption peaks of the attapulgite clay.
FIG. 2 is a scanning electron microscope image of an attapulgite crude ore (a) and a purified attapulgite (b). Fig. 2 (a) is a scanning electron microscope image of an attapulgite crude ore, and it can be seen that a large amount of impurities are contained therein, and the purified attapulgite crude ore is obtained after purification to obtain fig. 2 (b), and it can be seen from the image that the purified attapulgite is free of other impurities by the combined action of egg white and ammonia.
FIG. 3 is a DGA-ATG infrared spectrum. As can be seen from the figure, organic matters in DGA molecules are grafted on the surface of the attapulgite, and 2920 cm -1 And 2850 cm -1 The peaks at the two positions are C-H stretching vibration, and the characteristic peaks of DGA are also arranged in the fingerprint area.
Fig. 4 and 5 are respectively DGA-ATG scanning electron microscope images and ESD analysis. As can be seen from a scanning electron microscope photograph (figure 4), the rod crystal of the attapulgite is shortened, the diameter of the rod crystal is thickened, but the basic rod-shaped morphology of the attapulgite is not changed. Table 1 shows the EDS element content analysis data of DGA-ATG. As can be seen from Table 1, the content of element C on the surface of the attapulgite is very high, indicating that DGA is successfully grafted onto the surface of the attapulgite.
Adsorption performance test: in the invention, the modified attapulgite is used for carrying out an adsorption experiment on lead ions and methylene blue wastewater, and the specific experimental process is as follows: respectively taking 15 mg of the modified attapulgite prepared by the invention, adding purified attapulgite and attapulgite raw ore into a 50 mL iodine flask, adding 15 mL solution (pH=7), and putting into a constant temperature water bath oscillator for oscillation at 30 ℃ and 160 rpm. The initial concentration of methylene blue in the solution was 800 mg/L and the concentration of lead ions was 100 mg/L.
Water retention test: 100 g of the modified attapulgite, purified attapulgite and attapulgite raw ore powder prepared by the method are respectively taken, wrapped by a 600-mesh screen, immersed in tap water to fully absorb water for 5 hours, then taken out and placed until no water drops ooze out, three saturated water-absorbing clays are placed in a 500mL beaker, dried at 40 ℃ and tested for the time of losing 50% of water.
From the above table, the adsorption capacity of the modified attapulgite clay to methylene blue and lead ions is greatly improved, and the time for losing 50% of water is also obviously improved, which proves that the modified attapulgite clay has good adsorption capacity to methylene blue and lead ions and good water retention property.
In conclusion, the purified attapulgite is obtained through the combined action of egg white and ammonia, the DGA which is friendly to the skin is combined on the surface of the purified attapulgite through the non-covalent bond acting force, and the DGA modified attapulgite is stable and has good adsorption and moisture retention properties; the modified attapulgite can be used in cosmetics to effectively reduce the content of preservative, increase the content of trace elements in the cosmetics, improve the air permeability, and be healthier and more friendly to human body, and has universality in the field of cosmetics, and can be used in fine chemicals such as lipstick, eye shadow, cleansing water, facial cleanser, shampoo, hair dye, blush, lipstick, make-up powder, mascara, eyeliner and the like.
Drawings
FIG. 1 is an XRD profile of purified attapulgite clay;
FIG. 2 is a scanning electron micrograph of an attapulgite crude ore (a) and a purified attapulgite (b);
FIG. 3 is an infrared spectrum of DGA-ATG;
FIG. 4 is a scanning electron microscope image of DGA-ATG;
FIG. 5 is an EDS analysis of DGA-ATG.
Detailed Description
The method for modifying the attapulgite clay for cosmetics and the properties of the modified attapulgite clay according to the present invention are described in detail by way of specific examples.
Example 1
(1) Crushing attapulgite raw ore into small particles with the size of 2-5 cm, naturally airing or manually heating and dehydrating to constant weight;
(2) Weighing 100 g of the dry particles obtained in the step (1), adding into 900 mL of water, preparing into slurry with the mass fraction of 10%, stirring at high speed (3000 r/min) for 50min, performing ultrasonic dispersion for 30min, sieving with 1200 meshes for separation, and concentrating the filtrate to obtain slurry with the water content of 70%;
(3) Adding 10 g egg white into the slurry (100 g) prepared in the step (2), stirring at 2 ℃ for 30min, and introducing ammonia gas to float the attapulgite-containing foam;
(4) Collecting the floating foam obtained in the step (3), adding 1 g citric acid to defoam, centrifuging, and washing to obtain purified attapulgite with the purity of 93.5%;
(5) Modification of attapulgite: weighing 100 g purified attapulgite and 10 g D-glucuronic acid, adding into water, mixing well, refluxing at 80deg.C for 24 hr, centrifuging, washing, and drying to obtain modified attapulgite;
(6) Performance of modified attapulgite: the adsorption rate for methylene blue was 97.9%, the adsorption rate for lead ions was 96.7%, and the time to lose 50% of the water was 10.4 hours.
Example 2
(1) Crushing attapulgite raw ore into small particles with the size of 2-5 cm, naturally airing or manually heating and dehydrating to constant weight;
(2) Weighing 100 g of the dry particles obtained in the step (1), adding the dry particles into 1900 mL of water, preparing slurry with the mass fraction of 5%, stirring at a high speed (4000 r/min) for 50min, performing ultrasonic dispersion for 30min, sieving with a 1200-mesh sieve, separating, and concentrating the filtrate to obtain slurry with the water content of 50%;
(3) Adding 5 g egg white into the slurry (100 g) prepared in the step (2), stirring at 10 ℃ for 15 min, and introducing ammonia gas to float the attapulgite-containing foam;
(4) Collecting the floating foam obtained in the step (3), adding 10 g citric acid to defoam, centrifuging, and washing to obtain purified attapulgite with the purity of 97.5%;
(5) Modification of attapulgite: weighing 100 g purified attapulgite and 100 g D-glucuronic acid, adding into water, mixing well, refluxing at 60deg.C for 15 hr, centrifuging, washing, and drying to obtain modified attapulgite;
(6) Performance of modified attapulgite: the adsorption rate for methylene blue was 98.6%, the adsorption rate for lead ions was 97.4%, and the time to lose 50% of the water was 11.2 hours.
Example 3
(1) Crushing attapulgite raw ore into small particles with the size of 2-5 cm, naturally airing or manually heating and dehydrating to constant weight;
(2) Weighing 100 g of the dry particles obtained in the step (1), adding the dry particles into 400 mL of water, preparing slurry with the mass fraction of 20%, stirring at a high speed (2000 r/min) for 50min, performing ultrasonic dispersion for 30min, sieving with a 1200-mesh sieve, separating, and concentrating the filtrate to obtain slurry with the water content of 75%;
(3) Adding 20 g egg white into the slurry (100 g) prepared in the step (2), stirring at 8 ℃ for 45min, and introducing ammonia gas to float the attapulgite-containing foam;
(4) Collecting the floating foam obtained in the step (3), adding 5 g citric acid to defoam, centrifuging, and washing to obtain purified attapulgite with the purity of 94.5%;
(5) Modification of attapulgite: weighing 100 g purified attapulgite and 50 g D-glucuronic acid, adding into water, mixing well, refluxing at 100deg.C for 30 hr, centrifuging, washing, and drying to obtain modified attapulgite;
(6) Performance of modified attapulgite: the adsorption rate for methylene blue was 99.1%, the adsorption rate for lead ions was 98.9%, and the time to lose 50% of the water was 12 hours.
Claims (5)
1. A modification method of attapulgite clay for cosmetics comprises the following process steps:
(1) Crushing attapulgite raw ore into small particles with the size of 2-5 cm, naturally airing or manually heating and dehydrating to constant weight;
(2) Preparing the dry particles obtained in the step (1) into slurry with the mass fraction of 5-20%, stirring, performing ultrasonic dispersion, sieving with a 1200-mesh sieve, separating, and concentrating filtrate to obtain slurry with the water content of 50-75%;
(3) Adding egg white into the slurry obtained in the step (2), stirring for 15-40 min at 2-10 ℃, and introducing ammonia gas to float the foam containing the attapulgite;
(4) Collecting the floating foam obtained in the step (3), adding citric acid to defoam, centrifuging, and washing to obtain purified attapulgite;
(5) And (3) uniformly mixing the purified attapulgite and D-glucuronic acid in water, refluxing for 15-30 hours at 60-100 ℃, centrifuging, washing and drying to obtain the modified attapulgite.
2. The method for purifying attapulgite clay according to claim 1, wherein: in the step (2), stirring time is 20-60 min; the ultrasonic dispersion time is 15-45 min.
3. The method for purifying attapulgite clay according to claim 1, wherein: in the step (3), the addition amount of egg white is 5-20% of the mass of the slurry.
4. The method for purifying attapulgite clay according to claim 1, wherein: in the step (4), the addition amount of the citric acid is 1-10% of the mass of the slurry.
5. The method for modifying attapulgite clay according to claim 1, wherein the method comprises the steps of: in the step (5), the mass ratio of the purified attapulgite to the D-glucuronic acid is 1:0.1-1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911416417.5A CN111003714B (en) | 2019-12-31 | 2019-12-31 | Modification method of attapulgite clay for cosmetics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911416417.5A CN111003714B (en) | 2019-12-31 | 2019-12-31 | Modification method of attapulgite clay for cosmetics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111003714A CN111003714A (en) | 2020-04-14 |
| CN111003714B true CN111003714B (en) | 2023-04-25 |
Family
ID=70120104
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911416417.5A Active CN111003714B (en) | 2019-12-31 | 2019-12-31 | Modification method of attapulgite clay for cosmetics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111003714B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113208951B (en) * | 2021-05-17 | 2022-05-27 | 西北师范大学 | Butter modified attapulgite and application thereof in preparation of lipstick |
| CN115215350B (en) * | 2022-08-05 | 2023-10-13 | 西北师范大学 | Method for purifying attapulgite clay and attapulgite-based mineralized water agent |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2203009A1 (en) * | 1994-10-18 | 1996-04-25 | Malireddy S. Reddy | Odor inhibiting pet litter |
| FR2862222B1 (en) * | 2003-11-18 | 2008-10-10 | Oreal | COSMETIC COMPOSITION COMPRISING GELLANE GUM OR ONE OF ITS DERIVATIVES, A SOLID COMPOUND AND A MONOVALENT SALT, METHODS USING THE SAME, AND USES THEREOF |
| ATE523248T1 (en) * | 2007-03-21 | 2011-09-15 | Omya Development Ag | SURFACE TREATED CALCIUM CARBONATE AND USE THEREOF FOR WASTEWATER TREATMENT |
| EP2025364A1 (en) * | 2007-08-13 | 2009-02-18 | Procter & Gamble International Operations SA. | Compositions comprising dye-loaded particles |
| US8728230B2 (en) * | 2010-03-15 | 2014-05-20 | Ciments Francais | Temperature-stable liquid aqueous polysaccharide suspensions and use thereof as thickening agents in cementitious compositions |
| CN108498354A (en) * | 2018-05-23 | 2018-09-07 | 佛山市汇汾化妆品科技有限公司 | A kind of sepiolite absorption facial cleanser and preparation method thereof |
| CN109127150B (en) * | 2018-09-10 | 2020-09-15 | 西安建筑科技大学 | Method for inhibiting copper activation blende by whey protein |
| CN110092386B (en) * | 2019-05-07 | 2021-02-05 | 西北师范大学 | Method for purifying attapulgite clay |
-
2019
- 2019-12-31 CN CN201911416417.5A patent/CN111003714B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111003714A (en) | 2020-04-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111003714B (en) | Modification method of attapulgite clay for cosmetics | |
| CN106010601A (en) | Biochar prepared from banana peel, preparation method and application thereof | |
| CN103933936B (en) | A kind of preparation method and application of antibiotic compound adsorbent | |
| CN109534432A (en) | The preparation method of the biological carbon modified material of phosphorus in a kind of removal eutrophication water | |
| Silva et al. | Microwave-assisted alginate extraction from Portuguese Saccorhiza polyschides–influence of acid pretreatment | |
| CN104888705A (en) | Preparation method of magnetic ferric oxide/bagasse active carbon | |
| CN110142032B (en) | Chitosan biochar composite material and preparation method and application thereof | |
| CN107282001B (en) | Preparation and application method of polyaluminium chloride modified graphene oxide adsorbent | |
| CN107583609A (en) | A kind of modified mangosteen shell charcoal and the method using vanadium in its reduction water body | |
| CN113683095B (en) | Method for purifying natural sodium bentonite containing cristobalite | |
| CN104261421A (en) | Hydrothermal method for preparing creamy white attapulgite | |
| CN103506066A (en) | Novel mineral silicon dioxide desiccant powder and preparation method thereof | |
| CN104759252A (en) | A method of preparing porous carbon by adopting spherical zinc oxide as a template and applications of the porous carbon | |
| CN108722359A (en) | A kind of preparation method that carboxymethyl chitosan is modified montmorillonite used | |
| CN106890618A (en) | A kind of preparation method of attapulgite ore drier | |
| CN107597059A (en) | The preparation method of modified microplate stratiform feature feather charcoal before a kind of hydro-thermal soda acid | |
| CN108579628A (en) | A kind of kappa-carrageenan/graphene oxide gel bead and its preparation method and application | |
| CN114871198A (en) | Method for extracting uniaxial siliceous spongy spicules | |
| CN112011066B (en) | Production process of high-purity humic acid | |
| Fang et al. | Adsorption behavior and mechanism of an ether amine collector on collophane and quartz | |
| CN107617425A (en) | A kind of modified cocoanut shell and the method using vanadium in its reduction water body | |
| US7393402B2 (en) | Pure pearl powder preparation method | |
| CN102585017B (en) | Preparation method of nanoscale solidago canadensis L. microcrystalline cellulose | |
| CN107855095A (en) | A kind of copper molybdate sorbing material and preparation method thereof | |
| CN115121228B (en) | Lanthanum modified carbon nanotube hydrogel as well as preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |