CN112957281A

CN112957281A - High-elasticity, high-stability and quick-drying hair styling spray composition and preparation method thereof

Info

Publication number: CN112957281A
Application number: CN202110167374.2A
Authority: CN
Inventors: 王绍梅; 张太军; 秦涛; 李涛; 郭星星; 张界墨; 祝雪梅; 林沛东
Original assignee: Guangzhou Quanzhi Meifu Biotechnology Research Institute Co ltd; Pelai Brand Management Co ltd
Current assignee: Guangzhou Quanzhi Meifu Biotechnology Research Institute Co ltd; Pelai Brand Management Co ltd
Priority date: 2021-02-05
Filing date: 2021-02-05
Publication date: 2021-06-15

Abstract

The invention discloses a high-elasticity, high-stability and quick-drying hair styling spray composition. The high-elasticity high-stability quick-drying hair styling spray composition comprises the following components in percentage by mass: 1.0-10.0% of film forming agent; 0.01-5.0% of nano natural fiber substances; 80.0-99.0% of anhydrous solvent; 0.001-15.0% of other active additives soluble in the above combination. The high-elasticity, high-stability and quick-drying hair styling spray composition disclosed by the invention can enable the hair style to be always in the initial perfect state, help consumers to relieve the use troubles and improve the self-confidence of the consumers in social interaction.

Description

High-elasticity, high-stability and quick-drying hair styling spray composition and preparation method thereof

Technical Field

The invention belongs to the technical field of hair care products, and particularly relates to a liquid conditioning composition for helping hair style to be fixed quickly and a preparation method thereof.

Background

With the improvement of life quality, people pay more and more attention to the beauty, touch, shape, color, luster and the like of hairstyles, and the requirements are more and more refined in the coming months. The hair reflects the personal taste, social status and life attitude of a person from a certain angle. Therefore, always having a healthy and styled hair is becoming one of the important parts of people for good life. On the other hand, the hair is fine, numerous and long, and it is not easy to easily manage the hair. How to keep the carefully combed hair style in the original state in various scenes is becoming a more and more concerned issue for consumers.

CN201510528781.6 discloses a solution for aqueous hair fixative liquid compositions, CN201880083767.1 discloses a hair fixative composition of amino substituted alkoxy silanes, CN201880030941.6 discloses a composition of polyammonium salts as hair fixatives, which, although they all solve the need of hair fixatives from a certain point of view, still face a number of specific problems, such as long time for hair fixations and even the need of dry air, such as non-permanent hair fixations, easy and messy hair in case of walking or blowing, and the lack of confidence of consumers for such products.

Disclosure of Invention

In order to overcome the defects of the technical scheme, the invention aims to provide a high-elasticity, high-stability and quick-drying hair styling spray composition, so that the hair style is always in the initial perfect state, the use trouble of consumers is relieved, and the self-confidence of the consumers in social interaction is improved.

The invention provides a high-elasticity, high-stability and quick-drying hair styling spray composition which comprises the following components in percentage by mass:

1.0-10.0% of film forming agent;

0.01-5.0% of nano natural fiber substances;

80.0-99.0% of anhydrous solvent;

0.001-15.0% of other active additives soluble in the above combination.

Further, the high-elasticity, high-stability and quick-drying hair styling spray composition comprises the following components in percentage by mass:

1.5-8.0% of film-forming agent,

0.01-4.0% of nano natural fiber substances;

85.0-99.0% of anhydrous solvent;

0.001-10.0% of other active additives soluble in the above combination.

The typical structure of the film-forming agent of the invention is as follows:

r is an alkane, alkene or aromatic structure with 10-18 carbons. n is a natural number from 1 to 50, m is a natural number from 1 to 25, and a more typical structure includes an acrylic/lauryl/stearyl/ethylamine oxide methacrylate copolymer.

The film-forming agent of the present invention also includes the typical structure:

x is a natural number of 5-50, y is a natural number of 1-30, and the component is typically PVP/VA copolymer

a is a natural number from 5 to 50, b + c is a natural number from 1 to 30, and typical ingredients include PVP/VA vinyl propionate copolymer.

the polymerization degree is 5-20, and typical components comprise polyvinylpyrrolidone, PVP K90K 30 and the like;

r is an alkane, alkene or aromatic hydrocarbon structure with 8-18 carbons. m, n are greater than 1, m + n is 5 to 60; x, y is greater than 1, and x + y is from 10 to 30, and typically includes POLYQUATERNIUM-69.

The nano natural cellulose substance has the following typical characteristics:

more than 94% of the fibers have a physical characteristic of 0-100 microns in length and 0-40 microns in diameter, and more preferably 94% of the fibers have a physical characteristic of 0-100 microns in length but 0-5 microns in diameter.

As shown in fig. 1 to 3, the nanocellulose-based materials of the present invention, after being dispersed in a solvent, have the following typical appearance characteristics under a polarization microscope (dark field):

the nano natural fiber substances can be obtained from rhizome parts of all natural plants and residues of the natural plants after being treated by various enzymolysis and other treatment means, as long as the physical form of the nano natural fiber substances meets the requirements of the invention and meets all requirements of cosmetic laws on raw material safety. But does not include various synthetic plastic fiber materials, synthetic chemical materials.

The anhydrous organic solvent of the present invention typically comprises one or more of alkanes or isoparaffins having less than 10 carbon atoms, ethanol, isopropanol, propanol, cyclomethicone, and the like.

The anhydrous means that the water content is less than 3%.

Other active additives of the present invention that are soluble in the above combinations are primarily various types of active ingredients having a water content of less than 3% including, but not limited to: plant extract, antioxidant, anti-free radical component, fullerene, various amino acids, anti-allergic agent, radix Paeoniae extract, rhizoma Gastrodiae extract, etc. by extracting with ethanol and oil, including herba Menthae (Mentha HAPLOCALIX) extract, radix Paeoniae (Paeonia ALBIFLORA) root extract, lysine, histidine, arginine, aspartic acid, threonine, serine, glutamic acid, proline, glycine, alanine, valine, isoleucine, leucine, tyrosine, phenylalanine, one or more of Carthami flos (Carthamus TINCTORIUS) flower extract, radix Saposhnikoviae (Saposhnikovia DIVARICATA) root extract, rhizoma Gastrodiae (Gastrodia ELATA) extract, Glycyrrhrizae radix (Glycyrrhiza URALENSIS) root extract, Candida/glucose/rapeseed methyl oleate fermentation product, bupleuri radix (Bupleurum CHINENSIS) root extract, rhizoma Polygonati (Polygonatum SIBIRICUM) extract, radix astragali (Astragalus COMPLANATUS) extract, glucosylrutin, etc.

The active additive is used in the amount of 0.001-20.0%, preferably 0.001-10.0%;

the final composition morphology of the invention includes the following physical appearances, from milky white suspension to a clear watery appearance: as shown in fig. 4.

The high-elasticity, high-stability and quick-drying hair styling spray composition is liquid and can be atomized at normal temperature.

The high-elasticity, high-stability and quick-drying hair styling spray composition has the viscosity of less than 800mPa.s at normal temperature.

The high-elasticity, high-stability and quick-drying hair styling spray composition provided by the invention has the advantages that the used materials conform to national and industrial regulations and standards, and more completely conform to various indexes in technical specifications for cosmetic safety (2015 edition) issued by the state, and the composition is safe and healthy.

In addition, the invention also discloses a preparation method of the high-elasticity, high-stability and quick-drying hair styling spray composition, which comprises the following steps:

1) adding a shaping agent into the anhydrous organic solvent, and properly stirring to form a transparent solution;

2) adding nanometer natural fiber substances into the homogenizer, performing high-speed average to activate active hydroxyl on the surface of the natural nanometer fiber, maintaining the average time within 30min and keeping attention to ventilation and static control of the working environment, wherein the linear speed of the tail end of the homogenizer rotor cannot be lower than 25 m/s;

3) sampling, observing and amplifying a field of view of 100 times under a microscope, wherein no clustered nano cellulose micelles are found, and stopping the mean value;

4) adding the rest materials, inspecting, and discharging.

By means of the technical scheme, the invention has the following advantages and beneficial technical effects:

1) the high-elasticity, high-stability and quick-drying hair styling spray composition is a water-free system, is obviously different from the conventional hair care composition, and has crystal clear and transparent appearance like water;

2) the hair styling conditioning composition not only maintains outstanding performance on hair styling capability, but also reduces the use of chemically synthesized styling agents, relieves the environmental stress, and reduces the emission of carbon dioxide caused by using more chemical styling agents;

3) the sizing conditioning composition disclosed by the invention has the advantages that under the condition of reducing the using amount of the chemical sizing agent, the strength of a film for fixing the hairstyle, which is formed by the sizing agent, is greatly improved by adding a material similar to a 'steel bar' into the film, so that the final sizing effect is increased. The hair is kept in the initial hairstyle state under the action of external force, such as wind blowing, sports, walking, running, scarf friction and the like, and the hairstyle holding force is obviously changed.

4) The styling conditioning composition of the present invention, which sets quickly, is fixed upon completion of a spray, and does not use compressed gas for filling, is obvious for savings in manufacturing investment.

5) The hair styling conditioning composition disclosed by the invention enables the styling liquid to have extremely low surface tension on the hair surface through compounding, and the hair styling conditioning composition can be rapidly spread and instantaneously volatilize, so that the problems that water with high surface tension is slow to spread and volatilize and a fan is used for drying in order to fix the hair style in the prior art are solved.

Drawings

Fig. 1 is a characteristic of a dispersion state of nanocellulose in an anhydrous solvent alcohol.

Fig. 2 is a characteristic of a dispersion state of nanocellulose in an anhydrous solvent isopropanol.

Fig. 3 is a characteristic of the dispersion state of nanocellulose in isoparaffin.

Fig. 4(a) and 4(b) are the final two-state appearance diagrams of the combination of the present invention, respectively.

FIG. 5 is a polarized light microscopic characterization of the morphological features of the random samples of examples 1-15 after drying to a film.

FIG. 6 is a polarized light microscopic feature of a random sample of the control example.

Fig. 7 is a diagram of an enlightened material of the present invention.

Fig. 8 is a graph comparing the effect of different examples and comparative examples on hair stiffness.

FIG. 9A is a state of a hair strand after pulse oscillation according to an embodiment; FIG. 9B shows the state of hair strands after blowing the air duct for 5 minutes in example; fig. 9C shows the embodiment continuing to hang the hair strand for 8 hours after the disturbance.

FIG. 10A is a state of a hair bundle after pulse rocking of the comparative example; FIG. 10B shows the state of hair strands after blowing the air duct for 5 minutes in the comparative example; fig. 10C shows the control example continuing to hang the tress for 8 hours after the disturbance.

FIG. 11 shows consumer results of a survey of sample examples and comparative examples.

Detailed Description

To facilitate an understanding of the invention, a more complete description of the invention will be given below in terms of preferred embodiments. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

The raw material percentages in the following examples and comparative examples are weight percentages.

The nano natural fiber substances can be obtained from rhizome parts of all natural plants and residues of the natural plants after being treated by various enzymolysis and other treatment means, as long as the physical forms of the nano natural fiber substances meet the requirements of the invention and meet all requirements of cosmetic laws on raw material safety. But does not include various synthetic plastic fiber materials, synthetic chemical materials.

The anhydrous organic solvent of the present invention typically comprises one or more of alkanes or isoparaffins having less than 10 carbon atoms, ethanol, isopropanol, propanol, cyclomethicone, and the like. The anhydrous means that the water content is less than 3%.

Other active additives of the present invention that are soluble in the above combinations are primarily active ingredients of various types having a water content of less than 3%, including but not limited to: plant extract, antioxidant, anti-free radical component, fullerene, various amino acids, anti-allergic agent, peony extract, rhizoma Gastrodiae extract, etc. by extracting with ethanol and oil.

The active additive comprises: one or more of herba Menthae (Mentha haplochia) extract, radix Paeoniae (Paeonia alba) root extract, lysine, histidine, arginine, aspartic acid, threonine, serine, glutamic acid, proline, glycine, alanine, valine, isoleucine, leucine, tyrosine, phenylalanine, Carthami flos (Carthamus TINCTORIUS) flower extract, radix Saposhnikoviae (Saposhnovata) root extract, rhizoma Gastrodiae (Gastrodia ELATA) extract, Glycyrrhrizae radix (Glycyrrhiza URALENSIS) root extract, Candida/glucose/rapeseed methyl oleate fermentation product, bupleuri radix (Bupleurum CHINENSIS) root extract, rhizoma Polygonati (Polygonatum SIBIRICUM) extract, radix astragali (Astragalus membranaceus) extract, glucosyl group, etc.

the final composition morphology of the present invention includes the following physical appearance, two different appearance plots from milky white suspension state to clear water sample, as shown in fig. 4(a) and 4 (b).

The invention provides a high-elasticity, high-stability and quick-drying hair styling spray composition, belongs to the technical field of hair care products, and particularly relates to a liquid conditioning composition for helping hair style to be fixed quickly and a preparation method thereof. The composition is prepared from the following raw materials in percentage by weight. Comprises the following components in percentage by mass:

1.0-10.0% of chemical synthesis shaping film-forming agent;

0.01-5.0% of nano natural fiber substances;

70.0-99.0% of anhydrous solvent;

0.001-15.0% of other active additives soluble in the above combination.

Further, a high-elasticity, high-stability and quick-drying hair styling spray composition comprises the following components in percentage by mass:

1.5-8.0% of chemical synthesis shaping film-forming agent;

0.01-4.0% of nano natural fiber substances;

85.0-99.0% of anhydrous solvent;

0.001-10.0% of other active additives soluble in the above combination.

The typical structure of the film-forming agent of the invention is as follows:

r is an alkane, alkene or aromatic structure with 10-18 carbons. More typical structures include acrylic/lauryl/stearyl acrylate/ethyl amine oxide methacrylate copolymers.

The high-elasticity, high-stability and quick-drying hair styling spray composition has the advantages that chemical synthesis components are reduced, the styling capability is not influenced, and even the hair styling spray composition is greatly helpful for improving the styling stability; meanwhile, the hair is more natural and soft through a compounding technology, and the hair does not feel stiff.

The method of using the high-elasticity, high-stability and quick-drying hair styling spray composition can be expressed as follows:

the hair is combed into the desired hairstyle with the aid of a tool, the composition is sprayed onto the hair with a spray pump head at a distance of 25cm from the hair, and after 5 seconds the hair is released, it is fixed into the desired shape and remains well in its original state after exercise, running or blowing.

Example 1

A high-elasticity, high-stability and quick-drying hair styling spray composition has the following formula composition in percentage by weight as shown in the following table 1.

TABLE 1 compositions and contents (% by weight) of formulations of examples 1-1 to 1-8

The method for preparing the high-elasticity, high-stability and quick-drying hair styling spray composition of the embodiment comprises the following steps:

1) adding PVP/VA copolymer or acrylic acid (ester)/lauryl alcohol acrylate/stearyl alcohol acrylate/ethylamine oxide methacrylate copolymer into 95% ethanol solution, and stirring to obtain transparent solution;

2) adding nanometer natural cellulose into the mixture, activating active hydroxyl on the surface of the natural nanometer fiber at a high speed average value, keeping the end linear speed of a rotor of a homogenizer not lower than 25m/s and the average value time not lower than 30min, and paying attention to ventilation and static control of a working environment;

4) adding the rest material of radix Paeoniae extract or glucosyl rutin, checking, and discharging.

Example 2

A high elasticity, high stability and quick drying hair styling spray composition comprises the following components in percentage by weight:

TABLE 2 compositions and contents (% by weight) of formulations of examples 2-1 to 2-8

1) adding PVP/VA vinyl propionate copolymer, polyvinylpyrrolidone, and POLYQUATERNIUM-69 into cyclomethicone and isopropanol, and stirring to obtain transparent solution;

4) adding the rest materials including flos Carthami (Carthamus TINCTORIUS) extract, radix astragali (Astragalus COMPLANATUS) extract, rhizoma Polygonati (Polygonatum SIBIRICUM) extract, and radix bupleuri (Bupleurum chinense) root extract, testing, and discharging.

The following are contents of the effect test examples.

Comparative example

An anhydrous clear liquid head conditioning composition having the composition, in weight percent, shown in table 3 below:

TABLE 3 compositions and contents (% by weight) of formulations of comparative examples 1-1 to 1-8

Comparative appearance, examples evaluation protocol and results:

1. polarized light microscope analysis

The samples of examples and the control samples were sprayed on a glass slide, dried, and then observed under a microscope for the physical form of the inside of the film-formed film. Example micrographs are shown in figure 5:

the microscopic image of the control example is shown in fig. 6:

the sizing agent film observed in the examples has a fiber structure similar to that of concrete reinforcement inside, and they are uniformly distributed inside the sizing cement, as shown in fig. 7, which is inspired by the design of the plastic reinforced pipe. No imaging traces were visible from the control.

The observation shows that the nano-cellulose can well diffuse into the mucilage of the sizing agent, thereby helping to enhance the strength of the sizing film and helping the product to have more lasting and stable sizing capability.

1. Hair bundle shaping comparison;

2. three-point bending test of hair

Experimental materials: healthy hair tresses are purchased commercially.

An experimental instrument: hair tester (Beijing gold sail commercial, LLC); constant temperature and humidity case.

The experimental principle is as follows: the elastic modulus E represents the rigidity of the material, the larger the value of E, the larger the rigidity is, the less deformation is caused, the larger the value of E/E1 is, the larger the rigidity is, the less deformation is caused, and the hair style can be maintained more durably without being damaged by factors including movement, wind blowing and the like, regardless of the sectional area of the material.

The experimental method comprises the following steps:

newly purchased hair tresses (about 8g, about 25 cm) are put into 0.3% NaOH solution to be soaked for 2.5 hours, and the hair tresses are taken out, cleaned and dried in the air. Washing with 10% K12 solution for 2 times, washing with water, soaking in 50% ethanol solution for 50 min, and air drying. Each hair tress was coated with 0.8g of the product, which was then left to dry in a constant temperature and humidity environment at 25 ℃ and 50% RH overnight and tested with a hair tester.

As shown in fig. 8, the above data show that the rigidity of the styling agents of examples 1-15 significantly enhances the styling ability of the hair strands supported by significant mechanical rigidity through the addition of nanocellulose. The data from example 1 and example 16 more clearly show that the combination of the two has a significant synergistic effect. The values of controls 1-8 show that nanocellulose alone has little significant value when used alone, but that it exhibits surprising value when used in combination with a styling cement.

4. Hair Strand styling durability control

Experimental materials: healthy hair tresses are purchased commercially.

The experimental method comprises the following steps:

newly purchased hair tresses (about 8g, about 25 cm) are put into 0.3% NaOH solution to be soaked for 2.5 hours, and the hair tresses are taken out, cleaned and dried in the air. Washing with 10% K12 solution for 2 times, washing with water, soaking in 50% ethanol solution for 50 min, and air drying. Each bundle of hair was styled using the samples of the examples and the control examples, fixed on the same support, the support was given fixed pulse swing for 1 minute, simulated human movement and blowing with an air duct for 15 minutes in different directions, and was stood, hung and photographed. The styling effect was judged by observing the hold of the hair curls.

Example samples were randomly drawn:

the hair bundle state after pulse oscillation in the embodiment of fig. 9A, the hair bundle state after 5 minutes of air cylinder blowing in the embodiment of fig. 9B, and the hair bundle state after 8 hours of hanging after the two treatments in the embodiment of fig. 9C.

Random extraction control example:

fig. 10A shows the state of hair strand after pulse oscillation in comparison example, fig. 10B shows the state of hair strand after 5 minutes of blowing in wind cylinder in comparison example, and fig. 10C shows the state of hair strand after 8 hours of hanging after the above two treatments in comparison example.

From the test results, the control example showed poor hair style retention under exercise and wind blowing, and after 8 hours, the hair was almost returned to the original shape with a great change in the degree of curling, which indicates poor hair style retention. The examples continued to maintain a better hairstyle after the movement and after the wind blowing, without much change in the degree of curling. The technical scheme of the invention has the capability of obviously improving the hair style retention of the traditional styling product and greatly improving the capability of the product for retaining the original hair style.

5. Example consumer sensory experience testing

Samples 3 and 16 of the conditioning compositions prepared in examples 1-15 were randomly drawn and numbered as samples 1-4, respectively, and controls 3, 7, 8 were numbered as controls for 1-3, respectively, and the shaped spray controls from the two brands best known in the world. In winter, (the temperature is about 5-11 ℃), 42 volunteers, half of male and female, 18-50 years old, half of underhaired and fine haired are respectively randomly divided into 7 groups for trial test.

Volunteers observed the experience throughout the day after use and filled out the use report faithfully.

The staff collects the reported data, the conditions of the hairstyle fixing speed, the hair brightness, the touch naturalness, the white scurf combing amount, the hairstyle retention force, the sensory hair amount increase and the second hair washing comfort test of the volunteer after use are tracked and counted, and the test subjects score according to the use feelings of the test subjects.

The scoring criteria were taken to be 10 points, 1 being the worst and 10 being the best. The average value of each group of data is used as the final measurement result, and the statistical result of the data of the final test is shown in the following figure 11:

from the statistical results, the product corresponding to the technical scheme of the invention has relative advantages in various aspects compared with the control product. Wherein, the hair style has bright appearance on the performance indexes of increasing the sensory hair amount, maintaining the hair style endurance and setting the hair style.

From the data, the technical scheme of the invention has obvious performance characteristics and market attraction. Has outstanding characteristics on the actual performance index.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, so that any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.

Claims

1. A high-elasticity, high-stability and quick-drying hair styling spray composition is characterized in that: the paint comprises the following components in percentage by mass:

1.0-10.0% of film forming agent;

0.01-5.0% of nano natural fiber substances;

80.0-99.0% of anhydrous solvent;

0.001-15.0% of other active additives soluble in the above combination.

2. A highly elastic highly stable quick-drying hair styling spray composition according to claim 1 characterized by: the paint comprises the following components in percentage by mass:

1.5-8.0% of film forming agent;

0.01-4.0% of nano natural fiber substances;

85.0-99.0% of anhydrous solvent;

0.001-10.0% of other active additives soluble in the above combination.

3. A highly elastic highly stable quick-drying hair styling spray composition according to claim 1 characterized by: the structure of the film forming agent is as follows:

r is an alkane, alkene or aromatic hydrocarbon structure of 10-18 carbons;

n is a natural number from 1 to 50, m is a natural number from 1 to 25, and a more typical structure includes an acrylic/lauryl/stearyl/ethylamine oxide methacrylate copolymer.

4. A highly elastic highly stable quick-drying hair styling spray composition according to claim 3 characterized by: the structure of the film forming agent is as follows:

x is a natural number from 5 to 50, y is a natural number from 1 to 30, and a more typical composition is a PVP/VA copolymer.

5. A highly elastic highly stable quick-drying hair styling spray composition according to claim 3 characterized by: the structure of the film forming agent is as follows:

6. A highly elastic highly stable quick-drying hair styling spray composition according to claim 3 characterized by: the structure of the film forming agent is as follows:

the polymerization degree is 5-20, and typical components comprise polyvinylpyrrolidone, PVP K90, K30.

7. A highly elastic highly stable quick-drying hair styling spray composition according to claim 3 characterized by: the structure of the film forming agent is as follows:

r is an alkane, alkene or aromatic hydrocarbon structure of 8-18 carbons; m and n are respectively larger than 1, and m + n is 5 to 60; x, y is greater than 1, x + y is 10-30, and typically includes POLYQUATERNIUM-69.

8. A highly elastic highly stable quick-drying hair styling spray composition according to claim 3 characterized by: the nano natural cellulose substance has the following special characteristics:

9. A highly elastic highly stable quick-drying hair styling spray composition according to claim 3 characterized by: the viscosity of the high-elasticity, high-stability and quick-drying hair styling spray composition is lower than 800mPa.s at normal temperature.

10. A process for preparing a highly elastic highly stable quick drying hair styling spray composition according to any of claims 1 to 9, characterized in that it comprises the steps of:

2) adding nano natural fiber substances into the transparent solution obtained in the step 1), carrying out high-speed average to activate active hydroxyl on the surface of natural nano fibers, keeping the linear speed of the tail end of a rotor of the homogenizer not lower than 25m/s, keeping the average time not lower than 30min, and paying attention to ventilation and static control of a working environment;

4) adding the rest materials, inspecting, and discharging.