CN108277640B - Process for doping silk by using ternary silica sol - Google Patents
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- CN108277640B CN108277640B CN201810142950.6A CN201810142950A CN108277640B CN 108277640 B CN108277640 B CN 108277640B CN 201810142950 A CN201810142950 A CN 201810142950A CN 108277640 B CN108277640 B CN 108277640B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic System
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
- D06M11/71—Salts of phosphoric acids
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Abstract
The invention discloses a process for doping silk by ternary silica sol, which comprises the following steps: (1) preparing pure silica sol; (2) modification of silica sol: putting the silica sol and sodium chloride into a high-pressure container, heating to 50-63 ℃, stirring at 100-300 r/min, introducing mixed gas containing carbon dioxide, raising the pressure to 5-10 MPa, adding sodium phosphate at the speed of 2g/min while stirring, and continuously reacting for 2-3 h to obtain ternary silica sol; (3) doping: soaking silk in ternary silica sol, heating to 35-42 ℃, soaking for 15-25 min under the condition of ultrasonic treatment, performing double-soaking and triple-pressing on a small padder, and finally drying to obtain the silk after doping treatment. The technical means adopted by the invention can obviously improve the limit oxygen index of the silk, so as to improve the flame retardance of the silk, and the silk has wide market application value.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of silk modification, in particular to a process for doping silk by ternary silica sol.
[ background of the invention ]
The silk is popular with consumers due to the unique soft luster, unique silky feeling and the like. The silk contains N, S elements and good moisture absorption, so that the silk has certain flame retardant property, the limited oxygen index is about 23.0 percent and is obviously higher than 18.0 percent of the cellulose fiber, but the silk still belongs to flammable textiles. Nowadays, the fire-fighting concept of the public fire is continuously enhanced, and the requirements of people on the flame-retardant property of silk are more and more strict. When used as clothes and household articles, silk is generally in direct contact with human skin and is easy to damage human bodies once on fire. Therefore, the research on the flame resistance of the silk has wide market application value. At present, the common method for improving the flame resistance of the silk is to dope flame-retardant raw materials in the silk, but the method has small improvement range on the flame resistance of the silk and can not meet the requirement of flame resistance.
Silica has been widely used as an additive type inorganic silicon flame retardant in the flame retardation of various high molecular polymers such as plastics, synthetic rubbers and synthetic fibers. But it hardly produces effective adsorption bonding with fabrics when it is applied to flame-retardant finishing of natural fibers due to its large particle size. The fiber can only be physically attached to the surface of the fiber in the finishing process, and the fiber has no washability and seriously affects the hand feeling. The sol-gel method is an effective means for synthesizing nano materials, can prepare nano-scale silica sol particles, and can react with active groups on the surface of fibers such as-OH and-NH in the finishing process2And the like, so that the good adsorption combination is realized, the washability of the finishing is improved, and the influence on the hand feeling of the fabric is small.
Therefore, the research on the process for doping and modifying the silk by the silica sol and improving the flame retardant doped in the silk has very important practical significance for improving the use added value of the silk, enhancing the competitiveness of the silk and products thereof in the textile market at home and abroad and stabilizing and expanding the market share of silk products.
[ summary of the invention ]
The invention aims to provide a process for doping silk by ternary silica sol, which comprises the steps of firstly preparing pure silica sol; then modifying the silica sol to prepare ternary silica sol; and finally, under the auxiliary condition of ultrasonic treatment, the ternary silica sol is doped into the silk, so that the flame retardant property of the silk is improved. The technical means adopted by the invention can obviously improve the limit oxygen index of the silk, so as to improve the flame retardance of the silk, and the silk has wide market application value.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a process for doping silk by using ternary silica sol comprises the following steps:
(1) preparation of pure silica sol: adding 10 parts by weight of ethyl orthosilicate, 50-70 parts by weight of absolute ethyl alcohol and 200-300 parts by weight of purified water into a flask, adjusting the pH value to be 4.8-6.5, stirring at the speed of 200-500 r/min, and then reacting for 4-6 hours under the conditions that the ultrasonic treatment power is 1200-2000W and the infrared irradiation power is 500-800W to obtain silica sol;
(2) modification of silica sol: putting 100 parts by weight of silica sol and 0.1 part by weight of sodium chloride into a high-pressure container, heating to 50-63 ℃, starting a stirrer, stirring at the speed of 100-300 r/min, introducing a mixed gas containing carbon dioxide into the high-pressure container to increase the system pressure of the reaction container to 5-10 MPa, adding 6-10 parts by weight of sodium phosphate at the speed of 2g/min while stirring, and continuing to react for 2-3 hours after the addition is finished to obtain ternary silica sol;
(3) doping: according to the weight portion, 10 portions of silk is soaked in 500-700 portions of ternary silica sol, the temperature is raised to 35-42 ℃, the silk is soaked for 15-25 min under the condition that the ultrasonic treatment power is 800-1500W, then the silk is subjected to double soaking and three pressing on a small padder, and finally the silk after doping treatment is obtained after drying treatment.
In the invention, as a further explanation, the carbon dioxide-containing mixed gas in the step (2) is prepared by mixing, by volume ratio, 10-20: 3: 0.1 of carbon dioxide, nitrogen and chlorine.
In the present invention, the silica sol in the step (1) or the step (2) has a particle size of 20 to 100 nm.
In the present invention, as a further illustration, the sodium chloride described in step (2) may be replaced with sodium bicarbonate.
In the present invention, as a further explanation, the process parameters of the drying treatment in step (3) are as follows: drying at 45 ℃ for 25-36 min, then drying at 75 ℃ for 10-15 min, and finally drying at 110 ℃ for 2 min.
In the present invention, as a further explanation, the rolling allowance of the double-dipping triple-pressing in the step (3) is 75 to 85%.
The functions of part of the raw materials are introduced as follows:
tetraethoxysilane, the main raw material used in the present invention for preparing pure silica sol.
Absolute ethanol, the main raw material used in the present invention for preparing pure silica sol.
Sodium chloride, sodium bicarbonate, is used in the present invention to provide sodium ions.
Carbon dioxide, chlorine, is used as the acid gas in the present invention to provide an acidic environment for the reaction system.
Nitrogen is used as an inert shielding gas in the present invention while keeping the reaction system in a high pressure state.
The invention has the following beneficial effects:
1. the preparation method of the pure silica sol can be used for reaction under the condition of low acidity with the pH value of 4.8-6.5, and meanwhile, the reaction time can be shortened. Under the auxiliary conditions of ultrasonic treatment and infrared treatment, the vibration performance of ultrasonic waves can be utilized, so that materials are in continuous vibration, and the collision probability among the materials is improved; and under the irradiation of infrared rays, water molecules are heated and activated, so that large water molecular groups are activated into small water molecular groups, mutual collision and interaction between materials are further improved, the reaction rate is further improved, and the reaction time is shortened.
2. The modification method of the silica sol can efficiently prepare the ternary silica sol, and is used for burying the underlying pen in the subsequent doping process. The invention promotes the silica sol to graft sodium phosphate and sodium chloride under the high-pressure reaction condition of the mixed gas containing carbon dioxide. Under the high-pressure condition of mixed gas containing carbon dioxide, partial gas in carbon dioxide and chlorine can be dissolved in water to form an acidic liquid environment, and then under the high-pressure action of nitrogen, sodium phosphate and sodium chloride are grafted in a silica sol system by using a strong external force to form ternary silica sol containing a silicon-phosphorus system.
3. The doping method adopted by the invention can efficiently dope the ternary silica sol into the structure of the silk. The invention adopts the ultrasonic treatment condition, so that the ternary silica sol can be continuously touched and adhered with the silk under the continuous vibration action of ultrasonic waves, and finally, the ternary silica sol is tightly adhered to the surface of the silk to form a layer of compact protective film, thereby improving the limit oxygen index of the silk and further improving the flame resistance of the silk.
[ detailed description ] embodiments
Example 1:
a process for doping silk by using ternary silica sol comprises the following steps:
(1) preparation of pure silica sol: adding 10 parts by weight of ethyl orthosilicate, 50 parts by weight of absolute ethyl alcohol and 200 parts by weight of purified water into a flask, adjusting the pH value to 4.8, stirring at the speed of 200r/min, and then reacting for 4 hours under the conditions that the ultrasonic treatment power is 1200W and the infrared irradiation power is 500W to obtain silica sol with the particle size of 20 nm;
(2) modification of silica sol: putting 100 parts by weight of silica sol and 0.1 part by weight of sodium chloride into a high-pressure container, heating to 50 ℃, starting a stirrer, stirring at the speed of 100r/min, introducing mixed gas containing carbon dioxide into the high-pressure container to increase the system pressure of the reaction container to 5MPa, adding 6 parts by weight of sodium phosphate at the speed of 2g/min while stirring, and continuing to react for 2 hours after the addition is finished to obtain ternary silica sol; the mixed gas containing carbon dioxide is prepared from the following components in percentage by volume of 10: 3: 0.1 of carbon dioxide, nitrogen and chlorine;
(3) doping: according to parts by weight, 10 parts of silk is soaked in 500 parts of ternary silica sol, the temperature is raised to 35 ℃, the silk is soaked for 15min under the condition that the ultrasonic treatment power is 800W, then the silk is dried for 25min at 45 ℃ after double-soaking and three-pressing on a small padder, then the silk is dried for 10min at 75 ℃, and finally the silk is dried for 2min at 110 ℃ to obtain the silk after doping treatment; the rolling allowance rate of the double-dipping and three-pressing is 75 percent.
Through detection, the limit oxygen index of the silk after being doped with the ternary silica sol is 56.7%.
Example 2:
a process for doping silk by using ternary silica sol comprises the following steps:
(1) preparation of pure silica sol: adding 10 parts by weight of ethyl orthosilicate, 55 parts by weight of absolute ethyl alcohol and 220 parts by weight of purified water into a flask, adjusting the pH value to be 5.2, stirring at the speed of 300r/min, and then reacting for 4.5 hours under the conditions that the ultrasonic treatment power is 1500W and the infrared irradiation power is 570W to obtain silica sol with the particle size of 30 nm;
(2) modification of silica sol: putting 100 parts by weight of silica sol and 0.1 part by weight of sodium bicarbonate into a high-pressure container, heating to 53 ℃, starting a stirrer, stirring at the speed of 200r/min, introducing mixed gas containing carbon dioxide into the high-pressure container to increase the system pressure of the reaction container to 6MPa, adding 8 parts by weight of sodium phosphate at the speed of 2g/min while stirring, and continuing to react for 2.5 hours after the addition is finished to obtain ternary silica sol; the mixed gas containing carbon dioxide is prepared from the following components in percentage by volume of 14: 3: 0.1 of carbon dioxide, nitrogen and chlorine;
(3) doping: according to parts by weight, 10 parts of silk is soaked in 550 parts of ternary silica sol, the temperature is raised to 37 ℃, the silk is soaked for 17min under the condition that the ultrasonic treatment power is 1000W, then the silk is dried for 28min at 45 ℃ after double-soaking and three-pressing on a small padder, then the silk is dried for 11min at 75 ℃, and finally the silk is dried for 2min at 110 ℃ to obtain the silk after doping treatment; the rolling residual rate of the double-dipping and triple-pressing is 82 percent.
Through detection, the limit oxygen index of the silk after being doped with the ternary silica sol is 54.3%.
Example 3:
a process for doping silk by using ternary silica sol comprises the following steps:
(1) preparation of pure silica sol: adding 10 parts by weight of ethyl orthosilicate, 65 parts by weight of absolute ethyl alcohol and 240 parts by weight of purified water into a flask, adjusting the pH value to 5.5, stirring at the speed of 400r/min, and then reacting for 5 hours under the conditions that the ultrasonic treatment power is 1600W and the infrared irradiation power is 700W to obtain silica sol with the particle size of 70 nm;
(2) modification of silica sol: putting 100 parts by weight of silica sol and 0.1 part by weight of sodium chloride into a high-pressure container, heating to 56 ℃, starting a stirrer, stirring at the speed of 190r/min, introducing mixed gas containing carbon dioxide into the high-pressure container to increase the system pressure of the reaction container to 6MPa, adding 7 parts by weight of sodium phosphate at the speed of 2g/min while stirring, and continuing to react for 3 hours after the addition is finished to obtain ternary silica sol; the mixed gas containing carbon dioxide is prepared from the following components in percentage by volume of 14: 3: 0.1 of carbon dioxide, nitrogen and chlorine;
(3) doping: according to parts by weight, 10 parts of silk is soaked in 650 parts of ternary silica sol, the temperature is raised to 40 ℃, the silk is soaked for 20min under the condition that the ultrasonic treatment power is 1200W, then the silk is dried for 33min at 45 ℃ after double-soaking and three-pressing on a small padder, then the silk is dried for 12min at 75 ℃, and finally the silk is dried for 2min at 110 ℃ to obtain the silk after doping treatment; the rolling allowance rate of the double-dipping and three-pressing is 78 percent.
Through detection, the limit oxygen index of the silk after being doped with the ternary silica sol is 55.8%.
Example 4:
a process for doping silk by using ternary silica sol comprises the following steps:
(1) preparation of pure silica sol: adding 10 parts by weight of ethyl orthosilicate, 63 parts by weight of absolute ethyl alcohol and 260 parts by weight of purified water into a flask, adjusting the pH value to 5.5, stirring at the speed of 450r/min, and then reacting for 5.5 hours under the conditions that the ultrasonic treatment power is 1600W and the infrared irradiation power is 700W to obtain silica sol with the particle size of 70 nm;
(2) modification of silica sol: putting 100 parts by weight of silica sol and 0.1 part by weight of sodium chloride into a high-pressure container, heating to 60 ℃, starting a stirrer, stirring at the speed of 160r/min, introducing mixed gas containing carbon dioxide into the high-pressure container to increase the system pressure of the reaction container to 7MPa, adding 8 parts by weight of sodium phosphate at the speed of 2g/min while stirring, and continuing to react for 2.5 hours after the addition is finished to obtain ternary silica sol; the mixed gas containing carbon dioxide is prepared from the following components in percentage by volume of 15: 3: 0.1 of carbon dioxide, nitrogen and chlorine;
(3) doping: according to parts by weight, 10 parts of silk is soaked in 670 parts of ternary silica sol, the temperature is raised to 40 ℃, the silk is soaked for 24min under the condition that the ultrasonic treatment power is 1300W, then the silk is dried for 30min at 45 ℃ after double-soaking and three-pressing on a small padder, then the silk is dried for 14min at 75 ℃, and finally the silk is dried for 2min at 110 ℃ to obtain the silk after doping treatment; the rolling residual rate of the double-dipping and triple-pressing is 82 percent.
Through detection, the limit oxygen index of the silk after being doped with the ternary silica sol is 57.2%.
Example 5:
a process for doping silk by using ternary silica sol comprises the following steps:
(1) preparation of pure silica sol: adding 10 parts by weight of ethyl orthosilicate, 65 parts by weight of absolute ethyl alcohol and 270 parts by weight of purified water into a flask, adjusting the pH value to 5.7, stirring at the speed of 440r/min, and then reacting for 5 hours under the conditions that the ultrasonic treatment power is 1700W and the infrared irradiation power is 750W to obtain silica sol with the particle size of 80 nm;
(2) modification of silica sol: putting 100 parts by weight of silica sol and 0.1 part by weight of sodium bicarbonate into a high-pressure container, heating to 57 ℃, starting a stirrer, stirring at the speed of 200r/min, introducing mixed gas containing carbon dioxide into the high-pressure container to increase the system pressure of the reaction container to 9MPa, adding 9 parts by weight of sodium phosphate at the speed of 2g/min while stirring, and continuing to react for 2 hours after the addition is finished to obtain ternary silica sol; the mixed gas containing carbon dioxide is prepared from the following components in percentage by volume of 13: 3: 0.1 of carbon dioxide, nitrogen and chlorine;
(3) doping: according to parts by weight, 10 parts of silk is soaked in 680 parts of ternary silica sol, the temperature is raised to 40 ℃, the silk is soaked for 22min under the condition that the ultrasonic treatment power is 1400W, then the silk is dried for 32min at 45 ℃ after double-soaking and triple-pressing on a small padder, then the silk is dried for 11min at 75 ℃, and finally the silk is dried for 2min at 110 ℃ to obtain the silk after doping treatment; the rolling residual rate of the double-dipping and triple-pressing is 81 percent.
Through detection, the limit oxygen index of the silk after being doped with the ternary silica sol is 56.5%.
Example 6:
a process for doping silk by using ternary silica sol comprises the following steps:
(1) preparation of pure silica sol: adding 10 parts by weight of ethyl orthosilicate, 70 parts by weight of absolute ethyl alcohol and 300 parts by weight of purified water into a flask, adjusting the pH value to 6.5, stirring at the speed of 500r/min, and then reacting for 6 hours under the conditions that the ultrasonic treatment power is 2000W and the infrared irradiation power is 800W to obtain silica sol with the particle size of 100 nm;
(2) modification of silica sol: putting 100 parts by weight of silica sol and 0.1 part by weight of sodium bicarbonate into a high-pressure container, heating to 63 ℃, starting a stirrer, stirring at the speed of 300r/min, introducing mixed gas containing carbon dioxide into the high-pressure container to increase the system pressure of the reaction container to 10MPa, adding 10 parts by weight of sodium phosphate at the speed of 2g/min while stirring, and continuing to react for 3 hours after the addition is finished to obtain ternary silica sol; the mixed gas containing the carbon dioxide is prepared from the following components in percentage by volume of 20: 3: 0.1 of carbon dioxide, nitrogen and chlorine;
(3) doping: according to parts by weight, 10 parts of silk is soaked in 700 parts of ternary silica sol, the temperature is raised to 42 ℃, the silk is soaked for 25min under the condition that the ultrasonic treatment power is 1500W, then the silk is dried for 36min at 45 ℃ after double-soaking and three-pressing on a small padder, then the silk is dried for 15min at 75 ℃, and finally the silk is dried for 2min at 110 ℃ to obtain the silk after doping treatment; the rolling residual rate of the double-dipping and three-pressing is 85 percent.
Through detection, the limit oxygen index of the silk after being doped with the ternary silica sol is 56.1%.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (5)
1. A process for doping silk by ternary silica sol is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of pure silica sol: adding 10 parts by weight of ethyl orthosilicate, 50-70 parts by weight of absolute ethyl alcohol and 200-300 parts by weight of purified water into a flask, adjusting the pH value to be 4.8-6.5, stirring at the speed of 200-500 r/min, and then reacting for 4-6 hours under the conditions that the ultrasonic treatment power is 1200-2000W and the infrared irradiation power is 500-800W to obtain silica sol;
(2) modification of silica sol: putting 100 parts by weight of silica sol and 0.1 part by weight of sodium chloride into a high-pressure container, heating to 50-63 ℃, starting a stirrer, stirring at the speed of 100-300 r/min, introducing a mixed gas containing carbon dioxide into the high-pressure container to increase the system pressure of the reaction container to 5-10 MPa, adding 6-10 parts by weight of sodium phosphate at the speed of 2g/min while stirring, and continuing to react for 2-3 hours after the addition is finished to obtain ternary silica sol;
(3) doping: according to the weight portion, 10 portions of silk is soaked in 500-700 portions of ternary silica sol, the temperature is raised to 35-42 ℃, the silk is soaked for 15-25 min under the condition that the ultrasonic treatment power is 800-1500W, then the silk is soaked in a small padder for three times, and finally the silk is dried to obtain the silk after doping treatment;
the carbon dioxide-containing mixed gas in the step (2) is prepared from the following components in a volume ratio of 10-20: 3: 0.1 of carbon dioxide, nitrogen and chlorine.
2. The process for doping silk by using ternary silica sol as claimed in claim 1, which is characterized in that: the particle size of the silica sol in the step (1) or the step (2) is 20-100 nm.
3. The process for doping silk by using ternary silica sol as claimed in claim 1, which is characterized in that: the sodium chloride in the step (2) can be replaced by sodium bicarbonate.
4. The process for doping silk by using ternary silica sol as claimed in claim 1, which is characterized in that: the drying treatment in the step (3) has the following process parameters: drying at 45 ℃ for 25-36 min, then drying at 75 ℃ for 10-15 min, and finally drying at 110 ℃ for 2 min.
5. The process for doping silk by using ternary silica sol as claimed in claim 1, which is characterized in that: and (4) the rolling residual rate of the double-leaching and triple-pressing in the step (3) is 75-85%.
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