CN108277640A - A kind of technique of ternary Ludox doping real silk - Google Patents
A kind of technique of ternary Ludox doping real silk Download PDFInfo
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- CN108277640A CN108277640A CN201810142950.6A CN201810142950A CN108277640A CN 108277640 A CN108277640 A CN 108277640A CN 201810142950 A CN201810142950 A CN 201810142950A CN 108277640 A CN108277640 A CN 108277640A
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- ludox
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- ternary
- real silk
- doping
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 25
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 21
- 238000002525 ultrasonication Methods 0.000 claims abstract description 20
- 238000002386 leaching Methods 0.000 claims abstract description 17
- 238000010792 warming Methods 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 230000004048 modification Effects 0.000 claims abstract description 11
- 238000012986 modification Methods 0.000 claims abstract description 11
- 239000011780 sodium chloride Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 5
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 12
- 239000001569 carbon dioxide Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052801 chlorine Inorganic materials 0.000 claims description 10
- 239000000460 chlorine Substances 0.000 claims description 10
- 230000005855 radiation Effects 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 8
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical class CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 claims description 8
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 8
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- 235000011008 sodium phosphates Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 abstract description 10
- 239000001301 oxygen Substances 0.000 abstract description 10
- 229910000162 sodium phosphate Inorganic materials 0.000 abstract description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- 239000003063 flame retardant Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 241000790917 Dioxys <bee> Species 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- LQXOAOAFWIHNHD-UHFFFAOYSA-K C(=O)=O.P(=O)([O-])([O-])[O-].[Na+].[Na+].[Na+] Chemical compound C(=O)=O.P(=O)([O-])([O-])[O-].[Na+].[Na+].[Na+] LQXOAOAFWIHNHD-UHFFFAOYSA-K 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002844 continuous effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- 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
-
- 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 Table
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Silicon Compounds (AREA)
- Cosmetics (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses the techniques that a kind of ternary Ludox adulterates real silk, include the following steps：(1) preparation of pure silicon colloidal sol；(2) modification of Ludox：Ludox and sodium chloride are placed in high-pressure bottle, 50~63 DEG C is warming up to, is stirred with 100~300r/min, it is passed through carbonated mixed gas, pressure is made to rise to 5~10MPa, sodium phosphate is added with 2g/min speed while stirring, the reaction was continued 2~3h, obtains ternary Ludox；(3) it adulterates：Real silk is immersed in ternary Ludox, is warming up to 35~42 DEG C, 15~25min is impregnated under the conditions of ultrasonication, then finally passes through drying and processing after three pressure of double leachings on small-sized padding machine, obtains the silk after doping treatment.The technological means that the present invention uses can significantly improve the limit oxygen index of real silk, and then improve the anti-flammability of real silk, have large market application value.
Description
【Technical field】
The present invention relates to the modification field of silk, more particularly to a kind of technique of ternary Ludox doping real silk.
【Background technology】
Real silk is deep to be welcome by consumers in general because of its unique soft gloss, unique scrooping feel etc..Silk
Silk because in chemical composition containing the elements such as N, S and good hygroscopicity due to make itself just have certain flame-retarding characteristic,
Its limit oxygen index is 23.0% or so, hence it is evident that is higher than the 18.0% of cellulose fibre, but it still falls within flammable textile.
Today that public fire fire-fighting idea constantly enhances, requirement of the people to real silk flame retardant property are also increasingly stringenter.Silk
Silk in use, be generally in direct contact with human skin, is easy to cause to hinder to body as clothes, household items once catching fire
Evil.Therefore the anti-fire of research real silk has large market application value.Raising real silk common at present is anti-
Fire-retardant method is that fire-retardant raw material is adulterated in real silk, but to the flame retardant property increase rate of real silk in this method
It is small, the requirement of anti-fire cannot be reached.
A kind of inorganic silicon-series five-retardant of the silica as addition type, already in various high molecular polymers, as plastics,
The fire-retardant middle extensive use of synthetic rubber and synthetic fibers.But when it is applied to the flame-proof treatment of natural fiber due to grain
It spends larger, effective absorption can hardly be generated with fabric and is combined.Physical it can only be attached to fiber surface during arrangement,
Do not have washability not only, also seriously affects feel.And sol-gal process is as a kind of effective means of nano materials, energy
The silica sol particles for preparing nanoscale, during arrangement can with the active group on fiber surface such as-OH ,-
NH2It is combined Deng good absorption occurs, not only improves the washability of arrangement, fabric feeling influenced also little.
Therefore a kind of technique that Ludox is adulterated, is modified real silk, improves real silk doping fire retardant is studied, it is right
In use the added value for improving real silk, enhance the competitiveness that silk and its product are at home and abroad weaved in the market, stablize with
Expand the market share of true silk products, it may have highly important realistic meaning.
【Invention content】
Present invention aims at a kind of technique of ternary Ludox doping real silk is provided, it is molten that the present invention first prepares pure silicon
Glue；Then Ludox is modified, prepares ternary Ludox；Finally under the subsidiary conditions of ultrasonication, by ternary silicon
Sol Doping enters in real silk, and then improves the flame retardant property of real silk.The technological means that the present invention uses can be notable
The limit oxygen index of real silk is improved, and then improves the anti-flammability of real silk, there is large market application value.
In order to achieve the above objectives, the technical solution adopted in the present invention is：A kind of ternary Ludox doping real silk
Technique includes the following steps：
(1) preparation of pure silicon colloidal sol：It counts in parts by weight, by 10 parts of ethyl orthosilicates, 50~70 parts of absolute ethyl alcohols and 200
~300 parts of pure water are added in flask, and it is 4.8~6.5 to adjust pH value, is stirred with the speed of 200~500r/min, so
4~6h is reacted under conditions of ultrasonication power is 1200~2000W, infrared radiation power is 500~800W afterwards, is obtained
To Ludox；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium chloride is placed in high-pressure bottle
In, 50~63 DEG C are warming up to, starts blender, is stirred with the speed of 100~300r/min, is then led in high-pressure bottle
Enter carbonated mixed gas, the system pressure of reaction vessel is made to rise to 5~10MPa, while stirring with 2g/min speed
6~10 parts of sodium phosphates are added, after addition, the reaction was continued 2~3h obtains ternary Ludox；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 500~700 parts of ternary Ludox, heat up
To 35~42 DEG C, 15~25min is impregnated under conditions of ultrasonication power is 800~1500W, then on small-sized padding machine
After three pressure of double leachings, finally passes through drying and processing, obtain the silk after doping treatment.
In the present invention, as further explanation, the carbonated mixed gas described in step (2) is by pressing volume
Than being 10~20：3：0.1 carbon dioxide, nitrogen and chlorine mixes.
In the present invention, as further explanation, the grain size of the Ludox described in step (1) or step (2) is 20~
100nm。
In the present invention, as further explanation, the sodium chloride described in step (2) can be substituted with sodium bicarbonate.
In the present invention, as further explanation, the technological parameter of the drying and processing described in step (3) is：At 45 DEG C
25~36min is dried, then dry 10~15min at 75 DEG C, finally the dry 2min at 110 DEG C.
In the present invention, as further explanation, the pick-up that double leachings three described in step (3) are pressed is 75~85%.
The function introduction of part material is as follows：
Ethyl orthosilicate is used to prepare the primary raw material of pure silicon colloidal sol in the present invention.
Absolute ethyl alcohol is used to prepare the primary raw material of pure silicon colloidal sol in the present invention.
Sodium chloride, sodium bicarbonate are used to provide sodium ion in the present invention.
Carbon dioxide, chlorine are used as sour gas, acidic environment are provided for reaction system in the present invention.
Nitrogen is used as inert protective gas in the present invention, while making to be in high pressure conditions in reaction system.
The invention has the advantages that：
1. the preparation method for the pure silicon colloidal sol that the present invention uses, can be under conditions of pH value be 4.8~6.5 Low acid
Reaction, while the reaction time can also be shortened.The present invention uses under the subsidiary conditions of ultrasonication and infra red treatment, can
Using the vibration performance of ultrasonic wave, so that material is among constantly vibration, improve the collision probability between material；Along with infrared
Under the radiation of line, hydrone activated by heat makes the activation of big water clusters into small water molecule group, further increases between material
Mutually collision and interaction, and then reaction rate is improved, shorten the reaction time.
It is subsequent doping process 2. the method for modifying for the Ludox that the present invention uses can efficiently prepare ternary Ludox
Carry out hide the foreshadowing.The present invention promotes Ludox grafting in the reaction under high pressure condition of the mixed gas containing carbon dioxide
Sodium phosphate and sodium chloride.Under the condition of high voltage of the mixed gas containing carbon dioxide, the part gas in carbon dioxide and chlorine
Body can dissolve in water, form acid liquid environment, then under the effect of the high pressure of nitrogen, using strong external force, by sodium phosphate
It is grafted in Ludox system with sodium chloride, forms the ternary Ludox containing silicon-phosphorus system.
3. doping method of the present invention can efficiently be doped into ternary Ludox in the structure of real silk.This
Invention is enable ternary Ludox under the continuous effect of vibration of ultrasonic wave, is promoted ternary silicon using the condition of ultrasonication
Colloidal sol is constantly touched with real silk, is adhered to, and is finally adhered tightly to the surface of real silk, formed one layer it is fine and close
Protective film, and then the limit oxygen index of real silk is improved, further increase the resistance to anti-flammability of real silk.
【Specific implementation mode】
Embodiment 1：
A kind of technique of ternary Ludox doping real silk, includes the following steps：
(1) preparation of pure silicon colloidal sol：It counts in parts by weight, 10 parts of ethyl orthosilicates, 50 parts of absolute ethyl alcohols and 200 parts are pure
Water purification is added in flask, and it is 4.8 to adjust pH value, is stirred with the speed of 200r/min, then in ultrasonication power
4h is reacted under conditions of being 500W for 1200W, infrared radiation power, obtains the Ludox that grain size is 20nm；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium chloride is placed in high-pressure bottle
In, 50 DEG C are warming up to, starts blender, is stirred with the speed of 100r/min, is then passed through containing dioxy in high-pressure bottle
The mixed gas for changing carbon, makes the system pressure of reaction vessel rise to 5MPa, and 6 parts of phosphoric acid are added with 2g/min speed while stirring
Sodium, after addition, the reaction was continued 2h obtains ternary Ludox；The carbonated mixed gas is by pressing volume
Than being 10：3：0.1 carbon dioxide, nitrogen and chlorine mixes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 500 parts of ternary Ludox, are warming up to 35
DEG C, 15min is impregnated under conditions of ultrasonication power is 800W, then on small-sized padding machine after three pressure of double leachings,
25min is dried at 45 DEG C, then the dry 10min at 75 DEG C, finally at 110 DEG C after dry 2min, after obtaining doping treatment
Silk；The pick-up that double leachings three are pressed is 75%.
After testing, real silk, limit oxygen index 56.7% after present invention ternary Ludox doping.
Embodiment 2：
A kind of technique of ternary Ludox doping real silk, includes the following steps：
(1) preparation of pure silicon colloidal sol：It counts in parts by weight, 10 parts of ethyl orthosilicates, 55 parts of absolute ethyl alcohols and 220 parts are pure
Water purification is added in flask, and it is 5.2 to adjust pH value, is stirred with the speed of 300r/min, then in ultrasonication power
4.5h is reacted under conditions of being 570W for 1500W, infrared radiation power, obtains the Ludox that grain size is 30nm；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium bicarbonate is placed in high-pressure bottle
In, 53 DEG C are warming up to, starts blender, is stirred with the speed of 200r/min, is then passed through containing dioxy in high-pressure bottle
The mixed gas for changing carbon, makes the system pressure of reaction vessel rise to 6MPa, and 8 parts of phosphoric acid are added with 2g/min speed while stirring
Sodium, after addition, the reaction was continued 2.5h obtains ternary Ludox；The carbonated mixed gas is by pressing body
Product is than being 14：3：0.1 carbon dioxide, nitrogen and chlorine mixes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 550 parts of ternary Ludox, are warming up to 37
DEG C, 17min is impregnated under conditions of ultrasonication power is 1000W, then on small-sized padding machine after three pressure of double leachings,
28min is dried at 45 DEG C, then the dry 11min at 75 DEG C, finally at 110 DEG C after dry 2min, after obtaining doping treatment
Silk；The pick-up that double leachings three are pressed is 82%.
After testing, real silk, limit oxygen index 54.3% after present invention ternary Ludox doping.
Embodiment 3：
A kind of technique of ternary Ludox doping real silk, includes the following steps：
(1) preparation of pure silicon colloidal sol：It counts in parts by weight, 10 parts of ethyl orthosilicates, 65 parts of absolute ethyl alcohols and 240 parts are pure
Water purification is added in flask, and it is 5.5 to adjust pH value, is stirred with the speed of 400r/min, then in ultrasonication power
5h is reacted under conditions of being 700W for 1600W, infrared radiation power, obtains the Ludox that grain size is 70nm；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium chloride is placed in high-pressure bottle
In, 56 DEG C are warming up to, starts blender, is stirred with the speed of 190r/min, is then passed through containing dioxy in high-pressure bottle
The mixed gas for changing carbon, makes the system pressure of reaction vessel rise to 6MPa, and 7 parts of phosphoric acid are added with 2g/min speed while stirring
Sodium, after addition, the reaction was continued 3h obtains ternary Ludox；The carbonated mixed gas is by pressing volume
Than being 14：3：0.1 carbon dioxide, nitrogen and chlorine mixes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 650 parts of ternary Ludox, are warming up to 40
DEG C, 20min is impregnated under conditions of ultrasonication power is 1200W, then on small-sized padding machine after three pressure of double leachings,
33min is dried at 45 DEG C, then the dry 12min at 75 DEG C, finally at 110 DEG C after dry 2min, after obtaining doping treatment
Silk；The pick-up that double leachings three are pressed is 78%.
After testing, real silk, limit oxygen index 55.8% after present invention ternary Ludox doping.
Embodiment 4：
A kind of technique of ternary Ludox doping real silk, includes the following steps：
(1) preparation of pure silicon colloidal sol：It counts in parts by weight, 10 parts of ethyl orthosilicates, 63 parts of absolute ethyl alcohols and 260 parts are pure
Water purification is added in flask, and it is 5.5 to adjust pH value, is stirred with the speed of 450r/min, then in ultrasonication power
5.5h is reacted under conditions of being 700W for 1600W, infrared radiation power, obtains the Ludox that grain size is 70nm；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium chloride is placed in high-pressure bottle
In, 60 DEG C are warming up to, starts blender, is stirred with the speed of 160r/min, is then passed through containing dioxy in high-pressure bottle
The mixed gas for changing carbon, makes the system pressure of reaction vessel rise to 7MPa, and 8 parts of phosphoric acid are added with 2g/min speed while stirring
Sodium, after addition, the reaction was continued 2.5h obtains ternary Ludox；The carbonated mixed gas is by pressing body
Product is than being 15：3：0.1 carbon dioxide, nitrogen and chlorine mixes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 670 parts of ternary Ludox, are warming up to 40
DEG C, 24min is impregnated under conditions of ultrasonication power is 1300W, then on small-sized padding machine after three pressure of double leachings,
30min is dried at 45 DEG C, then the dry 14min at 75 DEG C, finally at 110 DEG C after dry 2min, after obtaining doping treatment
Silk；The pick-up that double leachings three are pressed is 82%.
After testing, real silk, limit oxygen index 57.2% after present invention ternary Ludox doping.
Embodiment 5：
A kind of technique of ternary Ludox doping real silk, includes the following steps：
(1) preparation of pure silicon colloidal sol：It counts in parts by weight, 10 parts of ethyl orthosilicates, 65 parts of absolute ethyl alcohols and 270 parts are pure
Water purification is added in flask, and it is 5.7 to adjust pH value, is stirred with the speed of 440r/min, then in ultrasonication power
5h is reacted under conditions of being 750W for 1700W, infrared radiation power, obtains the Ludox that grain size is 80nm；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium bicarbonate is placed in high-pressure bottle
In, 57 DEG C are warming up to, starts blender, is stirred with the speed of 200r/min, is then passed through containing dioxy in high-pressure bottle
The mixed gas for changing carbon, makes the system pressure of reaction vessel rise to 9MPa, and 9 parts of phosphoric acid are added with 2g/min speed while stirring
Sodium, after addition, the reaction was continued 2h obtains ternary Ludox；The carbonated mixed gas is by pressing volume
Than being 13：3：0.1 carbon dioxide, nitrogen and chlorine mixes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 680 parts of ternary Ludox, are warming up to 40
DEG C, 22min is impregnated under conditions of ultrasonication power is 1400W, then on small-sized padding machine after three pressure of double leachings,
32min is dried at 45 DEG C, then the dry 11min at 75 DEG C, finally at 110 DEG C after dry 2min, after obtaining doping treatment
Silk；The pick-up that double leachings three are pressed is 81%.
After testing, real silk, limit oxygen index 56.5% after present invention ternary Ludox doping.
Embodiment 6：
A kind of technique of ternary Ludox doping real silk, includes the following steps：
(1) preparation of pure silicon colloidal sol：It counts in parts by weight, 10 parts of ethyl orthosilicates, 70 parts of absolute ethyl alcohols and 300 parts are pure
Water purification is added in flask, and it is 6.5 to adjust pH value, is stirred with the speed of 500r/min, then in ultrasonication power
6h is reacted under conditions of being 800W for 2000W, infrared radiation power, obtains the Ludox that grain size is 100nm；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium bicarbonate is placed in high-pressure bottle
In, 63 DEG C are warming up to, starts blender, is stirred with the speed of 300r/min, is then passed through containing dioxy in high-pressure bottle
The mixed gas for changing carbon, makes the system pressure of reaction vessel rise to 10MPa, and 10 parts of phosphoric acid are added with 2g/min speed while stirring
Sodium, after addition, the reaction was continued 3h obtains ternary Ludox；The carbonated mixed gas is by pressing volume
Than being 20：3：0.1 carbon dioxide, nitrogen and chlorine mixes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 700 parts of ternary Ludox, are warming up to 42
DEG C, 25min is impregnated under conditions of ultrasonication power is 1500W, then on small-sized padding machine after three pressure of double leachings,
36min is dried at 45 DEG C, then the dry 15min at 75 DEG C, finally at 110 DEG C after dry 2min, after obtaining doping treatment
Silk；The pick-up that double leachings three are pressed is 85%.
After testing, real silk, limit oxygen index 56.1% after present invention ternary Ludox doping.
Above description is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, it is all the present invention suggested by technical spirit under completed same changes or modifications change, should all belong to
In the covered the scope of the claims of the present invention.
Claims (6)
1. a kind of technique of ternary Ludox doping real silk, it is characterised in that：Include the following steps：
(1) preparation of pure silicon colloidal sol：Count in parts by weight, by 10 parts of ethyl orthosilicates, 50~70 parts of absolute ethyl alcohols and 200~
300 parts of pure water are added in flask, and it is 4.8~6.5 to adjust pH value, is stirred with the speed of 200~500r/min, then
4~6h is reacted under conditions of ultrasonication power is 1200~2000W, infrared radiation power is 500~800W, is obtained
Ludox；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium chloride is placed in high-pressure bottle, rise
Temperature is started blender, is stirred with the speed of 100~300r/min, is then passed through and contains in high-pressure bottle to 50~63 DEG C
The mixed gas of carbon dioxide makes the system pressure of reaction vessel rise to 5~10MPa, is added 6 while stirring with 2g/min speed
~10 parts of sodium phosphates, after addition, the reaction was continued 2~3h obtains ternary Ludox；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 500~700 parts of ternary Ludox, are warming up to 35
~42 DEG C, 15~25min is impregnated under conditions of ultrasonication power is 800~1500W, is then passed through on small-sized padding machine
After three pressure of double leachings, finally passes through drying and processing, obtain the silk after doping treatment.
2. a kind of technique of ternary Ludox doping real silk according to claim 1, it is characterised in that：Step (2)
The carbonated mixed gas is by being 10~20 by volume：3：0.1 carbon dioxide, nitrogen and chlorine mixing
It forms.
3. a kind of technique of ternary Ludox doping real silk according to claim 1, it is characterised in that：Step (1)
Or the grain size of the Ludox described in step (2) is 20~100nm.
4. a kind of technique of ternary Ludox doping real silk according to claim 1, it is characterised in that：Step (2)
The sodium chloride can be substituted with sodium bicarbonate.
5. a kind of technique of ternary Ludox doping real silk according to claim 1, it is characterised in that：Step (3)
The technological parameter of the drying and processing is：25~36min is dried at 45 DEG C, then dry 10~15min at 75 DEG C, most
The dry 2min at 110 DEG C afterwards.
6. a kind of technique of ternary Ludox doping real silk according to claim 1, it is characterised in that：Step (3)
The pick-up that double leachings three are pressed is 75~85%.
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| CN104947499A (en) * | 2013-12-18 | 2015-09-30 | 艺康美国股份有限公司 | Silica sol, preparation equipment and method of silica sol and application of silica sol in papermaking |
| CN105401409A (en) * | 2015-11-27 | 2016-03-16 | 苏州大学 | Method for preparing durable flame retardant silk fabrics |
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