CN108277639A - A kind of technique of quaternary Ludox doping real silk - Google Patents
A kind of technique of quaternary Ludox doping real silk Download PDFInfo
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- CN108277639A CN108277639A CN201810141814.5A CN201810141814A CN108277639A CN 108277639 A CN108277639 A CN 108277639A CN 201810141814 A CN201810141814 A CN 201810141814A CN 108277639 A CN108277639 A CN 108277639A
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- Prior art keywords
- ludox
- parts
- quaternary
- real silk
- doping
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 26
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims abstract description 23
- 238000002525 ultrasonication Methods 0.000 claims abstract description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 20
- 238000002386 leaching Methods 0.000 claims abstract description 19
- 238000010792 warming Methods 0.000 claims abstract description 18
- 230000004048 modification Effects 0.000 claims abstract description 12
- 238000012986 modification Methods 0.000 claims abstract description 12
- 239000011780 sodium chloride Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011701 zinc Substances 0.000 claims abstract description 10
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 5
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 26
- 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 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 13
- 239000001569 carbon dioxide Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 11
- 229910052801 chlorine Inorganic materials 0.000 claims description 11
- 239000000460 chlorine Substances 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 230000005855 radiation Effects 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 9
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical class CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 claims description 9
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 9
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 11
- 239000001301 oxygen Substances 0.000 abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 abstract description 11
- 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
- 238000000746 purification Methods 0.000 description 7
- 238000012360 testing method Methods 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
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 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
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 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
- MXSJNBRAMXILSE-UHFFFAOYSA-N [Si].[P].[B] Chemical compound [Si].[P].[B] MXSJNBRAMXILSE-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
- CUXQLKLUPGTTKL-UHFFFAOYSA-M microcosmic salt Chemical compound [NH4+].[Na+].OP([O-])([O-])=O CUXQLKLUPGTTKL-UHFFFAOYSA-M 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
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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
-
- 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
- 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
- D06M11/80—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 boron or compounds thereof, e.g. borides
- D06M11/82—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 boron or compounds thereof, e.g. borides with boron oxides; with boric, meta- or perboric acids or their salts, e.g. with borax
-
- 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)
- Cosmetics (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Silicon Compounds (AREA)
- Peptides Or Proteins (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses the techniques that a kind of quaternary 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, are warming up to 50~63 DEG C, stirring, it is passed through carbonated mixed gas, so that pressure is risen to 4~8MPa, disodium hydrogen phosphate is added while stirring, nano-zinc borate is added simultaneously, the reaction was continued 2~3h obtains quaternary Ludox；(3) it adulterates：Real silk is immersed in quaternary Ludox, 40~48 DEG C are warming up to, 10~20min is impregnated under conditions of ultrasonication power is 800~1500W, then on small-sized padding machine after three pressure of double leachings, finally pass through drying and processing, 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 quaternary 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 fire-retardant raw material to be adulterated in real silk, but this method is to the flame retardant property increase rate of real silk
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 quaternary Ludox doping real silk is provided, it is molten that the present invention first prepares pure silicon
Glue；Then Ludox is modified, prepares quaternary Ludox；Finally under the subsidiary conditions of ultrasonication, by quaternary 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 quaternary 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 4~8MPa, is added while stirring with 2g/min speed
Enter 4~8 parts of disodium hydrogen phosphates, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued
2~3h obtains quaternary Ludox；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 500~700 parts of quaternary Ludox, heat up
To 40~48 DEG C, 10~20min 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.
Zinc borate is used to be grafted Ludox in the present invention, generates quaternary Ludox.
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 quaternary 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, zinc borate and sodium chloride.Under the condition of high voltage of the mixed gas containing carbon dioxide, in carbon dioxide and chlorine
Portion gas can dissolve in water, form acid liquid environment,, will using strong external force then under the effect of the high pressure of nitrogen
Sodium phosphate, zinc borate and sodium chloride are grafted in Ludox system, form the quaternary Ludox containing silicon-phosphorus-boron system.
3. doping method of the present invention can efficiently be doped into quaternary Ludox in the structure of real silk.This
Invention is enable quaternary Ludox under the continuous effect of vibration of ultrasonic wave, is promoted quaternary 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 quaternary 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 4MPa, and 4 parts of phosphoric acid hydrogen are added with 2g/min speed while stirring
Disodium, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued 2h obtains quaternary silicon
Colloidal sol；The carbonated mixed gas is by being 10 by volume：3：0.1 carbon dioxide, nitrogen and chlorine is mixed
It closes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 500 parts of quaternary Ludox, are warming up to 40
DEG C, 10min 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, double leachings three pressure pick-up be 75%.
After testing, real silk, limit oxygen index 59.1% after present invention ternary Ludox doping.
Embodiment 2：
A kind of technique of quaternary 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, 52 parts of absolute ethyl alcohols and 240 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 550W for 1500W, 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, 53 DEG C are warming up to, starts blender, is stirred with the speed of 180r/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 hydrogen are added with 2g/min speed while stirring
Disodium, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued 2.5h obtains quaternary
Ludox；The carbonated mixed gas is by being 16 by volume：3：0.1 carbon dioxide, nitrogen and chlorine
It mixes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 580 parts of quaternary Ludox, are warming up to 42
DEG C, 16min is impregnated under conditions of ultrasonication power is 1100W, then on small-sized padding machine after three pressure of double leachings,
28min is dried at 45 DEG C, then the dry 13min at 75 DEG C, finally at 110 DEG C after dry 2min, after obtaining doping treatment
Silk, double leachings three pressure pick-up be 78%.
After testing, real silk, limit oxygen index 58.8% after present invention ternary Ludox doping.
Embodiment 3：
A kind of technique of quaternary 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, 59 parts of absolute ethyl alcohols and 250 parts are pure
Water purification is added in flask, and it is 5.6 to adjust pH value, is stirred with the speed of 400r/min, then in ultrasonication power
5.5h is reacted under conditions of being 700W for 1700W, infrared radiation power, obtains the Ludox that grain size is 50nm；
(2) modification of Ludox：It counts in parts by weight, 100 parts of Ludox and 0.1 part of sodium chloride or sodium bicarbonate is placed in
In high-pressure bottle, 54 DEG C are warming up to, starts blender, is stirred with the speed of 240r/min, is then led in high-pressure bottle
Enter carbonated mixed gas, the system pressure of reaction vessel is made to rise to 7MPa, is added 5 while stirring with 2g/min speed
Part disodium hydrogen phosphate, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued 3h is obtained
To quaternary Ludox；The carbonated mixed gas is by being 18 by volume：3：0.1 carbon dioxide, nitrogen
It is mixed with chlorine；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 600 parts of quaternary Ludox, are warming up to 44
DEG C, 18min is impregnated under conditions of ultrasonication power is 1200W, 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, double leachings three pressure pick-up be 80%.
After testing, real silk, limit oxygen index 58.9% after present invention ternary Ludox doping.
Embodiment 4：
A kind of technique of quaternary 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, 60 parts of absolute ethyl alcohols and 280 parts are pure
Water purification is added in flask, and it is 5.6 to adjust pH value, is stirred with the speed of 290r/min, then in ultrasonication power
5.5h is reacted under conditions of being 750W for 1500W, 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 bicarbonate is placed in high-pressure bottle
In, 60 DEG C are warming up to, starts blender, is stirred with the speed of 140r/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 5 parts of phosphoric acid hydrogen are added with 2g/min speed while stirring
Disodium, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued 2.5h obtains quaternary
Ludox；The carbonated mixed gas is by being 18 by volume：3：0.1 carbon dioxide, nitrogen and chlorine
It mixes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 560 parts of quaternary Ludox, are warming up to 43
DEG C, 14min is impregnated under conditions of ultrasonication power is 1100W, then on small-sized padding machine after three pressure of double leachings,
35min 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, double leachings three pressure pick-up be 81%.
After testing, real silk, limit oxygen index 59.0% after present invention ternary Ludox doping.
Embodiment 5：
A kind of technique of quaternary 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 230 parts are pure
Water purification is added in flask, and it is 5.8 to adjust pH value, is stirred with the speed of 300r/min, then in ultrasonication power
4.5h is reacted under conditions of being 650W for 1800W, 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, 59 DEG C are warming up to, starts blender, is stirred with the speed of 170r/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 7 parts of phosphoric acid hydrogen are added with 2g/min speed while stirring
Disodium, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued 3h obtains quaternary silicon
Colloidal sol；The carbonated mixed gas is by being 12 by volume：3：0.1 carbon dioxide, nitrogen and chlorine is mixed
It closes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 590 parts of quaternary Ludox, are warming up to 43
DEG C, 17min is impregnated under conditions of ultrasonication power is 900W, then on small-sized padding machine after three pressure of double leachings,
30min 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, double leachings three pressure pick-up be 79%.
After testing, real silk, limit oxygen index 59.4% after present invention ternary Ludox doping.
Embodiment 6：
A kind of technique of quaternary 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, 66 parts of absolute ethyl alcohols and 280 parts are pure
Water purification is added in flask, and it is 6.2 to adjust pH value, is stirred with the speed of 450r/min, then in ultrasonication power
5h is reacted under conditions of being 730W for 1300W, infrared radiation power, obtains the Ludox that grain size is 40nm；
(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, 61 DEG C are warming up to, starts blender, is stirred with the speed of 250r/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 hydrogen are added with 2g/min speed while stirring
Disodium, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued 2h obtains quaternary silicon
Colloidal sol；The carbonated mixed gas is by being 15 by volume：3：0.1 carbon dioxide, nitrogen and chlorine is mixed
It closes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 680 parts of quaternary Ludox, are warming up to 42
DEG C, 13min is impregnated under conditions of ultrasonication power is 1400W, then on small-sized padding machine after three pressure of double leachings,
29min 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, double leachings three pressure pick-up be 78%.
After testing, real silk, limit oxygen index 59.0% after present invention ternary Ludox doping.
Embodiment 7：
A kind of technique of quaternary 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 chloride 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 8MPa, and 8 parts of phosphoric acid hydrogen are added with 2g/min speed while stirring
Disodium, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued 3h obtains quaternary silicon
Colloidal sol；The carbonated mixed gas is by being 20 by volume：3：0.1 carbon dioxide, nitrogen and chlorine is mixed
It closes；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 700 parts of quaternary Ludox, are warming up to 48
DEG C, 20min 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, double leachings three pressure pick-up be 85%.
After testing, real silk, limit oxygen index 58.9% 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 quaternary 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 4~8MPa, is added 4 while stirring with 2g/min speed
~8 parts of disodium hydrogen phosphates, while nano-zinc borate is added with the speed of 1.5g/min, all after addition, the reaction was continued 2~
3h obtains quaternary Ludox；
(3) it adulterates：It counts in parts by weight, 10 parts of real silks is immersed in 500~700 parts of quaternary Ludox, are warming up to 40
~48 DEG C, 10~20min 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 quaternary 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 quaternary 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 quaternary 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 quaternary 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 quaternary 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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| CN109338482A (en) * | 2018-09-21 | 2019-02-15 | 苏州经贸职业技术学院 | A kind of preparation method of nanocomposite degumming and refining agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 张强华: ""改性硼硅溶胶对真丝织物的阻燃整理及其性能研究"，张强华，《中国优秀硕士学位论文全文数据库 工程科技I辑》，2017年第01期，第B024-53页", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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| CN109338482A (en) * | 2018-09-21 | 2019-02-15 | 苏州经贸职业技术学院 | A kind of preparation method of nanocomposite degumming and refining agent |
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