CN114934386A - P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric and preparation method thereof - Google Patents
P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric and preparation method thereof Download PDFInfo
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 101
- 239000004744 fabric Substances 0.000 title claims abstract description 101
- 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 title claims abstract description 51
- 239000003063 flame retardant Substances 0.000 title claims abstract description 50
- 229910014299 N-Si Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 34
- 239000010703 silicon Substances 0.000 claims abstract description 34
- 238000005406 washing Methods 0.000 claims abstract description 29
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 24
- 239000010954 inorganic particle Substances 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 18
- 150000003017 phosphorus Chemical class 0.000 claims abstract description 17
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002262 Schiff base Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 150000004753 Schiff bases Chemical class 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000006482 condensation reaction Methods 0.000 claims abstract description 6
- 238000005342 ion exchange Methods 0.000 claims abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 239000011574 phosphorus Substances 0.000 claims abstract description 5
- 230000018044 dehydration Effects 0.000 claims abstract description 4
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 9
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 9
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- -1 aminoethyl propyl Chemical group 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims description 5
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 claims description 3
- 125000005375 organosiloxane group Chemical group 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 description 8
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 2
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229960000892 attapulgite Drugs 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052625 palygorskite Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 235000010413 sodium alginate Nutrition 0.000 description 2
- 239000000661 sodium alginate Substances 0.000 description 2
- 229940005550 sodium alginate Drugs 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012650 click reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
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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
-
- 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
- D06M11/30—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 oxides of halogens, oxyacids of halogens or their salts, e.g. with perchlorates
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
- D06M13/5135—Unsaturated compounds containing silicon atoms
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- D—TEXTILES; PAPER
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- 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
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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 relates to a P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric and a preparation method thereof. The preparation method comprises the following steps: (1) adding 10-20 parts of phosphorus inorganic particles, 10-20 parts of silane coupling agent and 60-80 parts of organic solvent into a three-neck flask according to molar weight parts, heating the mixed solution to 50-70 ℃, carrying out ion exchange reaction, washing, filtering and drying to obtain organic silicon coated modified phosphorus inorganic particles; (2) after the cotton fabric is subjected to primary oxidation by adopting a sodium periodate solution, further modifying the cotton fabric by using a silane coupling agent and Schiff base organic siloxane to obtain organic silicon modified cotton fabric; (3) by utilizing the principle of dehydration condensation reaction, organic silicon is coated with modified phosphorus inorganic particles, organic siloxane and organic silicon modified cotton fabric, and the P-N-Si organic-inorganic hybrid flame-retardant cotton fabric is successfully prepared. The limit oxygen index of the flame-retardant cotton fabric prepared by the method is more than 26 percent.
Description
Technical Field
The invention belongs to the field of preparation of novel functional cotton fabrics, and particularly relates to a P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric and a preparation method thereof.
Background
Cotton fabric is also called cotton fabric, and is widely used in the fields of clothing fabrics, decorative fabrics, industrial fabrics and the like because of excellent wearability, such as softness, air permeability, moisture absorption, wearing comfort and wear resistance all year round. The cotton fabric takes three elements of carbon, hydrogen and oxygen as main constituent units, the limiting oxygen index of the cotton fabric is only 18.5 percent, and the cotton fabric belongs to a combustible material. After the flame is ignited, the flame spread speed is high, the heat release amount is large, the smoke release amount is large, the flame is not easy to extinguish, the safety of human life and property and the ecological environment are seriously threatened, and the application and the development of the flame in some special fields are greatly limited.
At present, researchers have done a lot of work on the flame retardant modification aspect of cotton fabrics. For example, patent CN201810069765.9 discloses a self-extinguishing flame-retardant cotton fabric and a preparation method and application thereof. The method is characterized in that a silane coupling agent/sodium alginate/silane coupling agent/ammonium polyphosphate four-layer or a silane coupling agent/ammonium polyphosphate/silane coupling agent/sodium alginate four-layer is used as a flame-retardant unit layer, and the cotton fabric is subjected to flame-retardant modification by adopting an alternate spraying mode. The prepared coated cotton fabric has high carbon forming rate and can self extinguish after being away from fire. However, the flame-retardant fabric prepared by using physical spraying as a modification means usually has the defects of poor water washing resistance, non-lasting flame-retardant effect and the like in the later use process. Therefore, patent CN201910477141.5 discloses a flame retardant cotton fabric and a preparation method thereof. The method is characterized in that Attapulgite (ATP) is grafted to the surface of cotton fabric by sulfydryl-alkene click reaction under the irradiation of ultraviolet light by using two silane coupling agents of gamma-methacryloxypropyltrimethoxysilane (KH570) and 3 mercaptopropyltrimethoxysilane (KH590) as media. Compared with the raw cotton fabric, the burning rate and the maximum smoke density of the obtained flame-retardant cotton fabric are respectively reduced by 42.39 percent and 57.81 percent, the limit oxygen index is improved by 38.3 percent, and the flame retardant property is obviously improved. However, the preparation method is complicated and too high in cost, and is not suitable for industrial preparation.
Therefore, the invention adopts simple ion exchange technology and hydrolysis condensation reaction to carry out flame retardant finishing on the cotton fabric, thereby preparing the flame retardant cotton fabric with excellent washing resistance and good flame retardant effect.
Disclosure of Invention
In view of the above, the invention aims to provide a preparation method of a P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric with simple preparation process and low cost, and the prepared P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric has good flame-retardant effect and washing resistance.
The purpose of the invention can be realized by the following technical scheme: a preparation method of P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric is characterized by comprising the following steps:
step 1: the organic silicon coated modified phosphorus inorganic particles are prepared by adopting an ion exchange technology, and the structural general formula is as follows:
wherein R1 is independently selected from methoxy or ethoxy, R2 is independently selected from aminoethyl propyl or propyl;
adding 10-20 parts of phosphorus inorganic particles, 10-20 parts of silane coupling agent and 60-80 parts of organic solvent into a three-neck flask by mol, uniformly mixing, heating the mixed solution to 50-70 ℃, and condensing and refluxing for 1-4 hours under the condition. And then repeatedly washing, filtering and drying to obtain the organic silicon coated modified phosphorus inorganic particles.
Step 2: carrying out surface modification on the cotton fabric;
5-10 parts of sodium periodate and 90-95 parts of deionized water are selected and placed in a glass container according to the molar weight. After the sodium periodate is completely dissolved, a cotton fabric of 20cm multiplied by 20cm is selected and soaked in the mixed solution. And then, heating to 30-50 ℃, reacting for 2-6 h, taking out the fabric, and repeatedly washing and drying to obtain the primarily oxidized cotton fabric. And finally, putting 10-20 parts of silane coupling agent, 5-10 parts of Schiff base organic siloxane, 70-85 parts of organic solvent and 20cm multiplied by 20cm cotton fabric into a reaction vessel together in parts by mole, heating the solution to 50-70 ℃, and carrying out condensation reflux for 4-8 h. And washing and drying to obtain the organic silicon modified cotton fabric.
And 3, step 3: preparing a P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric by using a dehydration condensation reaction principle;
according to the weight parts, 5-10 parts of organic silicon coated modified phosphorus inorganic particles, 2-5 parts of organic siloxane and 85-93 parts of organic solvent are selected and placed in a glass container. And after the organic silicon modified cotton fabric is uniformly dispersed, soaking the prepared organic silicon modified cotton fabric into a mixed solvent, raising the temperature of the solution to 70-90 ℃, reacting for 2-5 hours, washing and drying to obtain the flame-retardant cotton fabric.
Preferably, the phosphorus-based inorganic particles are ammonium polyphosphate, and the polymerization degree of the ammonium polyphosphate is 50-200.
Preferably, the silane coupling agent is any one of KH550 (gamma-aminopropyltriethoxysilane), KH602(N- (. beta. -aminoethyl) -3-aminopropylmethyldimethoxysilane) and KH792 (N- (2-aminoethyl) -3-aminopropyltrimethoxysilane).
Preferably, the Schiff base organosiloxane has a structural general formula
Wherein R1 is independently selected from methoxy or ethoxy, R2 is independently selected from aminoethyl propyl or propyl;
preferably, the organic siloxane is any one of ethyl orthosilicate and diphenyl silanediol.
Preferably, the organic solvent is any one of absolute ethyl alcohol, toluene and acetone.
The invention also provides a P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric, wherein the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric is prepared according to the preparation method.
Compared with the prior art, the invention has the following advantages:
(1) the preparation method of the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric adopts the ion exchange technology and the hydrolytic condensation reaction to carry out flame-retardant finishing on the cotton fabric, has simple process operation process and easy operation, and is beneficial to industrial production.
(2) The P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric has excellent washing resistance and good flame-retardant effect.
Drawings
FIG. 1 is a preparation route diagram of a P-N-Si series organic-inorganic flame-retardant cotton fabric.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
As shown in figure 1, the preparation method of the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric mainly comprises the following preparation processes:
step 1: the organic silicon coated modified phosphorus inorganic particles are prepared by adopting an ion exchange technology, and the structural general formula is as follows:
wherein R1 is independently selected from methoxy or ethoxy, R2 is independently selected from aminoethyl propyl or propyl;
adding 10-20 parts of phosphorus inorganic particles, 10-20 parts of silane coupling agent and 60-80 parts of organic solvent into a three-neck flask by mol parts, uniformly mixing, heating the mixed solution to 50-70 ℃, and carrying out condensation reflux for 1-4h under the condition. And then repeatedly washing, filtering and drying to obtain the organic silicon coated modified phosphorus inorganic particles.
Step 2: carrying out surface modification on the cotton fabric;
5-10 parts of sodium periodate and 90-95 parts of deionized water are selected and placed in a glass container according to the molar weight. After the sodium periodate is completely dissolved, selecting a cotton fabric of 20cm multiplied by 20cm, and soaking the cotton fabric in the mixed solution. And then, heating to 30-50 ℃, reacting for 2-6 h, taking out the fabric, and repeatedly washing and drying to obtain the primarily oxidized cotton fabric. And finally, putting 10-20 parts of silane coupling agent, 5-10 parts of Schiff base organic siloxane, 70-85 parts of organic solvent and 20cm multiplied by 20cm cotton fabric into a reaction vessel together in parts by mole, heating the solution to 50-70 ℃, and carrying out condensation reflux for 4-8 h. And washing and drying to obtain the organic silicon modified cotton fabric.
And step 3: preparing a P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric by using a dehydration condensation reaction principle;
according to the weight parts, 5-10 parts of organic silicon coated modified phosphorus inorganic particles, 2-5 parts of organic siloxane and 85-93 parts of organic solvent are selected and placed in a glass container. And after the organic silicon modified cotton fabric is uniformly dispersed, soaking the prepared organic silicon modified cotton fabric into a mixed solvent, raising the temperature of the solution to 70-90 ℃, reacting for 2-5 hours, washing and drying to obtain the flame-retardant cotton fabric.
The following are specific examples.
Example 1
1) In parts by weight, 10 parts of ammonium polyphosphate (degree of polymerization n: 80), 10 parts of KH550 (gamma-aminopropyltriethoxysilane) and 80 parts of absolute ethanol were added to a three-necked flask, and after uniform mixing, the temperature of the mixed solution was raised to 50 ℃, and under these conditions, the mixture was refluxed for 4 hours. And then repeatedly washing, filtering and drying to obtain the organic silicon coated modified phosphorus inorganic particles-I (P-Si-I).
2) 5 parts of sodium periodate and 95 parts of deionized water are selected and put into a glass container by molar weight. After the sodium periodate is completely dissolved, selecting a cotton fabric of 20cm multiplied by 20cm, and soaking the cotton fabric in the mixed solution. And then, heating the temperature to 30 ℃, taking out the fabric after 6 hours of reaction, and obtaining the primarily oxidized cotton fabric after repeated washing and drying. And finally, according to parts by mole, 20 parts of gamma-aminopropyltriethoxysilane and 10 parts of Schiff base organosiloxane-I (structural formula:
) 70 parts of absolute ethyl alcohol and 20cm multiplied by 20cm cotton fabric are placed in a reaction vessel together, the temperature of the solution is raised to 70 ℃, and the solution is condensed and refluxed for 4 hours. And washing and drying to obtain the organic silicon modified cotton fabric-I.
3) According to the weight portion, 10 portions of P-Si-I, 2 portions of ethyl orthosilicate and 88 portions of absolute ethyl alcohol are selected and placed in a glass container. After the organic silicon modified cotton fabric-I is uniformly dispersed, soaking the prepared organic silicon modified cotton fabric-I into a mixed solvent, raising the temperature of the solution to 90 ℃, reacting for 2 hours, washing and drying to obtain the flame-retardant cotton fabric-I.
The limit oxygen index of the flame-retardant cotton fabric prepared by the embodiment can reach 27.5%.
Example 2
1) 20 parts by weight of ammonium polyphosphate (degree of polymerization N is 100), 20 parts by weight of KH602(N- (. beta. -aminoethyl) -3-aminopropylmethyldimethoxysilane) and 60 parts by weight of absolute ethanol were added to a three-necked flask, and after uniform mixing, the temperature of the mixed solution was raised to 50 ℃, and under these conditions, the solution was refluxed for 4 hours. And then repeatedly washing, filtering and drying to obtain the organic silicon coated modified phosphorus inorganic particle-II (P-Si-II).
2) 5 parts of sodium periodate and 95 parts of deionized water are selected and put into a glass container by molar weight. After the sodium periodate is completely dissolved, a cotton fabric of 20cm multiplied by 20cm is selected and soaked in the mixed solution. And then, heating the temperature to 40 ℃, taking out the fabric after 5 hours of reaction, and obtaining the primarily oxidized cotton fabric after repeated washing and drying. Finally, 10 parts of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane and 5 parts of Schiff base organosiloxane-II by molar weight
85 parts of toluene and 20cm by 20cm cotton fabric are placed together in a reaction vessel, the temperature of the solution is raised to 60 ℃ and the solution is refluxed for 4 hours. The organic silicon modified cotton fabric is obtained after washing and drying-Ⅱ。
3) According to the weight portion, 10 portions of P-Si-II, 5 portions of diphenyl silanediol and 85 portions of toluene are selected and placed in a glass container. After the organic silicon modified cotton fabric-II is uniformly dispersed, soaking the prepared organic silicon modified cotton fabric-II into a mixed solvent, raising the temperature of the solution to 80 ℃, reacting for 2 hours, washing and drying to obtain the flame-retardant cotton fabric-II.
The limit oxygen index of the flame-retardant cotton fabric prepared by the embodiment can reach 28.5%.
Example 3
1) 15 parts by weight of ammonium polyphosphate (degree of polymerization n: 150), 15 parts by weight of KH550 (gamma-aminopropyltriethoxysilane) and 60 parts by weight of acetone were added to a three-necked flask, and after uniform mixing, the temperature of the mixed solution was raised to 60 ℃, and under these conditions, the mixture was refluxed for 3 hours. And then repeatedly washing, filtering and drying to obtain the organic silicon coated modified phosphorus inorganic particles-III (P-Si-III).
2) 8 parts of sodium periodate and 92 parts of deionized water are selected and placed in a glass container by molar weight. After the sodium periodate is completely dissolved, selecting a cotton fabric of 20cm multiplied by 20cm, and soaking the cotton fabric in the mixed solution. And then, heating the temperature to 50 ℃, taking out the fabric after reacting for 3 hours, and obtaining the primarily oxidized cotton fabric after repeatedly washing and drying. Finally, 15 parts of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane and 5 parts of Schiff base organosiloxane-I by molar weight
80 parts of acetone and 20cm × 20cm cotton fabric are placed together in a reaction vessel, the temperature of the solution is raised to 50 ℃, and the solution is refluxed for 4 hours. And washing and drying to obtain the organic silicon modified cotton fabric-III.
3) According to the weight portion, 10 portions of P-Si-III, 5 portions of ethyl orthosilicate and 85 portions of absolute ethyl alcohol are selected and placed in a glass container. After uniform dispersion, soaking the prepared organic silicon modified cotton fabric-III into a mixed solvent, raising the temperature of the solution to 80 ℃, reacting for 2 hours, washing and drying to obtain the flame-retardant cotton fabric-III.
The limit oxygen index of the flame-retardant cotton fabric prepared by the embodiment can reach 26.9%.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. The invention provides a preparation method of a P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric, which is characterized by comprising the following preparation routes:
step 1: the organic silicon coated modified phosphorus inorganic particles are prepared by adopting an ion exchange technology, and the structural general formula is as follows:
wherein R1 is independently selected from methoxy or ethoxy, R2 is independently selected from aminoethyl propyl or propyl;
and 2, step: carrying out surface modification on the cotton fabric; firstly, preparing preliminarily oxidized cotton fabric by using a sodium periodate solution, and then treating the cotton fabric by using a silane coupling agent and a Schiff base organic siloxane organic solvent to obtain organic silicon modified cotton fabric;
and step 3: the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric is prepared by utilizing the principle of dehydration condensation reaction.
2. The preparation method of the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric according to claim 1, wherein the preparation process of the organosilicon-coated modified phosphorus inorganic particles is as follows: adding 10-20 parts of phosphorus inorganic particles, 10-20 parts of silane coupling agent and 60-80 parts of organic solvent into a three-neck flask by mol, uniformly mixing, heating the mixed solution to 50-70 ℃, and condensing and refluxing for 1-4 hours under the condition. And then repeatedly washing, filtering and drying to obtain the organic silicon coated modified phosphorus inorganic particles.
3. The preparation method of the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric is characterized in that 5-10 parts of sodium periodate and 90-95 parts of deionized water are selected and placed in a glass container, after the sodium periodate is completely dissolved, a cotton fabric of 20cm multiplied by 20cm is selected and soaked in a mixed solution, then the temperature is raised to 30-50 ℃, the reaction is carried out for 2-6 hours, the fabric is taken out, and after repeated washing and drying, the primarily oxidized cotton fabric is obtained; and finally, putting 10-20 parts of silane coupling agent, 5-10 parts of Schiff base organic siloxane, 70-85 parts of organic solvent and 20cm multiplied by 20cm cotton fabric into a reaction vessel together in parts by mole, heating the solution to 50-70 ℃, condensing and refluxing for 4-8 h, and washing and drying to obtain the organic silicon modified cotton fabric.
4. The preparation method of the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric according to claim 1, wherein the step 3 specifically comprises the following steps: according to the weight parts, 5-10 parts of organic silicon coated modified phosphorus inorganic particles, 2-5 parts of organic siloxane and 85-93 parts of organic solvent are selected and placed in a glass container, after the organic silicon coated modified phosphorus inorganic particles and the organic siloxane are uniformly dispersed, the prepared organic silicon modified cotton fabric is immersed in a mixed solvent, the temperature of the solution is raised to 70-90 ℃, the reaction is carried out for 2-5 hours, and then the flame-retardant cotton fabric is obtained through washing and drying.
5. The method for preparing the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric according to any one of claims 1 to 4, wherein the phosphorus series inorganic particles are ammonium polyphosphate, and the polymerization degree of the ammonium polyphosphate is 50 to 200.
6. The method for preparing the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric according to any one of claims 1 to 4, wherein the silane coupling agent is any one of KH550 and KH 602.
7. According to claim1-4, the preparation method of the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric is characterized in that the structural general formula of the Schiff base organosiloxane is
Wherein R1 is independently selected from methoxy or ethoxy, R2 is independently selected from aminoethyl propyl or propyl.
8. The method for preparing the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric according to any one of claim 4, wherein the organosiloxane is any one of ethyl orthosilicate and diphenylsilanediol.
9. The method for preparing the P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric according to any one of claims 2, 3 or 4, wherein the organic solvent is any one of absolute ethyl alcohol, toluene and acetone.
10. A P-N-Si series organic-inorganic hybrid flame-retardant cotton fabric is characterized by being prepared according to the preparation method of any one of claims 1 to 9.
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