CN114737399A - Environment-friendly flame-retardant sizing mixing formula for fabric - Google Patents
Environment-friendly flame-retardant sizing mixing formula for fabric Download PDFInfo
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- CN114737399A CN114737399A CN202210532474.5A CN202210532474A CN114737399A CN 114737399 A CN114737399 A CN 114737399A CN 202210532474 A CN202210532474 A CN 202210532474A CN 114737399 A CN114737399 A CN 114737399A
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- hydrotalcite
- retardant
- polyborosiloxane
- reaction kettle
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- 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 55
- 239000003063 flame retardant Substances 0.000 title claims abstract description 55
- 239000004744 fabric Substances 0.000 title claims abstract description 37
- 238000002156 mixing Methods 0.000 title claims abstract description 32
- 238000004513 sizing Methods 0.000 title claims abstract description 18
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 74
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 74
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 50
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 26
- -1 hydrotalcite compound Chemical class 0.000 claims abstract description 24
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- 229920000609 methyl cellulose Polymers 0.000 claims abstract description 7
- 239000001923 methylcellulose Substances 0.000 claims abstract description 7
- 235000010981 methylcellulose Nutrition 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 45
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 17
- 239000004327 boric acid Substances 0.000 claims description 17
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 14
- 229920002545 silicone oil Polymers 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000004753 textile Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 230000002687 intercalation Effects 0.000 claims description 5
- 238000009830 intercalation Methods 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 239000003377 acid catalyst Substances 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 12
- 229910002923 B–O–B Inorganic materials 0.000 abstract description 5
- 229910002808 Si–O–Si Inorganic materials 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 16
- 239000010410 layer Substances 0.000 description 13
- 230000006872 improvement Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 7
- 239000000779 smoke Substances 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 230000001988 toxicity Effects 0.000 description 6
- 231100000419 toxicity Toxicity 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 230000004888 barrier function Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 229920004933 Terylene® Polymers 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000010559 graft polymerization reaction Methods 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical group [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000009987 spinning Methods 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
-
- 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
- D06M11/73—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 carbon or compounds thereof
- D06M11/76—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 carbon or compounds thereof with carbon oxides or carbonates
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/05—Cellulose or derivatives thereof
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
-
- 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 & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides an environment-friendly flame-retardant sizing and size mixing formula for fabric, which comprises, by weight, 100 parts of a polyborosiloxane grafted hydrotalcite compound, 40-60 parts of polyacrylamide, 1-3 parts of polyethylene glycol, 10-20 parts of methyl cellulose and 10-30 parts of a solvent. The polyborosiloxane grafted hydrotalcite composite and the polyacrylamide are used as main components, the polyborosiloxane grafted hydrotalcite composite contains Si-O-Si, Si-O-B and B-O-B bonds, the polyborosiloxane is condensed with hydroxyl of hydrotalcite to realize grafting, and hydrotalcite layers contain moisture and a large amount of hydroxyl.
Description
Technical Field
The invention relates to the technical field of flame-retardant sizing agents, in particular to an environment-friendly flame-retardant sizing agent mixing formula for fabrics.
Background
The fabric is closely related to the life of people, such as the fields of clothing, carpets, sofas and the like, and therefore, the improvement of the flame retardance of the fabric to reduce the harm of fire to human life has important significance. Flame resistant fabrics are fabrics that prevent ignition or retard and terminate combustion when exposed to a flame or hot object. The flame retardance of the fabric can be realized by adding a flame retardant into the spinning solution or carrying out flame retardance sizing and finishing. The flame-retardant cost of after-finishing is low, and the fabric has flame retardant property through the flame retardant effect of the flame retardant. The flame retardant performance of the post-finishing flame retardant fabric depends on the flame retardant effect of the flame retardant, so the quality of the flame retardant directly determines the quality of the flame retardant of the post-finishing flame retardant fabric. Patent CN201510337327.2 discloses an anti-dripping flame-retardant polyester fabric compound and a preparation method thereof, wherein the anti-dripping flame-retardant polyester fabric is obtained by padding polyester fabric in a flame-retardant additive and anti-dripping additive dispersion liquid. Wherein the anti-dripping additive comprises a boron-containing auxiliary agent, a polyhydroxy compound capable of complexing with boron, a phosphorus-containing flame-retardant adhesive and an organic silicon cross-linking agent; the complex reaction of boron and polyhydroxy and the crosslinking reaction of organosilicon crosslinking agent and hydroxyl are utilized to make polyhydroxy compound form a space network structure, and the space network structure is tightly bonded on the surface of terylene by phosphorus-containing adhesive. When meeting flame, the polyhydroxy compound is rapidly dehydrated into carbon under the multiple catalytic dehydration action of the phosphorus-containing flame retardant, the phosphorus-containing adhesive and the flame-retardant terylene, and a space reticular carbon layer with a compact structure is formed, so that the flame-retardant terylene can effectively resist flame and dripping. However, the combustion improver added with phosphorus has high volatility, poor heat resistance and poor compatibility, and has certain toxicity to human bodies due to generation of drops during combustion.
In view of the above, there is a need to design an improved environment-friendly flame-retardant sizing formula for fabric to solve the above problems.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an environment-friendly flame-retardant sizing mixing formula for fabrics, which takes a polyborosiloxane grafted hydrotalcite compound and polyacrylamide as main components, wherein the polyborosiloxane grafted hydrotalcite compound has high flame retardance, can quickly form an inorganic oxygen-insulating and heat-insulating protective layer during combustion, has low smoke toxicity, is green and environment-friendly and is suitable for flame retardance of textiles.
In order to achieve the purpose, the invention provides an environment-friendly flame-retardant sizing and size mixing formula for textile, which comprises 100 parts by weight of polyborosiloxane grafted hydrotalcite compound, 40-60 parts by weight of polyacrylamide, 1-3 parts by weight of polyethylene glycol, 10-20 parts by weight of methyl cellulose and 10-30 parts by weight of solvent.
As a further improvement of the invention, the addition amount of the polyacrylamide is 45-55 parts.
As a further improvement of the invention, the solvent is one or more of water, ethanol and acetone.
As a further improvement of the present invention, the mass ratio of the polyborosiloxane to the hydrotalcite in the polyborosiloxane grafted hydrotalcite composite is 1: (0.2-0.5).
As a further improvement of the invention, the polyborosiloxane is obtained by reacting methyl triethoxysilane, hydroxy silicone oil and boric acid.
As a further improvement of the invention, the mass ratio of the methyl triethoxysilane to the hydroxyl silicone oil to the boric acid is 1: (0.1-0.3): (0.3-0.6).
As a further improvement of the present invention, the method for preparing the polyborosiloxane grafted hydrotalcite composite comprises:
s1, placing hydrotalcite in a first-stage high-pressure reaction kettle, and introducing high-temperature high-pressure superheated steam for staying for 1-3 min;
s2, adding methyl triethoxysilane, hydroxyl silicone oil and boric acid into the aqueous solution, and then placing the aqueous solution into a second-stage high-pressure reaction kettle;
s3, introducing the hydrotalcite treated in the step S1 into the second-stage high-pressure reaction kettle to perform intercalation, grafting and polymerization reactions to obtain a polyborosiloxane grafted hydrotalcite compound; the temperature and the pressure of the second-stage high-pressure reaction kettle are lower than those of the first-stage high-pressure reaction kettle.
As a further improvement of the invention, the temperature of the first-stage high-pressure reaction kettle is 150-220 ℃, and the pressure is 1.5-2 MPa; the temperature of the second-stage high-pressure reaction kettle is 70-90 ℃, and the pressure is 0.2-1 MPa.
As a further improvement of the invention, the temperature of the first-stage high-pressure reaction kettle is 180-200 ℃, and the pressure is 1.6-1.8 MPa; the temperature of the second-stage high-pressure reaction kettle is 80-90 ℃, and the pressure is 0.3-0.6 MPa. As a further improvement of the invention, the aqueous solution also contains an acid catalyst.
The invention has the beneficial effects that:
1. the invention provides an environment-friendly flame-retardant slashing size mixing formula for fabrics, which takes a polyborosiloxane grafted hydrotalcite compound and polyacrylamide as main components, wherein the polyborosiloxane grafted hydrotalcite compound contains Si-O-Si, Si-O-B and B-O-B bonds, the polyborosiloxane is condensed with hydroxyl of hydrotalcite to realize grafting, and the hydrotalcite layers contain water and a large amount of hydroxyl.
2. According to the environment-friendly flame-retardant slashing size mixing formula for the fabric, provided by the invention, hydrotalcite permeates into the layers of hydrotalcite in a first-stage high-pressure reaction kettle under high temperature and high pressure, when the hydrotalcite enters a second-stage high-pressure reaction kettle, due to sudden drop of temperature and pressure, instantaneous pressure release is realized, so that internal water vapor is released to peel the hydrotalcite to a certain extent, and simultaneously, methyltriethoxysilane, hydroxyl silicone oil and boric acid in the second-stage high-pressure reaction kettle conveniently enter the layers to perform polycondensation reaction, and alkoxy and hydroxyl can be grafted with hydroxyl on the hydrotalcite.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in detail with reference to specific embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme of the present invention are shown in the specific embodiments, and other details not closely related to the present invention are omitted.
In addition, it is also to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The environment-friendly flame-retardant sizing and mixing formula for the textile comprises, by weight, 100 parts of a polyborosiloxane grafted hydrotalcite compound, 40-60 parts of polyacrylamide, 1-3 parts of polyethylene glycol, 10-20 parts of methyl cellulose and 10-30 parts of a solvent. Preferably, the addition amount of the polyacrylamide is 45-55 parts. Preferably, the composite material comprises, by weight, 100 parts of a polyborosiloxane grafted hydrotalcite composite, 45-55 parts of polyacrylamide, 2-3 parts of polyethylene glycol, 12-18 parts of methylcellulose and 15-20 parts of a solvent.
By the operation, the polyborosiloxane grafted hydrotalcite compound contains Si-O-Si, Si-O-B and B-O-B bonds, the polyborosiloxane is grafted by the condensation of hydroxyl of hydrotalcite, and hydrotalcite layers contain moisture and a large amount of hydroxyl.
The solvent is one or more of water, ethanol and acetone, and is preferably water.
The mass ratio of the polyborosiloxane to the hydrotalcite in the polyborosiloxane grafted hydrotalcite compound is 1: (0.2-0.5), preferably 1: (0.3-0.4). When the content of the hydrotalcite is too much, the uniformity and the film forming property of the slurry are not favorably improved, and the high-strength and compact ceramic barrier layer is formed by the polyborosiloxane and the hydrotalcite during combustion through a proper composite proportion.
The polyborosiloxane is prepared from the following components in a mass ratio of 1: (0.1-0.3): (0.3-0.6) methyl triethoxysilane, hydroxy silicone oil and boric acid. The mass ratio is preferably 1: (0.2-0.3): (0.4-0.5). The appropriate amount of boric acid facilitates the formation of Si-O-B and B-O-B bonds.
The preparation method of the polyborosiloxane grafted hydrotalcite compound comprises the following steps:
s1, placing hydrotalcite in a first-stage high-pressure reaction kettle, and introducing high-temperature high-pressure superheated steam for staying for 1-3 min; s2, adding methyl triethoxysilane, hydroxyl silicone oil and boric acid into the aqueous solution, and then placing the aqueous solution into a second-stage high-pressure reaction kettle; preferably, the aqueous solution further comprises an acid catalyst.
S3, introducing the hydrotalcite treated in the step S1 into the second-stage high-pressure reaction kettle to perform intercalation, grafting and polymerization reactions to obtain a polyborosiloxane grafted hydrotalcite compound; the temperature and the pressure of the second-stage high-pressure reaction kettle are lower than those of the first-stage high-pressure reaction kettle.
By the operation, high-temperature high-pressure superheated steam permeates into the layers of the hydrotalcite in the first-stage high-pressure reaction kettle, when the hydrotalcite enters the second-stage high-pressure reaction kettle, due to sudden drop of temperature and pressure, instantaneous pressure release is realized, so that internal steam is released to peel the hydrotalcite to a certain extent, and simultaneously, methyltriethoxysilane, hydroxyl silicone oil and boric acid in the second-stage high-pressure reaction kettle conveniently enter the layers to perform polycondensation reaction, and alkoxy and hydroxyl can be grafted with hydroxyl on the hydrotalcite, so that the obtained polyborosiloxane grafted hydrotalcite composite has high grafting rate and increased interlayer spacing, and has obvious high barrier property as a combustion improver.
The temperature of the first-stage high-pressure reaction kettle is 150-; the temperature of the second-stage high-pressure reaction kettle is 70-90 ℃, and the pressure is 0.2-1 MPa.
Preferably, the temperature of the first-stage high-pressure reaction kettle is 180-; the temperature of the second-stage high-pressure reaction kettle is 80-90 ℃, and the pressure is 0.3-0.6 MPa.
Example 1
An environment-friendly flame-retardant sizing mixing formula for fabric comprises, by weight, 100 parts of a polyborosiloxane grafted hydrotalcite compound, 50 parts of polyacrylamide, 2.5 parts of polyethylene glycol, 15 parts of methyl cellulose and 18 parts of solvent water. Mixing the components, and then padding and sizing the cotton fabric to obtain the flame-retardant cotton fabric.
The preparation method of the polyborosiloxane grafted hydrotalcite composite comprises the following steps:
s1, placing hydrotalcite in a first-stage high-pressure reaction kettle, and introducing high-temperature high-pressure superheated steam for staying for 2 min; the temperature of the first-stage high-pressure reaction kettle is 180 ℃, and the pressure is 1.8 MPa;
s2, mixing the components in a mass ratio of 1: 0.2: 0.5 of methyl triethoxysilane, hydroxyl silicone oil and boric acid are added into the water solution and then placed in a second-stage high-pressure reaction kettle; the temperature of the second-stage high-pressure reaction kettle is 80 ℃, and the pressure is 0.5 MPa. The total mass ratio of the hydrotalcite to the methyltriethoxysilane, the hydroxyl silicone oil and the boric acid is 0.4: 1.
And S3, introducing the hydrotalcite treated in the step S1 into the second-stage high-pressure reaction kettle to perform intercalation, grafting and polymerization reactions, so as to obtain the polyborosiloxane grafted hydrotalcite compound.
Example 2
Compared with the example 1, the environment-friendly flame-retardant slashing size mixing formula for the fabric is different from the formula in that the size mixing formula comprises 100 parts by weight of a polyborosiloxane grafted hydrotalcite compound, 40 parts by weight of polyacrylamide, 1 part by weight of polyethylene glycol, 10 parts by weight of methyl cellulose and 12 parts by weight of solvent water. The rest is substantially the same as that of embodiment 1, and will not be described herein.
Comparative example 1
Compared with the example 1, the difference of the environment-friendly flame-retardant slashing size mixing formula for the fabric is that the polyborosiloxane grafted hydrotalcite composite is replaced by the polyborosiloxane and hydrotalcite which are not grafted. The rest is substantially the same as that of embodiment 1, and will not be described herein.
Comparative example 2
Compared with the example 1, the difference of the environment-friendly flame-retardant sizing and size mixing formula for the textile is that the preparation method of the polyborosiloxane grafted hydrotalcite compound comprises the following steps: mixing the components in a mass ratio of 1: 0.2: 0.5 of methyltriethoxysilane, hydroxysilicone oil and boric acid were added to the aqueous solution, followed by addition of hydrotalcite and reaction at 80 ℃ and normal pressure.
The rest is substantially the same as that of embodiment 1, and will not be described herein.
Comparative example 3
Compared with the example 1, the difference of the environment-friendly flame-retardant sizing and size mixing formula for the textile is that the preparation method of the polyborosiloxane grafted hydrotalcite compound comprises the following steps:
s1, placing hydrotalcite in a first-stage high-pressure reaction kettle, and introducing high-temperature high-pressure superheated steam for staying for 2 min; the temperature of the first-stage high-pressure reaction kettle is 180 ℃, and the pressure is 1.8 MPa;
s2, introducing the hydrotalcite treated in the step S1 into a second-stage high-pressure reaction kettle to stay for 20min to obtain stripped hydrotalcite; the temperature of the second-stage high-pressure reaction kettle is 80 ℃, and the pressure is 0.5 MPa;
s3, mixing the components in a mass ratio of 1: 0.2: 0.5 of methyltriethoxysilane, a hydroxy silicone oil and boric acid were added to the aqueous solution, and then the exfoliated hydrotalcite obtained in step S2 was added, and condensation polymerization and grafting were carried out to obtain a polyborosiloxane grafted hydrotalcite composite.
The rest is substantially the same as that of embodiment 1, and will not be described herein.
Comparative example 4
Compared with the example 1, the difference of the environment-friendly flame-retardant sizing mixing formula for the fabric is that boric acid is not added in the step S2. The rest is substantially the same as that of embodiment 1, and will not be described herein.
Comparative example 5
Compared with the example 1, the difference of the environment-friendly flame-retardant sizing mixing formula for the textile fabric is that the polyborosiloxane grafted hydrotalcite compound is replaced by polyborosiloxane. The rest is substantially the same as that of embodiment 1, and will not be described herein.
TABLE 1 test results of examples 1-2 and comparative examples 1-5
| Test specimen | Limiting oxygen index (%) | Smoke density rating | Grade of smoke toxicity |
| Example 1 | 35.6 | 9.8 | AQ2 |
| Example 2 | 35.1 | 10.1 | AQ2 |
| Comparative example 1 | 32.5 | 11.2 | ZA1 |
| Comparative example 2 | 33.6 | 10.8 | ZA1 |
| Comparative example 3 | 33.8 | 10.5 | AQ2 |
| Comparative example 4 | 33.3 | 10.8 | AQ2 |
| Comparative example 5 | 30.1 | 12.3 | ZA1 |
As can be seen from the table 1, the slashing formula provided by the invention can obviously improve the limited oxygen index of the fabric, and has low smoke density and toxicity, so that the slashing formula is high in safety and good in flame retardant effect. In contrast, in comparative example 1, when the polyborosiloxane and the hydrotalcite are not grafted, the limiting oxygen index is reduced, the smoke density grade is increased, and the smoke toxicity is improved, which shows that the grafting of the polyborosiloxane and the hydrotalcite is helpful for forming a composite ceramic barrier layer, so that the heat insulation and flame retardance are improved, the smoke release amount is reduced, and the structure of a release object is improved, so that the toxicity is reduced. In comparative example 2, the conventional graft polymerization method is adopted, the flame retardant effect is not the same as that of the invention, and the invention adopts special steam explosion intercalation and grafting, which is beneficial to improving the grafting rate and grafting uniformity, and simultaneously enables the polyborosiloxane to be interpenetrated between layers, thereby improving the compactness of the barrier layer. In comparative example 3, the flame retardant effect is also reduced by first blasting and peeling and then graft polymerization. Comparative example 4, in which boric acid was not added, the flame retardant effect was also reduced, indicating that the silicon boron chain contributes to the improvement of the flame retardancy of the compound. In the comparative example 5, when no hydrotalcite is added, the flame retardant effect is remarkably reduced, which shows that the polyborosiloxane and the hydrotalcite are compounded to be beneficial to forming a compact barrier ceramic layer, thereby realizing high-efficiency flame retardant.
In conclusion, the environment-friendly flame-retardant sizing and mixing formula for the textile provided by the invention takes the polyborosiloxane grafted hydrotalcite compound and the polyacrylamide as main components, the polyborosiloxane grafted hydrotalcite compound contains Si-O-Si, Si-O-B and B-O-B bonds, the polyborosiloxane is condensed with hydroxyl of hydrotalcite to realize grafting, and the hydrotalcite layers contain moisture and a large amount of hydroxyl.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (10)
1. An environment-friendly flame-retardant sizing mixing formula for textile fabrics is characterized by comprising, by weight, 100 parts of polyborosiloxane grafted hydrotalcite compound, 40-60 parts of polyacrylamide, 1-3 parts of polyethylene glycol, 10-20 parts of methyl cellulose and 10-30 parts of solvent.
2. The environment-friendly flame-retardant slashing size mixing formula for the fabric according to claim 1, wherein the addition amount of the polyacrylamide is 45-55 parts.
3. The environment-friendly flame-retardant slashing size mixing formula for the fabric according to claim 1, wherein the solvent is one or more of water, ethanol and acetone.
4. The environment-friendly flame-retardant slashing size mixing formula for fabrics according to claim 1, wherein the mass ratio of the polyborosiloxane to the hydrotalcite in the polyborosiloxane grafted hydrotalcite compound is 1: (0.2-0.5).
5. The environmentally friendly flame retardant slashing size mixing formula for fabric according to claim 4, wherein the polyborosiloxane is obtained by reacting methyltriethoxysilane, hydroxy silicone oil and boric acid.
6. The environment-friendly flame-retardant slashing size mixing formula for the fabric according to claim 5, wherein the mass ratio of the methyltriethoxysilane to the hydroxy silicone oil to the boric acid is 1: (0.1-0.3): (0.3-0.6).
7. The environmentally friendly flame retardant slashing size mixing formula for fabric according to claim 5, wherein the preparation method of the polyborosiloxane grafted hydrotalcite compound comprises the following steps:
s1, placing hydrotalcite in a first-stage high-pressure reaction kettle, and introducing high-temperature high-pressure superheated steam for staying for 1-3 min;
s2, adding methyl triethoxysilane, hydroxyl silicone oil and boric acid into the aqueous solution, and then placing the aqueous solution into a second-stage high-pressure reaction kettle;
s3, introducing the hydrotalcite treated in the step S1 into the second-stage high-pressure reaction kettle to perform intercalation, grafting and polymerization reactions to obtain a polyborosiloxane grafted hydrotalcite compound; the temperature and the pressure of the second-stage high-pressure reaction kettle are lower than those of the first-stage high-pressure reaction kettle.
8. The environment-friendly flame-retardant slashing size mixing formula for fabric as claimed in claim 7, wherein the temperature of the first-stage high-pressure reaction kettle is 150-220 ℃, and the pressure is 1.5-2 MPa; the temperature of the second-stage high-pressure reaction kettle is 70-90 ℃, and the pressure is 0.2-1 MPa.
9. The environment-friendly flame-retardant slashing size mixing formula for fabric according to claim 8, wherein the temperature of the first-stage high-pressure reaction kettle is 180-; the temperature of the second-stage high-pressure reaction kettle is 80-90 ℃, and the pressure is 0.3-0.6 MPa.
10. The environmentally friendly flame retardant slashing size mixing formulation for fabric according to claim 7, wherein the aqueous solution further comprises an acid catalyst.
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