CN112175136A - Reactive flame-retardant fabric modifier - Google Patents
Reactive flame-retardant fabric modifier Download PDFInfo
- Publication number
- CN112175136A CN112175136A CN202011249617.9A CN202011249617A CN112175136A CN 112175136 A CN112175136 A CN 112175136A CN 202011249617 A CN202011249617 A CN 202011249617A CN 112175136 A CN112175136 A CN 112175136A
- Authority
- CN
- China
- Prior art keywords
- weight
- finishing
- emulsion
- parts
- modifier
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
- C08F230/085—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon the monomer being a polymerisable silane, e.g. (meth)acryloyloxy trialkoxy silanes or vinyl trialkoxysilanes
-
- 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
- D06M15/356—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
- D06M15/3568—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms containing silicon
-
- 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
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
-
- 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
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a reactive flame-retardant fabric modifier, which comprises the following steps: (1) adding 1-allyl benzotriazole, vinyl (trifluoromethyl) dimethylsilane, a third monomer, an emulsifier, carboxymethyl cellulose, 1-allyl piperazine, an antistatic agent and deionized water into a reaction kettle, introducing nitrogen, stirring to obtain an emulsion 1, stirring the emulsion 1 while heating for reaction, simultaneously dropwise adding an initiator aqueous solution into the emulsion, and continuing to react after dropwise adding at a constant speed to obtain a seed emulsion; (2) mixing allyl magnesium bromide, a double-bond silane coupling agent, dodecyl mercaptan, AIBN and water uniformly in a container, then dripping into the seed emulsion at a constant speed, and continuing to keep the temperature and react fully after dripping to obtain the reactive flame-retardant fabric modifier. The fabric modifier prepared by the invention has the advantages of functions, stable and durable performance and excellent flame retardant effect.
Description
Technical Field
The invention relates to the field of textile auxiliaries, in particular to a reactive flame-retardant textile modifier.
Background
Various modifiers can be used in the processing process of the textile, so that the textile has various special functions and styles, such as softness, crease resistance, shrinkproof property, water resistance, bacteria resistance and the like, the dyeing and finishing process can be improved, the effects of saving energy and reducing processing cost are achieved, the grade and the added value of the textile are improved, and the textile auxiliary is very important for improving the overall level of the textile industry and the effect in the textile industry chain.
Because the fabric is very easy to be stained with pollutants such as oil, pigment, fruit juice and the like, the surface of the fabric becomes dirty and is difficult to clean, so that the fabric modifying agent is required to endow the fabric with the functions; because fabrics are extremely flammable and affect the safety of people's lives and properties, there is a need for fabric modifiers that impart flame retardant properties to fabrics.
Patent CN201810468207.X discloses an ultraviolet-resistant flame-retardant multifunctional coating fabric finishing agent, which comprises the following components in parts by weight: 10-15 parts of ammonium polyphosphate, 5-8 parts of chitosan, 6-8 parts of fullerene nano carbon material, 4-6 parts of nano titanium dioxide, 4-6 parts of nano zinc oxide, 5-6 parts of polydimethylsiloxane, 3-5 parts of modified polysiloxane, 8-10 parts of toluene, 1-2 parts of organic silicon emulsion, 0.3-0.5 part of gamma-aminopropyltriethoxysilane, 2-4 parts of hydroxymethyl cellulose, 1-2 parts of tris (2, 4-di-tert-butylphenyl) phosphite and 1-2 parts of 1-ethyl-3-methylimidazol hexyl sulfate. The invention also discloses a finishing process of the anti-ultraviolet and flame-retardant multifunctional coating fabric finishing agent. The fabric obtained by the method of the patent has the advantage that the flame retardant performance of the fabric is gradually reduced along with the washing process because the flame retardant is not chemically bonded with the fabric.
Patent CN201911094985.8 discloses an anti-ultraviolet, flame-retardant multifunctional coating fabric finishing agent and a finishing process, comprising: 5-26 parts of phenyl ortho-hydroxybenzoate, 0.4-0.6 part of stabilizer, 1.5-23 parts of surfactant, 1-1.2 parts of antioxidant, 5-15 parts of flatting agent, 2.5-15 parts of polyvinyl alcohol, 1.2-26 parts of flame retardant and 2.5-60 parts of organic solvent; wherein, the polyvinyl alcohol is an organic compound, is a white powdery solid and is tasteless; the surfactant comprises 2-ethyl hexanol potassium phosphate diester, tetrabutyl phosphonium iodide and phytic acid dodecasodium; the antioxidant comprises a light stabilizer, a pH value stabilizer and a heat stabilizer; the phenyl o-hydroxybenzoate is colorless or light yellow crystals; the solubility in water is extremely low, the water is not decomposed by concentrated alkali and concentrated acid, and the dissolution point of the water is 130 ℃. After the finishing agent is coated on the fabric, the ultraviolet-resistant performance is stable, and the flame retardant performance is achieved. The flame retardant of the patent also has no chemical bond linkage with the surface of the fabric, so that the flame retardant performance of the fabric is gradually reduced in the washing process, and an organic solvent is used in the preparation process of the finishing agent, so that the environmental pollution is great.
Patent CN106120338A discloses an environment-friendly fluorine-containing fabric finishing agent, which is prepared by addition reaction of fluorine-containing chain segments, polysiloxane and allyl polyoxyethylene ether. The invention also provides a preparation method of the environment-friendly fluorine-containing fabric finishing agent, which comprises the steps of vacuumizing a reaction container, and then adding the fluorine-containing chain segment, polysiloxane and allyl polyoxyethylene ether; adding an organic solvent and a platinum catalyst under the protection of inert gas nitrogen, heating to 40-60 ℃, reacting for 16-20h to obtain a polymer solution, naturally cooling to ambient temperature, distilling under reduced pressure at 35-45 ℃, and then putting into a vacuum drying oven for drying to obtain a finished product. The fluorine-containing fabric finishing agent prepared by the invention contains organic silicon functional groups and introduces fluorine-containing chain segments, and can effectively improve the water and oil repellency of fabrics. The fluorine-containing fabric finishing agent prepared by the invention has the advantages of safe raw materials, simple preparation process and no pollution to the environment. The fabric obtained in this patent has a certain stain resistance, but poor flame retardancy.
Because the fabric modifier prepared by the prior art focuses on one performance or function, the problems that the flame-retardant fabric cannot be used, the flame-retardant fabric cannot be flame-retardant, the flame-retardant fabric has poor durability and the like exist, and the requirements of social development cannot be met, so that the development of a reactive flame-retardant fabric modifier has important value.
Disclosure of Invention
The invention provides a reactive flame-retardant fabric modifier, which has stable and durable performance and excellent and stable flame-retardant effect. .
A reactive flame retardant fabric modifier, comprising the steps of:
(1) 4 to 8 weight portions of 1-allyl benzotriazole, 40 to 60 weight portions of vinyl (trifluoromethyl) dimethylsilane, 0.2 to 0.5 weight portion of emulsifier, 0.1 to 0.5 weight portion of carboxymethyl cellulose, 1 to 5 weight portions of 1-allyl piperazine and 1 to 10 weight portions ofAdding an antistatic agent and 150-200 parts by weight of deionized water into a reaction kettle, introducing nitrogen, stirring for 30-60min at 50-120r/min to obtain emulsion 1, stirring the emulsion 1 at 50-120r/min, and heating to 50-100%oC, simultaneously, dripping 1-5 parts by weight of initiator aqueous solution with the mass fraction of 10% into the emulsion, controlling the speed to be within 60-90min, finishing dripping at a constant speed, and continuing to react for 30-60min after finishing dripping to obtain seed emulsion;
(2) uniformly mixing 3-7 parts by weight of allyl magnesium bromide, 10-20 parts by weight of silane coupling agent with double bonds, 0.01-0.05 part by weight of dodecyl mercaptan, 0.01-0.05 part by weight of AIBN and 50-60 parts by weight of water in a container, then uniformly dropping into the seed emulsion within 60-90min at a constant speed, continuing to perform heat preservation reaction for 120-180min after dropping is finished, and obtaining a reactive flame-retardant fabric modifier after full reaction;
preferably, the emulsifier in step (1) is one or a combination of several of nonylphenol polyoxyethylene ether, sorbitan tristearate, dodecyl trimethyl ammonium chloride, polyoxyethylene sorbitan monopalmitate, sodium dodecyl benzene sulfonate, calcium dodecyl benzene sulfonate, octadecyl amine polyoxyethylene ether biquaternary ammonium salt, hexadecyl trimethyl ammonium bromide and hexadecyl pyridine bromide.
Preferably, the antistatic agent in the step (1) is one or a combination of more of tetraalkyl monomethyl diethylhydroxyl ammonium bromide, hexadecyl monomethyl diethylhydroxyl ammonium bromide, ditrimethylolpropane diphosphate potassium salt and nano conductive powder antimony doped tin dioxide.
Preferably, the initiator in step (1) is one or a combination of azodiisobutyronitrile, azodiisoheptonitrile, dibenzoyl peroxide, potassium persulfate, ammonium persulfate, dicumyl peroxide and peroxydicarbonate.
Preferably, the silane coupling agent with double bonds in the step (2) is one or a combination of more of KH570, A171, KH-A172 and A151.
Part of reaction mechanism in the preparation process of the fabric modifier is shown as follows:
compared with the prior art, the invention has the beneficial effects that:
1. the performance modification capability of the fabric modifier is improved by adding vinyl (trifluoromethyl) dimethylsilane into the nuclear monomer;
2. the allyl magnesium bromide is added into the shell monomer, so that the flame retardant modification capability of the fabric modifier is improved;
3. 1-allyl piperazine and 1-allyl benzotriazole are introduced into the nuclear monomer to initiate the nuclear matrix to generate certain crosslinking, so that the stability of the matrix is improved, and the water resistance of the modifier is improved;
4. by adding the silane coupling agent with double bonds into the shell monomer, the allyl magnesium bromide generates a copolymer, so that the fabric modifier is connected with the fabric through chemical bonds, and the water washing resistance of the fabric modifier is improved.
Drawings
FIG. 1 is a Fourier Infrared Spectroscopy of the product obtained in example 1:
a carbon hydrogen telescopic absorption peak exists near 2953cm < -1 >, an ester carbonyl absorption peak exists near 1761cm < -1 >, and a silicon carbon absorption peak exists near 729cm < -1 >, so that the vinyl (trifluoromethyl) dimethylsilane participates in the reaction; an absorption peak of a benzene ring skeleton exists near 1465/1421cm < -1 >, which indicates that 1-allyl benzotriazole participates in the reaction; an antisymmetric telescopic absorption peak of a silicon-oxygen bond exists near 1094cm < -1 >, which indicates that KH570 participates in the reaction; an expansion absorption peak of a carbon-nitrogen single bond exists near 1368cm-1, indicating that allylpiperazine participates in the reaction.
Detailed Description
The fabric modifier for the unfinished cotton fabric made of the same material is added at 80 DEGoC, finishing for 20min, then taking out, and finishing at 80 DEGoBaking for 20min at 120 deg.CoDrying for 10min under the condition of C, and drying at 30 DEGoSoaping in warm water C, and then using 10oC, water washing, and drying and then testing as follows:
1. static contact angle test, the treated fabric is measured by using a JC2000C3 model sessile drop contact angle measuring instrument;
2. the water-washing resistance effect of the finishing agent is tested according to the test method of GB/T12490-2007, and the water-washing resistance effect of the finished fabric is judged before and after washing;
3. LOI test, according to GB/T5454-1997;
example 1
(1) Adding 4g of 1-allyl benzotriazole, 40g of vinyl (trifluoromethyl) dimethylsilane, 0.2g of nonylphenol polyoxyethylene ether, 0.1g of carboxymethyl cellulose, 1g of 1-allyl piperazine, 1g of tetraalkyl-monomethyl-diethylhydroxyl ammonium bromide and 150g of deionized water into a reaction kettle, introducing nitrogen, stirring at 50r/min for 30min to obtain emulsion 1, stirring the emulsion 1 at the lower side of 50r/min, and heating to 50r/min while stirringoC, simultaneously, dropwise adding 1g of azodiisobutyronitrile aqueous solution with the mass fraction of 10% into the emulsion, controlling the speed to be within 60min, and continuously reacting for 30min after dropwise adding to obtain seed emulsion;
(2) uniformly mixing 3g of allyl magnesium bromide, 10gKH570 g of allyl magnesium bromide, 0.01g of dodecyl mercaptan, 0.01g of AIBN and 50g of water in a container, then dripping into the seed emulsion at a constant speed within 60min, continuing to perform heat preservation reaction for 120min after dripping is finished, and obtaining a reactive flame-retardant fabric modifier after full reaction;
the static contact angle of the fabric before finishing by the modifier is 105 degrees, the static contact angle after finishing is 142 degrees, the effect before finishing is 1.4, the effect after finishing is 3, the effect after 30 times of soaping is 2.9, the LOI of the fabric before finishing by the modifier is 18, the LOI after finishing is 28, and the LOI after 30 times of soaping is 28.
Example 2
(1) 5g of 1-allylbenzotriazole, 41.5g of vinyl (trifluoromethyl) dimethylsilane, 0.2g of sorbitan tristearate, 0.12g of carboxymethylcellulose, 1.4g of 1Adding allyl piperazine, 1.6g of hexadecyl-methyl-diethyl-hydroxy-ammonium bromide and 153.3g of deionized water into a reaction kettle, introducing nitrogen, stirring at 54r/min for 32min to obtain emulsion 1, stirring the emulsion 1 at 54r/min, and heating to 53 DEG while stirringoC, simultaneously, dropwise adding 1.4g of azodiisoheptanonitrile aqueous solution with the mass fraction of 10% into the emulsion, controlling the speed to be within 64min, and continuing to react for 34min after dropwise adding is finished to obtain seed emulsion;
(2) uniformly mixing 4g of allyl magnesium bromide, 10.7g of A171, 0.01g of dodecyl mercaptan, 0.01g of AIBN and 50.7g of water in a container, then dripping into the seed emulsion at a constant speed within 63min, continuing to perform heat preservation reaction for 124min after finishing dripping, and obtaining a reactive flame-retardant fabric modifier after full reaction;
the static contact angle of the fabric before the finishing by the modifier is 107.8 degrees, the static contact angle after the finishing is 142.2 degrees, the effect before the finishing is 1.4, the effect after the finishing is 3, the effect after 30 soaping is 2.9, the LOI of the fabric before the finishing by the modifier is 18, the LOI after the finishing is 28.2, and the LOI after 30 soaping is 28.
Example 3
(1) Adding 6g of 1-allyl benzotriazole, 43.7g of vinyl (trifluoromethyl) dimethylsilane, 0.2g of dodecyl trimethyl ammonium chloride, 0.14g of carboxymethyl cellulose, 1.7g of 1-allyl piperazine, 2.6g of potassium ditrimethylolpropane diphosphate and 157.1g of deionized water into a reaction kettle, introducing nitrogen, stirring for 33min at 62r/min to obtain emulsion 1, and heating the emulsion 1 to 58 r/min while stirring at 57r/minoC, simultaneously, dropwise adding 2g of 10% dibenzoyl peroxide aqueous solution into the emulsion, controlling the speed to be within 67min, and continuously reacting for 37min after dropwise adding to obtain seed emulsion;
(2) 4g of allyl magnesium bromide, 11.5gKH-A172, 0.01g of dodecyl mercaptan, 0.01g of AIBN and 51.2g of water are uniformly mixed in a container, then the mixture is dripped into the seed emulsion at a constant speed within 65min, the heat preservation reaction is continued for 127min after the dripping is finished, and a reaction type flame retardant fabric modifier is obtained after the full reaction;
the static contact angle of the fabric before the finishing by the modifier is 106.4 degrees, the static contact angle after the finishing is 143.7 degrees, the effect before the finishing is 1.4, the effect after the finishing is 3, the effect after 30 soaping is 2.9, the LOI of the fabric before the finishing by the modifier is 18, the LOI after the finishing is 28.3, and the LOI after 30 soaping is 28.
Example 4
(1) Adding 7g of 1-allyl benzotriazole, 44.8g of vinyl (trifluoromethyl) dimethylsilane, 0.2g of polyoxyethylene sorbitan monopalmitate, 0.16g of carboxymethyl cellulose, 1.9g of 1-allyl piperazine, 3.2g of nano conductive powder antimony doped tin dioxide and 159.8g of deionized water into a reaction kettle, introducing nitrogen, stirring at 69r/min for 37min to obtain emulsion 1, and heating the emulsion 1 to 61 r/min while stirring at 67r/minoC, simultaneously, dropwise adding 2.4g of 10 mass percent potassium persulfate aqueous solution into the emulsion, controlling the speed to be within 69min, and continuously reacting for 40min after dropwise adding to obtain seed emulsion;
(2) uniformly mixing 5g of allyl magnesium bromide, 13g of A151, 0.01g of dodecyl mercaptan, 0.01g of AIBN and 51.9g of water in a container, then dripping into the seed emulsion at a constant speed within 68min, continuing to perform heat preservation reaction for 131min after dripping is finished, and obtaining a reactive flame-retardant fabric modifier after full reaction;
the static contact angle of the fabric before the finishing by the modifier is 107.2 degrees, the static contact angle after the finishing is 145.9 degrees, the effect before the finishing is 1.4, the effect after the finishing is 3, the effect after 30 soaping is 2.9, the LOI of the fabric before the finishing by the modifier is 18, the LOI after the finishing is 28.4, and the LOI after 30 soaping is 27.
Example 5
(1) Adding 6g of 1-allyl benzotriazole, 47g of vinyl (trifluoromethyl) dimethylsilane, 0.2g of sodium dodecyl benzene sulfonate, 0.2g of carboxymethyl cellulose, 2.4g of 1-allyl piperazine, 3.9g of tetraalkyl-monomethyl-diethyl-hydroxy-ammonium bromide and 164.2g of deionized water into a reaction kettle, introducing nitrogen, stirring at 77r/min for 41min to obtain emulsion 1, stirring the emulsion 1 at 70r/min, and heating to 66 r/min while stirringoC, simultaneously, dropwise adding 2.8g of 10 mass percent ammonium persulfate aqueous solution into the emulsion, controlling the speed to be within 73min, and continuously reacting for 43min after dropwise adding to obtain seed emulsion;
(2) uniformly mixing 5g of allyl magnesium bromide, 13.6gKH570 g of allyl magnesium bromide, 0.01g of dodecyl mercaptan, 0.01g of AIBN and 53g of water in a container, then dripping into the seed emulsion at a constant speed within 70min, continuing to perform heat preservation reaction for 139min after dripping is finished, and obtaining a reactive flame-retardant fabric modifier after full reaction;
the static contact angle of the fabric before the finishing by the modifier is 108.4 degrees, the static contact angle after the finishing is 148.1 degrees, the effect before the finishing is 1.4, the effect after the finishing is 3, the effect after 30 soaping is 2.9, the LOI of the fabric before the finishing by the modifier is 18, the LOI after the finishing is 28.5, and the LOI after 30 soaping is 28.
Example 6
(1) Adding 8g of 1-allyl benzotriazole, 48.7g of vinyl (trifluoromethyl) dimethylsilane, 0.2g of calcium dodecylbenzenesulfonate, 0.25g of carboxymethylcellulose, 3g of 1-allyl piperazine, 4.9g of hexadecyl monomethyl ammonium diethylhydroxy bromide and 170.8g of deionized water into a reaction kettle, introducing nitrogen, stirring at 84r/min for 45min to obtain emulsion 1, and heating the emulsion 1 to 68 r/min while stirring at 75r/minoC, simultaneously, dropwise adding 3.2g of dicumyl peroxide aqueous solution with the mass fraction of 10% into the emulsion, controlling the speed to be within 76min, and continuously reacting for 47min after dropwise adding is finished to obtain seed emulsion;
(2) uniformly mixing 6g of allyl magnesium bromide, 14.4g of A171, 0.01g of dodecyl mercaptan, 0.01g of AIBN and 53.6g of water in a container, then dripping into the seed emulsion at a constant speed within 74min, continuing to perform heat preservation reaction for 143min after finishing dripping, and obtaining a reactive flame-retardant fabric modifier after full reaction;
the static contact angle of the fabric before the finishing by the modifier is 108.4 degrees, the static contact angle after the finishing is 148.7 degrees, the effect before the finishing is 1.4, the effect after the finishing is 3, the effect after 30 soaping is 2.9, the LOI of the fabric before the finishing by the modifier is 18, the LOI after the finishing is 28.7, and the LOI after 30 soaping is 28.
Example 7
(1) 8g of 1-allylbenzotriazole, 49.8g of vinyl (trifluoromethyl) dimethylsilane, 0.2g of octadecylamine polyoxyethylene ether diquaternary ammonium salt and 0.31g ofAdding carboxymethyl cellulose, 3.4g of 1-allyl piperazine, 5.8g of potassium ditrimethylolpropane diphosphate and 174.6g of deionized water into a reaction kettle, introducing nitrogen, stirring at 90r/min for 49min to obtain emulsion 1, stirring the emulsion 1 at 84r/min, and heating to 72 DEG while stirringoC, simultaneously, dropwise adding 3.7g of 10 mass percent aqueous solution of peroxydicarbonate into the emulsion, controlling the speed to finish dropwise adding at a constant speed within 78min, and continuing to react for 49min after dropwise adding to obtain seed emulsion;
(2) uniformly mixing 6g of allyl magnesium bromide, 15.2gKH-A172, 0.01g of dodecyl mercaptan, 0.01g of AIBN and 54.7g of water in a container, then dripping into the seed emulsion at a constant speed within 77min, continuing to perform heat preservation reaction for 151min after dripping is finished, and obtaining a reactive flame-retardant fabric modifier after full reaction;
the static contact angle of the fabric before the finishing by the modifier is 109 degrees, the static contact angle after the finishing is 148.7 degrees, the effect before the finishing is 1.4, the effect after the finishing is 3, the effect after 30 soaping is 2.9, the LOI of the fabric before the finishing by the modifier is 18, the LOI after the finishing is 28.9, and the LOI after 30 soaping is 28.
Example 8
(1) Adding 8g of 1-allyl benzotriazole, 52.4g of vinyl (trifluoromethyl) dimethylsilane, 0.2g of hexadecyl trimethyl ammonium bromide, 0.34g of carboxymethyl cellulose, 3.8g of 1-allyl piperazine, 6.8g of nano conductive powder antimony doped tin dioxide and 177.3g of deionized water into a reaction kettle, introducing nitrogen, stirring at 100r/min for 52min to obtain emulsion 1, stirring the emulsion 1 at 87r/min, and heating to 77r/min while stirringoC, simultaneously, dropwise adding 3.9g of azodiisobutyronitrile aqueous solution with the mass fraction of 10% into the emulsion, controlling the speed to be within 81min, and continuously reacting for 52min after dropwise adding is finished to obtain seed emulsion;
(2) uniformly mixing 7g of allyl magnesium bromide, 16.7g of A151, 0.01g of dodecyl mercaptan, 0.01g of AIBN and 56g of water in a container, then dripping into the seed emulsion at a constant speed within 80min, continuing to perform heat preservation reaction for 157min after dripping is finished, and obtaining a reactive flame-retardant fabric modifier after full reaction;
the static contact angle of the fabric before the finishing by the modifier is 109.4 degrees, the static contact angle after the finishing is 148.8 degrees, the effect before the finishing is 1.4, the effect after the finishing is 3, the effect after 30 soaping is 2.9, the LOI of the fabric before the finishing by the modifier is 18, the LOI after the finishing is 29, and the LOI after 30 soaping is 29.
Example 9
(1) Adding 8g of 1-allyl benzotriazole, 60g of vinyl (trifluoromethyl) dimethylsilane, 0.5g of hexadecylpyridine bromide, 0.5g of carboxymethyl cellulose, 5g of 1-allyl piperazine, 10g of tetraalkyl-monomethyl-diethyl-ammonium bromide and 200g of deionized water into a reaction kettle, introducing nitrogen, stirring at 120r/min for 60min to obtain emulsion 1, stirring the emulsion 1 at 120r/min, and heating to 100 DEG while stirringoC, simultaneously, dripping 5g of 10 mass percent dibenzoyl peroxide aqueous solution into the emulsion, controlling the speed to finish dripping at a constant speed within 90min, and continuing to react for 60min after finishing dripping to obtain seed emulsion;
(2) uniformly mixing 7g of allyl magnesium bromide, 20g of A171, 0.05g of dodecyl mercaptan, 0.05g of AIBN and 60g of water in a container, then dripping into the seed emulsion at a constant speed within 90min, continuing to perform heat preservation reaction for 180min after dripping is finished, and obtaining a reactive flame-retardant fabric modifier after full reaction;
the static contact angle of the fabric before finishing by the modifier is 110 degrees, the static contact angle after finishing is 150 degrees, the effect before finishing is 1.6, the effect after finishing is 3.2, the effect after 30 soaping is 3, the LOI of the fabric before finishing by the modifier is 18, the LOI after finishing is 30, and the LOI after 30 soaping is 29.
Comparative example 1
Relative to example 1, the content of vinyl (trifluoromethyl) dimethylsilane was 0g, the static contact angle of the fabric before finishing with the modifier was 101 degrees, the static contact angle after finishing was 133 degrees, the effect before finishing was 1.6, the effect after finishing was 3.1, the effect after 30 soaping was 3, the LOI of the fabric before finishing with the modifier was 18, and the LOI of the fabric after finishing was 20.
Comparative example 2
Relative to example 1, 0g of 1-allylbenzotriazole, 104 degrees static contact angle before the fabric was finished with the modifier, 138 degrees static contact angle after the finishing, 1.6 before the finishing, 3.1 after the finishing, 1.9 after 30 soaping, 18 LOI of the fabric before the finishing with the modifier, and 28.5 after the finishing.
Comparative example 3
Relative to example 1, 0g of 1-allylpiperazine, a static contact angle of 103 degrees before the fabric was finished with the modifier, a static contact angle after the finishing of 139 degrees, an effect before the finishing of 1.5, an effect after the finishing of 3.0, an effect after 30 soaping of 2.9, an LOI of 18 before the fabric was finished with the modifier, an LOI of 28 after the finishing, and an LOI of 19 after 30 soaping.
Comparative example 4
Relative to example 1, the content of allylmagnesium bromide was 0g, the static contact angle of the fabric before finishing with the modifier was 105 degrees, the static contact angle after finishing was 140 degrees, the effect before finishing was 1.6, the effect after finishing was 3.1, the effect after 30 soaping was 2.6, the LOI of the fabric before finishing with the modifier was 18, the LOI after finishing was 29, and the LOI after 30 soaping was 25.
Claims (5)
1. A reactive flame retardant fabric modifier, comprising the steps of:
(1) adding 40-60 parts by weight of 1-allyl benzotriazole, 40-60 parts by weight of vinyl (trifluoromethyl) dimethylsilane, 0.2-0.5 part by weight of emulsifier, 0.1-0.5 part by weight of carboxymethyl cellulose, 1-5 parts by weight of 1-allyl piperazine, 1-10 parts by weight of antistatic agent and 200 parts by weight of deionized water of 150-fold into a reaction kettle, introducing nitrogen, stirring for 30-60min at 50-120r/min to obtain emulsion 1, stirring the emulsion 1 at 50-120r/min, and heating to 50-100 r/minoC, simultaneously, dripping 1-5 parts by weight of initiator aqueous solution with the mass fraction of 10% into the emulsion, controlling the speed to be within 60-90min, finishing dripping at a constant speed, and continuing to react for 30-60min after finishing dripping to obtain seed emulsion;
(2) 10-20 parts by weight of allyl magnesium bromide, 10-20 parts by weight of silane coupling agent with double bonds, 0.01-0.05 part by weight of dodecyl mercaptan, 0.01-0.05 part by weight of AIBN and 50-60 parts by weight of water are uniformly mixed in a container, then the mixture is dripped into the seed emulsion at a constant speed within 60-90min, the heat preservation reaction is continued for 120-180min after the dripping is finished, and the reaction type flame retardant fabric modifier is obtained after the full reaction.
2. The method of claim 1, wherein the emulsifier in step (1) is one or more selected from polyoxyethylene nonyl phenyl ether, sorbitan tristearate, dodecyl trimethyl ammonium chloride, polyoxyethylene sorbitan monopalmitate, sodium dodecyl benzene sulfonate, calcium dodecyl benzene sulfonate, octadecyl amine polyoxyethylene ether biquaternary ammonium salt, hexadecyl trimethyl ammonium bromide and hexadecyl pyridine bromide.
3. The method of claim 1, wherein the antistatic agent in step (1) is one or more of tetraalkyl-monomethyl-diethylhydroxyl ammonium bromide, hexadecyl-monomethyl-diethylhydroxyl ammonium bromide, potassium ditrimethylolpropane diphosphate, and nano-conductive powder antimony doped tin dioxide.
4. The method of claim 1, wherein the initiator in step (1) is one or more selected from the group consisting of azobisisobutyronitrile, azobisisoheptonitrile, dibenzoyl peroxide, potassium persulfate, ammonium persulfate, dicumyl peroxide, and peroxydicarbonate.
5. The method of claim 1, wherein the double-bond silane coupling agent in step (2) is a combination of one or more of KH570, A171, KH-A172 and A151.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011249617.9A CN112175136B (en) | 2020-11-11 | 2020-11-11 | Reactive flame-retardant fabric modifier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011249617.9A CN112175136B (en) | 2020-11-11 | 2020-11-11 | Reactive flame-retardant fabric modifier |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112175136A true CN112175136A (en) | 2021-01-05 |
| CN112175136B CN112175136B (en) | 2022-12-16 |
Family
ID=73918138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011249617.9A Active CN112175136B (en) | 2020-11-11 | 2020-11-11 | Reactive flame-retardant fabric modifier |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112175136B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1589483A (en) * | 1977-01-24 | 1981-05-13 | Kao Corp | Fabric stiffening composition |
| CN1214345A (en) * | 1997-10-15 | 1999-04-21 | 乙基公司 | Functionalized olefin copolymer additives |
| CN101604607A (en) * | 2007-06-11 | 2009-12-16 | 三星Sdi株式会社 | Coating composition for electrode interconnection member and plasma display panel comprising same |
| CN110256623A (en) * | 2019-04-22 | 2019-09-20 | 苏州大学 | Perfluoroalkyl tetrafluoro sulphur methylene styrol copolymer and its application |
| CN111909505A (en) * | 2020-08-16 | 2020-11-10 | 东阳市琰安建筑工程有限公司 | Preparation method of reactive flame-retardant sealing material for buildings |
-
2020
- 2020-11-11 CN CN202011249617.9A patent/CN112175136B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1589483A (en) * | 1977-01-24 | 1981-05-13 | Kao Corp | Fabric stiffening composition |
| CN1214345A (en) * | 1997-10-15 | 1999-04-21 | 乙基公司 | Functionalized olefin copolymer additives |
| CN101604607A (en) * | 2007-06-11 | 2009-12-16 | 三星Sdi株式会社 | Coating composition for electrode interconnection member and plasma display panel comprising same |
| CN110256623A (en) * | 2019-04-22 | 2019-09-20 | 苏州大学 | Perfluoroalkyl tetrafluoro sulphur methylene styrol copolymer and its application |
| CN111909505A (en) * | 2020-08-16 | 2020-11-10 | 东阳市琰安建筑工程有限公司 | Preparation method of reactive flame-retardant sealing material for buildings |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112175136B (en) | 2022-12-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3433780A (en) | Colloidal silsesquioxanes and methods for making same | |
| CN109988264B (en) | Fluorine-free waterproof agent and preparation method and application thereof | |
| Waack et al. | Reactivities of organolithium compounds in tetrahydrofuran. I. As vinyl polymerization initiators | |
| NO169544B (en) | OIL AND WATER-RESISTANT SOLID FLUOR POLYMERS | |
| CN104594045B (en) | A fabric water and oil repellent finishing agent and preparation method thereof | |
| US3870767A (en) | Oleophobic and hydrophobic polymers containing polymerization product of fluorinated sulfonamideoethylene moieties | |
| CN110804864A (en) | Processing technology of flame-retardant antibacterial polyester fabric | |
| CN106866872A (en) | Water-proofing treatment composition dispersion liquid | |
| CN104927491A (en) | Antibacterial flame retardant coating and preparation method thereof | |
| EP1917282B8 (en) | Repellent composition containing graft copolymer, graft copolymer and method of preparing graft copolymer | |
| CN112175136B (en) | Reactive flame-retardant fabric modifier | |
| CN112300334A (en) | POSS/organosilicon modified polyacrylate fluorine-free waterproofing agent and preparation method thereof | |
| CN116180439A (en) | Antibacterial and oil-repellent fabric and its production process | |
| CN110358221B (en) | Lanthanum sorbate composite heat stabilizer for PVC | |
| CN116043547A (en) | A kind of acrylate fluorine-free water repellent and its application | |
| KR20080030572A (en) | Production processes and systems, compositions, surfactants, monomer units, metal complexes, phosphate esters, glycols, aqueous film forming foams, and foam stabilizers | |
| US3081274A (en) | Fluorocarbon vinyl benzenes and their polymers | |
| CN119305233A (en) | A kind of preparation method of polypropylene outdoor fabric | |
| GB951988A (en) | Phosphorus polymers | |
| CN113880981A (en) | Phosphorus-containing polyacrylate adhesive and preparation method and application thereof | |
| CN105924573B (en) | A kind of perfluoroalkyl polyolefin acid ester waterproofing agent, preparation method and application | |
| CN108004775A (en) | A kind of water-proof antibiotic finishing agent | |
| CN112553913A (en) | Hyperbranched polymer-containing heavy metal-free bromine-phosphorus synergistic aqueous textile flame-retardant coating composition, preparation method and flame-retardant fabric | |
| CN111187380A (en) | Copolymer emulsion containing chlorine and fluorine-free waterproofing agent and polymerization method thereof | |
| US2404779A (en) | Process for the copolymerization of asymmetrical dihalogenated ethylenes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |