CN111040055B - CaCO (calcium carbonate)3Preparation method of water-soluble flame-retardant hyperdispersant for powder modification - Google Patents
CaCO (calcium carbonate)3Preparation method of water-soluble flame-retardant hyperdispersant for powder modification Download PDFInfo
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Abstract
The invention discloses CaCO3A preparation method of a water-soluble flame-retardant hyperdispersant for modifying powder. Pentaerythritol, phosphorus oxychloride and melamine are used for preparing the flame retardant, namely the diphosphine melamine salt; mixing methacrylic acid, polyoxyethylene ether macromonomer and azodiisobutyronitrile at 60 ℃ for 4-6 h, adding the prepared bis-spiro phosphorus melamine salt and triphenylphosphine serving as a catalyst, heating to 80 ℃ and reacting for 2-3 h to obtain CaCO3The powder is modified by water-soluble flame-retardant hyperdispersant. The method has the characteristics of simple preparation process, low cost, small pollution, wide applicability and the like, and the prepared water-soluble flame-retardant hyper-dispersant contains 'multi-point anchoring' in the molecular structure and is easy to be adsorbed on the surface of inorganic powder.
Description
Technical Field
The invention belongs to the technical field of flame-retardant hyperdispersant for surface modification of inorganic powder, and particularly relates to CaCO3A preparation method of a water-soluble flame-retardant hyperdispersant for modifying powder.
Background
Surface modification technology has become one of the most important and necessary deep processing technologies for inorganic powders. The organic coating is mainly used for organic coating, and the used organic modifier comprises surfactants such as higher fatty acid containing 16-18 carbon atoms and resin acid, macromolecular dispersants such as polyethylene glycol and polymethyl methacrylate, and coupling agents such as titanate, aluminate and silane. But the coupling agent has high price, the modification process is complex, the titanate coupling agent generates pollution and the like, so the large-area popularization and application of the coupling agent are not always realized. Stearic acid, which is most widely used in industry, has only one carboxyl anchoring point and relatively long alkyl group, so the modification effect is not ideal. In addition, most of the currently produced hyperdispersants have single functions, and the application field is limited.
The double-spiro phosphorus melamine salt flame retardant (IFR) mainly comprises a carbon source, an acid source and a gas source. The molecular structure of the flame retardant contains a plurality of reactive amino anchoring groups and rich polyfunctional group carbon forming agents, and the flame retardant can generate an expanded porous carbon layer and release inert gas when heated, so that the flame retardant has the advantages of being difficult to combust, preventing flame diffusion, delaying the fire spread speed and the like.
The existing water-based acrylic resin and polyoxyethylene ether macromonomer basically have no flame resistance, a large amount of flame retardant is required to be added for achieving the flame retardant performance, and the product performance is influenced by the addition of a large amount of flame retardant. The polyoxyethylene ether macromonomer has the remarkable characteristic of designability of a molecular structure, unsaturated double bonds at the end group of the macromonomer and methacrylic acid monomers generate copolymerization reaction under the action of an initiator to generate a polycarboxylic acid main chain, and a water-soluble flame retardant section and an amino group are grafted on the polycarboxylic acid main chain through an amidation reaction of carboxyl and an amino group on a flame retardant molecular chain to form multi-point anchoring and are firmly adsorbed on the surface of inorganic powder with hydroxyl on the surface of the powder through the hydrogen bond action. The dispersion of the inorganic powder in the polymer matrix is improved through the steric hindrance effect, and the synthesized flame-retardant hyperdispersant has the characteristics of water solubility, dispersion, flame retardance and the like.
The invention discloses a water-based acrylate composite heat-insulating fireproof coating and a preparation method thereof (CN 107903746A) reported by Liuhuantian and the like, wherein the water-based acrylate emulsion is used as a film-forming substance, and an intumescent fire retardant, a flame retardant, a heat-insulating pigment filler and a small amount of auxiliary agent are added to prepare the water-based acrylate composite heat-insulating fireproof coating. The invention discloses a flame-retardant corrosion-resistant acrylic coating (CN 104356803A) reported by the Heizhengbei et al, and the flame-retardant corrosion-resistant acrylic coating is prepared from water-soluble acrylic resin, water-soluble phenolic resin, styrene-butadiene rubber, lauric acid diethanolamide, hydroxypropyl methyl cellulose, sepiolite powder, talcum powder, montmorillonite powder, melamine phosphate, nano magnesium hydroxide, tricresyl phosphate, fully methylated amino resin, manganese abietate, epoxy silane coupling agent and the like. The patent of invention "a method for preparing flame-retardant waterborne acrylic resin" (CN 108530576A) is reported, wherein methyl acrylate, butyl acrylate, ethyl methacrylate, dimethylaminopropyl methacrylamide, maleic acid dihydrazide, triethanolamine oleate, melamine phosphate, piperazine polyphosphate, piperazine pyrophosphate, tetraphenyl pyrophosphate, haloalkyl phosphate, bisphenol a diphosphate and the like are mixed, and a flame-retardant waterborne acrylic resin is prepared through five steps.
The research of the hyperdispersant does not relate to the preparation of the water-soluble flame-retardant hyperdispersant with double functions by using a polyoxyethylene ether macromonomer and methacrylic acid as an active modification section of the flame-retardant hyperdispersant and using grafted bis-spiro-phosphate melamine salt as a flame-retardant section, and the preparation method of the water-soluble flame-retardant hyperdispersant is not reported in documents at present.
Disclosure of Invention
The invention aims to overcome the technical defect of no flame retardancy of the existing water-soluble polyacrylic acid dispersant, and provides CaCO3A preparation method of a water-soluble flame-retardant hyperdispersant for modifying powder.
The invention is realized by the following technical scheme:
the invention prepares CaCO3The powder is modified by water-soluble flame-retardant hyperdispersant. The dispersant has multiple amino anchoring groups capable of reacting with CaCO3The hydroxyl on the surface of the powder forms multi-point anchoring by the action of hydrogen bonds, and the anchoring is carried out on CaCO3The powder has excellent dispersion and flame retardant properties. Meanwhile, the polyoxyethylene ether macromonomer and the methacrylic acid copolymer long chain on the hyperdispersant can be entangled with the polymer molecular chain, which is beneficial to improving CaCO3The interfacial compatibility between the powder and the polymer improves the mechanical property of the composite material.
The method comprises the following specific steps:
(1) adding 5-15 g of pentaerythritol and 15-45 g of phosphorus oxychloride into a three-neck flask, mechanically stirring, heating to 80 ℃, reacting for 4-5 h, heating to 100-110 ℃, continuing to react for 15-20 h, absorbing reaction tail gas by using 30-50 mL of 1M sodium hydroxide solution, after the reaction is finished, removing unreacted phosphorus oxychloride by suction filtration, washing a filter cake for 1 time by using 20-30 mL of carbon tetrachloride, then washing for 2 times by using 40-60 mL of absolute ethyl alcohol, and drying the washed filter cake for 12h at a constant temperature of 60 ℃ in a vacuum box to obtain white powdery dichlorospiro phosphorus (PDSPB).
(2) Adding 6-11 g of melamine and 5-9 g of the dispiro-phosphorodite prepared in the step (1) into 250mL of distilled water, stirring for 30-60 min at 80 ℃, adding 15-100 mg of sodium hydride as a deprotonating agent, continuously reacting for 4-5 h at 80 ℃, cooling to room temperature after the reaction is finished, standing for 48 h at 2-3 ℃, filtering, washing a crystallized product with distilled water for 1 time, and drying at constant temperature for 12h at 60-70 ℃ in a vacuum box to obtain the dispiro-phosphorotricyanamide salt (IFR).
(3) Adding 10-15 g of methacrylic acid, 10-15 g of polyoxyethylene ether macromonomer and 0.5-2 g of azobisisobutyronitrile into a three-neck flask, and magnetically stirring at 60 ℃ for 4-6 h; then 10-30 g of the double-spiro phosphorus melamine salt prepared in the step (2) and 0.1-1 g of triphenylphosphine are added, and the mixture reacts for 2-3 h at the constant temperature of 80 ℃ to obtain CaCO3The powder is modified by water-soluble flame-retardant hyperdispersant.
Preferably, the polyoxyethylene ether macromonomer in step (3) is one or a combination of methallyl alcohol polyoxyethylene ether, allyl polyoxyethylene ether, prenol polyoxyethylene ether and nonylphenol polyoxyethylene ether.
Preferably, the CaCO used in the step (3) is3The molecular weight of the water-soluble flame-retardant hyperdispersant for powder modification is 7000-9000.
The method of the invention has the following advantages:
(1) wide raw material source, low preparation cost and little environmental pollution.
(2) The synthesis process is simple and is suitable for industrial large-scale production.
(3) The prepared flame-retardant hyperdispersant can improve CaCO3The powder has uniform dispersibility in the polymer matrix, and the composite material has flame retardance.
Drawings
FIG. 1 shows CaCO prepared according to the invention3The molecular structural formula of the water-soluble flame-retardant hyperdispersant for modifying the powder.
Detailed Description
The main raw materials used in the examples: pentaerythritol (technical grade), melamine (technical grade), phosphorus oxychloride (chemically pure), methacrylic acid (technical grade), methallyl alcohol polyoxyethylene ether (technical grade), triphenylphosphine (chemically pure), azobisisobutyronitrile (chemically pure).
Example 1:
(1) 5g of pentaerythritol and 15g of phosphorus oxychloride are added into a three-neck flask, mechanical stirring is adopted, the temperature is increased to 80 ℃ for reaction for 4 hours, the temperature is increased to 110 ℃, the reaction is continued for 20 hours, and the reaction tail gas is absorbed by 30mL of 1M sodium hydroxide solution. After the reaction is finished, removing unreacted phosphorus oxychloride by suction filtration, washing a filter cake for 1 time by using 20mL of carbon tetrachloride, then washing for 2 times by using 40mL of absolute ethyl alcohol, and drying the washed filter cake for 12 hours in a vacuum oven at the constant temperature of 60 ℃ to obtain white powder of dispiro-chloro-phosphorus (PDSPB).
(2) 6g of melamine and 5g of PDSPB prepared in step (1) were added to 250mL of distilled water, stirred at 80 ℃ for 30 min, and then 15mg of sodium hydride as a proton-removing agent was added, and the reaction was continued at 80 ℃ for 4 h. After the reaction is finished, cooling to room temperature, standing for 48 h at the temperature of 3 ℃, filtering, washing the crystallized product with distilled water for 1 time, and drying in a vacuum oven at the constant temperature of 65 ℃ for 12h to obtain the double-spiro phosphorus melamine salt (IFR).
(3) Adding 10g of methacrylic acid, 10g of methallyl alcohol polyoxyethylene ether and 0.5g of azobisisobutyronitrile into a three-neck flask, and magnetically stirring for 4 hours at 60 ℃; then 10g of the double-spiro phosphorus melamine salt prepared in the step (2) and 0.1g of triphenylphosphine are added into the mixture to react for 2 hours at the constant temperature of 80 ℃, thus obtaining CaCO3The powder is modified by water-soluble flame-retardant hyperdispersant.
Example 2:
(1) 10g of pentaerythritol and 25g of phosphorus oxychloride are added into a three-neck flask, mechanical stirring is adopted, the temperature is increased to 80 ℃ for reaction for 4 hours, then the temperature is increased to 110 ℃ for further reaction for 20 hours, and the reaction tail gas is absorbed by 50mL of 1M sodium hydroxide solution. After the reaction is finished, removing unreacted phosphorus oxychloride by suction filtration, washing a filter cake for 1 time by 30mL of carbon tetrachloride, then washing for 2 times by 60mL of absolute ethyl alcohol, and drying the washed filter cake for 12 hours in a vacuum oven at the constant temperature of 90 ℃ to obtain white powder of dispiro-Phosphorane Dichloride (PDSPB).
(2) 11g of melamine and 9g of PDSPB prepared in step (1) were added to 250mL of distilled water, stirred at 80 ℃ for 40min, and then 50mg of sodium hydride as a proton-removing agent was added to continue the reaction at 80 ℃ for 4 h. After the reaction is finished, cooling to room temperature, standing for 48 h at the temperature of 3 ℃, filtering, washing the crystallized product with distilled water for 1 time, and drying in a vacuum oven at the constant temperature of 65 ℃ for 12h to obtain the double-spiro phosphorus melamine salt (IFR).
(3) Adding 10g of methacrylic acid, 15g of methallyl alcohol polyoxyethylene ether and 1g of azobisisobutyronitrile into a three-neck flask, and magnetically stirring for 4 hours at 60 ℃; then 15g of the double-spiro phosphorus melamine salt prepared in the step (2) and 0.5g of triphenylphosphine are added into the mixture to react for 2 hours at the constant temperature of 80 ℃, thus obtaining CaCO3The powder is modified by water-soluble flame-retardant hyperdispersant.
Example 3:
(1) adding 15g of pentaerythritol and 15g of phosphorus oxychloride into a three-neck flask, heating to 80 ℃ by adopting mechanical stirring, reacting for 4 hours, then heating to 110 ℃ to continue reacting for 20 hours, and absorbing reaction tail gas by 40mL of 1M sodium hydroxide solution. After the reaction is finished, removing unreacted phosphorus oxychloride by suction filtration, washing a filter cake for 1 time by 30mL of carbon tetrachloride, then washing for 2 times by 50mL of absolute ethyl alcohol, and drying the washed filter cake for 12 hours in a vacuum oven at the constant temperature of 90 ℃ to obtain white Powder of Dichlorophosphasphorus (PDSPB).
(2) 10g of melamine and 7g of PDSPB obtained in step (1) were added to 250mL of distilled water, stirred at 80 ℃ for 40min, and then 50mg of sodium hydride as a proton-removing agent was added, and the reaction was continued at 80 ℃ for 4 h. After the reaction is finished, cooling to room temperature, standing for 48 h at 2 ℃, filtering, washing the crystallized product with distilled water for 1 time, and drying in a vacuum oven at the constant temperature of 65 ℃ for 12h to obtain the double spiro phosphorus melamine salt (IFR).
(3) Adding 15g of methacrylic acid, 10g of methallyl alcohol polyoxyethylene ether and 2g of azobisisobutyronitrile into a three-neck flask, and magnetically stirring for 4 hours at 60 ℃; then 30g of the double-spiro phosphorus melamine salt prepared in the step (2) and 1g of triphenylphosphine are added into the mixture to react for 2 hours at the constant temperature of 80 ℃, thus obtaining CaCO3The powder is modified by water-soluble flame-retardant hyperdispersant.
The invention has the beneficial effect that the prepared water-soluble flame-retardant hyperdispersant contains a plurality of amino groups, namely CaCO3The powder has good anchoring effect. Meanwhile, the polyoxyethylene ether macromonomer and the acrylic copolymer flexible long chain and the flame retardant section on the dispersing agent endow the dispersing agent with CaCO3The dispersibility and the flame retardance of the powder in the polymer are favorable for improving CaCO3The interfacial compatibility between the powder and the polymer improves the mechanical property of the composite material.
Claims (3)
1. CaCO (calcium carbonate)3The preparation method of the water-soluble flame-retardant hyperdispersant for modifying the powder is characterized by comprising the following specific steps of:
(1) adding 5-15 g of pentaerythritol and 15-45 g of phosphorus oxychloride into a three-neck flask, mechanically stirring, heating to 80 ℃, reacting for 4-5 h, heating to 100-110 ℃, continuing to react for 15-20 h, absorbing reaction tail gas by using 30-50 mL of 1M sodium hydroxide solution, after the reaction is finished, removing unreacted phosphorus oxychloride by suction filtration, washing a filter cake for 1 time by using 20-30 mL of carbon tetrachloride, then washing for 2 times by using 40-60 mL of absolute ethyl alcohol, and drying the washed filter cake for 12h at a constant temperature of 60 ℃ in a vacuum box to obtain white powdery diclososporin;
(2) adding 6-11 g of melamine and 5-9 g of the dispiro-phosphorane dichloride prepared in the step (1) into 250mL of distilled water, stirring for 30-60 min at 80 ℃, adding 15-100 mg of sodium hydride as a deprotonating agent, continuously reacting for 4-5 h at 80 ℃, cooling to room temperature after the reaction is finished, standing for 48 h at 2-3 ℃, filtering, washing a crystallized product with distilled water for 1 time, and drying at constant temperature of 60-70 ℃ for 12h in a vacuum oven to obtain the dispiro-phosphorane melamine salt;
(3) adding 10-15 g of methacrylic acid, 10-15 g of polyoxyethylene ether macromonomer and 0.5-2 g of azobisisobutyronitrile into a three-neck flask, and magnetically stirring at 60 ℃ for 4-6 h; then 10-30 g of the double-spiro phosphorus melamine salt prepared in the step (2) and 0.1-1 g of triphenylphosphine are added, and the mixture reacts for 2-3 h at the constant temperature of 80 ℃ to obtain CaCO3The powder is modified by water-soluble flame-retardant hyperdispersant.
2. The CaCO of claim 13The preparation method of the water-soluble flame-retardant hyperdispersant for modifying the powder is characterized in that the polyoxyethylene ether macromonomer is one or a combination of more of methyl allyl alcohol polyoxyethylene ether, allyl polyoxyethylene ether and prenol polyoxyethylene ether.
3. The CaCO of claim 13The preparation method of the water-soluble flame-retardant hyperdispersant for modifying the powder is characterized in that the CaCO is used as the additive3The molecular weight of the water-soluble flame-retardant hyperdispersant for powder modification is 7000-9000.
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