CN115323796B - Flame-retardant dense mesh net for disc buckle frame and production process thereof - Google Patents
Flame-retardant dense mesh net for disc buckle frame and production process thereof Download PDFInfo
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
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- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/22—Amides of acids of phosphorus
- C07F9/24—Esteramides
- C07F9/2404—Esteramides the ester moiety containing a substituent or a structure which is considered as characteristic
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- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/22—Amides of acids of phosphorus
- C07F9/24—Esteramides
- C07F9/2454—Esteramides the amide moiety containing a substituent or a structure which is considered as characteristic
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- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/655—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms
- C07F9/65502—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms the oxygen atom being part of a three-membered ring
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
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- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
- D06N3/0088—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/06—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds with polyvinylchloride or its copolymerisation products
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- D06N2203/00—Macromolecular materials of the coating layers
- D06N2203/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N2203/045—Vinyl (co)polymers
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- D06N2209/00—Properties of the materials
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- D06N2209/067—Flame resistant, fire resistant
Abstract
The invention relates to a disc buckle frame flame-retardant dense mesh net and a production process thereof, belonging to the technical field of dense mesh nets, wherein the PVC paste resin comprises 80-90 parts, calcium carbonate 10-12 parts, flame-retardant plasticizer 80-90 parts, antioxidant 2-3 parts, light stabilizer 0.5-1 part and white carbon black 1-2 parts; 2-4 parts of auxiliary agent; the preparation method comprises the following steps: mixing the raw materials, grinding for 40-50min by a grinder, and vacuum defoaming after finishing grinding to obtain resin slurry; the resin sizing agent is soaked and coated on terylene industrial cloth by a coating machine, and then plasticizing treatment is carried out under the condition of 180-200 ℃. The flame-retardant plasticizer prepared by the invention belongs to epoxy plasticizers, has plasticizing effect on polyvinyl chloride, has better stability and compatibility with plastics due to the epoxy groups in the structure, and improves water resistance by matching with Si-O-Si chain segments in the structure.
Description
Technical Field
The invention belongs to the technical field of dense mesh networks, and particularly relates to a disc buckle frame flame-retardant dense mesh network and a production process thereof.
Background
The dense mesh net is totally called as dense mesh type safe vertical net, and the mesh density is not lower than 800 meshes/100 cm 2 A net mounted perpendicular to the horizontal plane. Generally comprises a net body, an open eye ring buckle, a side rope and an additional tether. The device is suitable for high-rise building construction, shipbuilding, ship repairing, water loading and unloading, large-scale equipment installation and other high-altitude operation places; for preventing people and objects from falling or for avoiding injury caused by falling objects. Can also be used as a protective net, a purse net, an anti-bird net and the like for various purposes.
With the development of the urban, technological and humanized society, the building industry is vigorously developed, and the problems of increased use amount of the safety net for the building, low strength of the safety net, low light transmission and fire resistance and the like are brought into play, so that the existing safety net for the building mainly adopts materials such as nylon or chemical fiber, and has low impact resistance, low penetration resistance, easy aging, low tensile force after aging and poor fire resistance.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a disc buckle frame flame-retardant dense mesh net and a production process thereof.
The aim of the invention can be achieved by the following technical scheme:
a flame-retardant dense mesh net of a plate buckle frame comprises terylene industrial cloth and resin slurry coated on the surface;
the resin slurry comprises the following raw materials in parts by weight: 80-90 parts of PVC paste resin, 10-12 parts of calcium carbonate, 80-90 parts of flame retardant plasticizer, 2-3 parts of antioxidant, 0.5-1 part of light stabilizer and 1-2 parts of white carbon black; 2-4 parts of auxiliary agent;
the flame retardant plasticizer is prepared by the following steps:
firstly, mixing cardanol, glutaric anhydride and p-toluenesulfonic acid, setting the temperature to 170 ℃ for reaction for 3 hours, setting condensation reflux in the reaction process, cooling to room temperature after the reaction is finished, adding 1, 4-dioxane, washing with deionized water, and then carrying out reduced pressure distillation to obtain an intermediate product a; esterification reaction is carried out under the catalysis of cardanol, glutaric anhydride and p-toluenesulfonic acid, and carboxyl is introduced to obtain an intermediate product a;
adding the intermediate product a and the synergistic flame retardant into N, N-dimethylformamide, stirring and dispersing, then adding 1, 8-diazabicyclo undec-7-ene, heating to 60 ℃, reacting for 4-5h, and distilling under reduced pressure after the reaction is finished to obtain an intermediate product b; the carboxyl in the structure of the intermediate product a and the hydroxyl in the synergistic flame retardant structure react under the catalysis of 1, 8-diazabicyclo undec-7-ene (DBU) to obtain an intermediate product b;
and thirdly, mixing the intermediate product b, m-chloroperoxybenzoic acid and methylene dichloride, keeping the temperature of the system at 30 ℃, reacting for 3 hours, filtering the crude product after the reaction is finished, washing the crude product with saturated sodium sulfite, saturated sodium bicarbonate and distilled water, drying and filtering an organic phase with anhydrous sodium sulfate, and removing a solvent from the filtrate by reduced pressure distillation to obtain the flame-retardant plasticizer. And (3) under the action of m-chloroperoxybenzoic acid, epoxidizing the double bond in the structure of the intermediate product b to obtain the flame-retardant plasticizer.
Further, the molar ratio of cardanol, glutaric anhydride and p-toluene sulfonic acid used in the first step is 1:1.5:0.015; the dosage ratio of the intermediate product a, the synergistic flame retardant, the N, N-dimethylformamide and the 1, 8-diazabicyclo undec-7-ene in the second step is 9g:5.5g:100mL:2.5g; the ratio of the amount of intermediate b, m-chloroperoxybenzoic acid and methylene dichloride in the third step is 3.5g:2.5g:15mL.
Further, the synergistic flame retardant is prepared by the steps of:
mixing 2- (allylamino) ethanol and toluene under the protection of nitrogen, heating to 50 ℃, adding a Karster catalyst, stirring for 30-40min, adding methyl disiloxane, heating to 70 ℃ after the addition, stirring for 24h, cooling to room temperature after the reaction is finished, and distilling under reduced pressure to remove toluene to obtain a hydroxyl-terminated monomer; performing hydrosilylation on 2- (allylamino) ethanol and methyldisiloxane under the action of a catalyst to obtain a hydroxyl-terminated monomer;
mixing carbon tetrachloride, dimethyl phosphate and tetrahydrofuran, adding hydroxyl-terminated monomers under ice water bath conditions, stirring and dispersing for 10min, adding triethylamine, heating to 20 ℃ after the addition, stirring and reacting for 11h, and distilling under reduced pressure to remove the solvent after the reaction is finished to obtain a synergistic flame retardant; and reacting the secondary amine in the hydroxyl-terminated monomer with dimethyl phosphate to obtain the synergistic flame retardant.
Further, the ratio of the amount of 2- (allylamino) ethanol, methyldisiloxane, the Kadster catalyst and toluene in the first step was 0.02mol:0.01mol:0.2mL:100mL;
in the second step, the dosage ratio of carbon tetrachloride, dimethyl phosphate, hydroxyl-terminated monomer, triethylamine and tetrahydrofuran is 4.6 by mass: 3:2:3.5:3.
further, the antioxidant is prepared by the steps of:
adding hydroxyl-terminated hyperbranched poly (amine-ester) and triethylamine into chloroform, adding 3, 5-di-tert-butyl-4-hydroxybenzoyl chloride, stirring under nitrogen protection and ice water bath conditions for reaction for 2 hours, heating to 20 ℃, continuing to react for 1 hour, washing the obtained reaction system with saturated sodium bicarbonate aqueous solution, retaining an organic phase, and concentrating under reduced pressure to remove chloroform to obtain the antioxidant. Hindered phenol antioxidant is widely applied to high polymer materials, but is easy to migrate into the environment through physical diffusion, extraction and other actions, so that the antioxidant effect of the hindered phenol antioxidant is affected. In order to reduce migration loss of the hindered phenol antioxidant, the hindered phenol antioxidant is added into a hyperbranched structure, so that the oxidation resistance and migration resistance of the hindered phenol antioxidant are improved.
Further, the dosage mass ratio of the hydroxyl-terminated hyperbranched poly (amine-ester), the 3, 5-di-tert-butyl-4-hydroxybenzoyl chloride and the chloroform is 20:8:15.
further, the light stabilizer is [ 2-hydroxy-4- (octyloxy) phenyl ] phenyl ketone, the auxiliary agent is zinc borate and stearic acid, and the mass ratio is 10:1.
a production process of a disc buckle frame flame-retardant dense mesh net comprises the following steps:
mixing the raw materials in parts by weight, grinding for 40-50min by a grinder, vacuum defoaming after finishing grinding, and standing at 20 ℃ to obtain resin slurry;
the resin sizing agent is soaked and coated on terylene industrial cloth by a coating machine, and then plasticizing treatment is carried out at 180-200 ℃ to obtain the disc buckle frame flame-retardant dense mesh net.
Further, the temperature is controlled to be not more than 35 ℃ in the grinding process. Preventing the gelation from affecting the coating uniformity caused by the excessive temperature.
The invention has the beneficial effects that:
the flame-retardant plasticizer prepared by the invention belongs to epoxy plasticizers, and has plasticizing effect on polyvinyl chloride, and has better stability and compatibility with plastics due to the epoxy groups in the structure, and the water resistance is improved by matching with Si-O-Si chain segments in the structure.
The flame-retardant plasticizer replaces the conventional plasticizer and adds an inorganic flame retardant, the synergistic flame retardant with flame-retardant effect is combined with cardanol through reaction, the compatibility of the synergistic flame retardant and polyvinyl chloride is improved, the molecular weight is increased, the migration resistance of components is improved, meanwhile, the problem that the plasticizer itself has combustibility is solved, the cardanol is a natural phenolic compound containing unsaturated long-carbon chain hydrocarbon and derived from cashew shells of low-value agriculture and forestry residues, the plasticizer has good plasticizing and heat-resisting effects, and nitrogen element in 2- (allylamino) ethanol, silicon element in methyldisiloxane and phosphorus element in dimethyl phosphate are combined in the structure of the synergistic flame retardant; the introduction of the phosphorus-containing group can lead to the reduction of thermal stability, the introduction of the silicon-containing structure plays a role in compensating the influence of the phosphorus-containing group on heat resistance, and the silicon-containing structure can be pyrolyzed to generate silicon dioxide at high temperature, so that the mechanical strength of a carbon layer can be enhanced, and the silicon dioxide can form a Si-O-Si network structure inside the carbon layer, so that the combustion is further prevented, and the smoke generation amount is reduced.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparation of an antioxidant:
adding hydroxyl-terminated hyperbranched poly (amine-ester) and triethylamine into chloroform, adding 3, 5-di-tert-butyl-4-hydroxybenzoyl chloride, stirring under nitrogen protection and ice water bath conditions for reaction for 2 hours, heating to 20 ℃, continuing to react for 1 hour, washing the obtained reaction system with saturated sodium bicarbonate aqueous solution, retaining an organic phase, and concentrating under reduced pressure to remove chloroform to obtain the antioxidant. Wherein the dosage mass ratio of the hydroxyl-terminated hyperbranched poly (amine-ester), the 3, 5-di-tert-butyl-4-hydroxybenzoyl chloride and the chloroform is 20:8:15. wherein the hydroxyl-terminated hyperbranched poly (amine-ester) is synthesized by referring to the molecular design of the hyperbranched poly (amine-ester) and the preparation thereof [ J ]. Polymer journal, 2000,4 (8): the preparation method of the third generation hydroxyl-terminated hyperbranched poly (amine-ester) in the synthesis method in 412-414.
Example 2
Preparing a synergistic flame retardant:
mixing 2- (allylamino) ethanol and toluene under the protection of nitrogen, heating to 50 ℃, adding a Karster catalyst, stirring for 30-40min, adding methyl disiloxane, heating to 70 ℃ after the addition, stirring for 24h, cooling to room temperature after the reaction is finished, and distilling under reduced pressure to remove toluene to obtain a hydroxyl-terminated monomer; wherein the dosage ratio of 2- (allylamino) ethanol, methyldisiloxane, kadster catalyst and toluene is 0.02mol:0.01mol:0.2mL:100mL;
mixing carbon tetrachloride, dimethyl phosphate and tetrahydrofuran, adding hydroxyl-terminated monomers under ice water bath conditions, stirring and dispersing for 10min, adding triethylamine, heating to 20 ℃ after the addition, stirring and reacting for 11h, and distilling under reduced pressure to remove the solvent after the reaction is finished, thereby obtaining the synergistic flame retardant. Wherein, the dosage ratio of carbon tetrachloride, dimethyl phosphate, hydroxyl-terminated monomer, triethylamine and tetrahydrofuran is 4.6 by mass: 3:2:3.5:3.
example 3
Preparing a flame retardant plasticizer:
firstly, mixing cardanol, glutaric anhydride and p-toluenesulfonic acid, setting the temperature to 170 ℃ for reaction for 3 hours, setting condensation reflux in the reaction process, cooling to room temperature after the reaction is finished, adding 1, 4-dioxane, washing with deionized water, and then carrying out reduced pressure distillation to obtain an intermediate product a; the dosage mole ratio of cardanol, glutaric anhydride and p-toluenesulfonic acid is controlled to be 1:1.5:0.015
Adding the intermediate product a and the synergistic flame retardant prepared in the embodiment 2 into N, N-dimethylformamide, stirring and dispersing, then adding 1, 8-diazabicyclo undec-7-ene, heating to 60 ℃, reacting for 4 hours, and distilling under reduced pressure after the reaction is finished to obtain an intermediate product b; controlling the dosage ratio of the intermediate product a, the synergistic flame retardant, the N, N-dimethylformamide and the 1, 8-diazabicyclo undec-7-ene to be 9g:5.5g:100mL:2.5g;
and thirdly, mixing the intermediate product b, m-chloroperoxybenzoic acid and methylene dichloride, keeping the temperature of the system at 30 ℃, reacting for 3 hours, filtering the crude product after the reaction is finished, washing the crude product with saturated sodium sulfite, saturated sodium bicarbonate and distilled water, drying and filtering an organic phase with anhydrous sodium sulfate, and removing a solvent from the filtrate by reduced pressure distillation to obtain the flame-retardant plasticizer. Control the ratio of the amounts of intermediate b, m-chloroperoxybenzoic acid and dichloromethane to 3.5g:2.5g:15mL.
Example 4
Preparing a flame retardant plasticizer:
firstly, mixing cardanol, glutaric anhydride and p-toluenesulfonic acid, setting the temperature to 170 ℃ for reaction for 3 hours, setting condensation reflux in the reaction process, cooling to room temperature after the reaction is finished, adding 1, 4-dioxane, washing with deionized water, and then carrying out reduced pressure distillation to obtain an intermediate product a; the dosage mole ratio of cardanol, glutaric anhydride and p-toluenesulfonic acid is controlled to be 1:1.5:0.015
Adding the intermediate product a and the synergistic flame retardant prepared in the embodiment 2 into N, N-dimethylformamide, stirring and dispersing, then adding 1, 8-diazabicyclo undec-7-ene, heating to 60 ℃, reacting for 5 hours, and distilling under reduced pressure after the reaction is finished to obtain an intermediate product b; controlling the dosage ratio of the intermediate product a, the synergistic flame retardant, the N, N-dimethylformamide and the 1, 8-diazabicyclo undec-7-ene to be 9g:5.5g:100mL:2.5g;
and thirdly, mixing the intermediate product b, m-chloroperoxybenzoic acid and methylene dichloride, keeping the temperature of the system at 30 ℃, reacting for 3 hours, filtering the crude product after the reaction is finished, washing the crude product with saturated sodium sulfite, saturated sodium bicarbonate and distilled water, drying and filtering an organic phase with anhydrous sodium sulfate, and removing a solvent from the filtrate by reduced pressure distillation to obtain the flame-retardant plasticizer. Control the ratio of the amounts of intermediate b, m-chloroperoxybenzoic acid and dichloromethane to 3.5g:2.5g:15mL.
Comparative example 1
Mixing cardanol, m-chloroperoxybenzoic acid and methylene dichloride, maintaining the system temperature at 30 ℃, reacting for 3 hours, filtering a crude product after the reaction is finished, washing the crude product with saturated sodium sulfite, saturated sodium bicarbonate and distilled water, drying an organic phase with anhydrous sodium sulfate, filtering, and removing a solvent from the filtrate by reduced pressure distillation to obtain the flame-retardant plasticizer. Controlling the dosage ratio of cardanol, m-chloroperoxybenzoic acid and dichloromethane to 3g:2.5g:15mL.
Example 5
A production process of a disc buckle frame flame-retardant dense mesh net comprises the following steps:
mixing 80 parts by weight of PVC paste resin, 10 parts by weight of calcium carbonate, 80 parts by weight of the flame retardant plasticizer prepared in example 3, 2 parts by weight of the antioxidant prepared in example 1, 0.5 part by weight of [ 2-hydroxy-4- (octyloxy) phenyl ] phenyl ketone, 1 part by weight of white carbon black and 2 parts by weight of an auxiliary agent, grinding for 40 minutes by a grinding machine, controlling the temperature in the grinding process to be not more than 35 ℃, performing vacuum defoaming after finishing grinding, and standing at the temperature of 20 ℃ to obtain resin slurry; the auxiliary agent is zinc borate and stearic acid, and the mass ratio of the auxiliary agent is 10:1.
the resin sizing agent is soaked and coated on terylene industrial cloth by a coating machine, and then plasticizing treatment is carried out at 180 ℃ to obtain the disc buckle frame flame-retardant dense mesh net.
Example 6
A production process of a disc buckle frame flame-retardant dense mesh net comprises the following steps:
mixing 85 parts of PVC paste resin, 12 parts of calcium carbonate, 90 parts of the flame retardant plasticizer prepared in the example 4, 3 parts of the antioxidant prepared in the example 1, 1 part of [ 2-hydroxy-4- (octyloxy) phenyl ] phenyl ketone, 2 parts of white carbon black and 4 parts of auxiliary agent according to parts by weight, grinding for 50 minutes by a grinding machine, controlling the temperature in the grinding process to be not more than 35 ℃, performing vacuum defoaming after finishing grinding, and standing at the temperature of 20 ℃ to obtain resin slurry; the auxiliary agent is zinc borate and stearic acid, and the mass ratio of the auxiliary agent is 10:1.
the resin sizing agent is soaked and coated on terylene industrial cloth by a coating machine, and then plasticizing treatment is carried out at the temperature of 200 ℃ to obtain the disc buckle frame flame-retardant dense mesh net.
Example 7
A production process of a disc buckle frame flame-retardant dense mesh net comprises the following steps:
mixing 90 parts of PVC paste resin, 12 parts of calcium carbonate, 90 parts of the flame retardant plasticizer prepared in example 4, 3 parts of the antioxidant prepared in example 1, 1 part of [ 2-hydroxy-4- (octyloxy) phenyl ] phenyl ketone, 2 parts of white carbon black and 4 parts of auxiliary agent according to parts by weight, grinding for 50 minutes by a grinding machine, controlling the temperature in the grinding process to be not more than 35 ℃, performing vacuum defoaming after finishing grinding, and standing at the temperature of 20 ℃ to obtain resin slurry; the auxiliary agent is zinc borate and stearic acid, and the mass ratio of the auxiliary agent is 10:1.
the resin sizing agent is soaked and coated on terylene industrial cloth by a coating machine, and then plasticizing treatment is carried out at the temperature of 200 ℃ to obtain the disc buckle frame flame-retardant dense mesh net.
Comparative example 2
The flame retardant plasticizer of example 7 was replaced with the sample prepared in comparative example 1, and the remaining raw materials and preparation process were kept unchanged.
Comparative example 3
The antioxidant in example 7 was replaced with antioxidant 1010.
Samples prepared in examples 5-7 and comparative examples 2-3 were tested and the test results are shown in Table 1 below: wherein the flame retardant property Limiting Oxygen Index (LOI) test method refers to GB/T2406-2008; vertical burn test (UL 94V) reference GB/T5455-1997; mechanical properties test reference GB/T1040-2006 "determination of tensile Properties of plastics", each sample was tested 5 times in parallel, and the average value was taken, and the sample size was 100 mm. Times.100 mm. Times.2 mm. The thermal aging oven was used to conduct a thermal aging test at 185 ℃ to record the overall discoloration time of the sample after thermal aging, and then the reduction rate of tensile strength and elongation at break after aging for 140 minutes was tested under the same conditions.
TABLE 1
From the test results, the sample prepared by the invention has good flame retardance, good heat aging resistance effect and more stable property.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (3)
1. A flame-retardant dense mesh net of a plate buckle frame comprises terylene industrial cloth and resin slurry coated on the surface; the resin slurry is characterized by comprising the following raw materials in parts by weight: 80-90 parts of PVC paste resin, 10-12 parts of calcium carbonate, 80-90 parts of flame retardant plasticizer, 2-3 parts of antioxidant, 0.5-1 part of light stabilizer and 1-2 parts of white carbon black; 2-4 parts of auxiliary agent;
the flame retardant plasticizer is prepared by the following steps:
firstly, mixing cardanol, glutaric anhydride and p-toluenesulfonic acid, and reacting for 3 hours at the temperature of 170 ℃ to obtain an intermediate product a; the molar ratio of the cardanol to the glutaric anhydride to the p-toluenesulfonic acid is 1:1.5:0.015;
adding the intermediate product a and the synergistic flame retardant into N, N-dimethylformamide, stirring and dispersing, then adding 1, 8-diazabicyclo undec-7-ene, heating to 60 ℃, and reacting for 4-5 hours to obtain an intermediate product b; the dosage ratio of the intermediate product a, the synergistic flame retardant, the N, N-dimethylformamide and the 1, 8-diazabicyclo undec-7-ene is 9g:5.5g:100mL:2.5g;
thirdly, mixing the intermediate product b, m-chloroperoxybenzoic acid and methylene dichloride, keeping the temperature of the system at 30 ℃, and reacting for 3 hours to obtain a flame-retardant plasticizer; intermediate b, m-chloroperoxybenzoic acid and dichloromethane in a ratio of 3.5g:2.5g:15mL;
the synergistic flame retardant is prepared by the following steps:
step one, mixing 2- (allylamino) ethanol and toluene under the protection of nitrogen, heating to 50 ℃, adding a Karster catalyst, stirring for 30-40min, adding methyl disiloxane, heating to 70 ℃ after the addition is finished, and stirring for reacting for 24h to obtain a hydroxyl-terminated monomer; the ratio of the amount of 2- (allylamino) ethanol, methyldisiloxane, the Kadster catalyst and toluene was 0.02mol:0.01mol:0.2mL:100mL;
mixing carbon tetrachloride, dimethyl phosphate and tetrahydrofuran, adding hydroxyl-terminated monomers under ice water bath conditions, stirring and dispersing for 10min, adding triethylamine, heating to 20 ℃ after the addition, and stirring and reacting for 11h to obtain a synergistic flame retardant; the dosage ratio of carbon tetrachloride, dimethyl phosphate, hydroxyl-terminated monomer, triethylamine and tetrahydrofuran is 4.6 by mass: 3:2:3.5:3, a step of;
the antioxidant is prepared by the following steps:
adding hydroxyl-terminated hyperbranched poly (amine-ester) and triethylamine into chloroform, then adding 3, 5-di-tert-butyl-4-hydroxybenzoyl chloride, stirring under nitrogen protection and ice water bath conditions for reaction for 2 hours, then heating to 20 ℃, and continuing to react for 1 hour to obtain an antioxidant; the dosage mass ratio of the hydroxyl-terminated hyperbranched poly (amine-ester), the 3, 5-di-tert-butyl-4-hydroxybenzoyl chloride and the chloroform is 20:8:15.
2. the process for producing the disc buckle frame flame-retardant dense mesh net according to claim 1, which is characterized by comprising the following steps:
mixing the raw materials, grinding for 40-50min by a grinder, and vacuum defoaming after finishing grinding to obtain resin slurry; the resin sizing agent is soaked and coated on terylene industrial cloth by a coating machine, and then plasticizing treatment is carried out at 180-200 ℃ to obtain the disc buckle frame flame-retardant dense mesh net.
3. The process for producing a flame retardant dense mesh net for a disc buckle according to claim 2, wherein the temperature is controlled to be not more than 35 ℃ during the grinding process.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286498A (en) * | 2017-05-16 | 2017-10-24 | 安徽中意胶带有限责任公司 | The Fabric Solid-woven Fire-resistant Conveyer Belt and its manufacture method of a kind of high abrasion |
| CN108864830A (en) * | 2018-05-31 | 2018-11-23 | 江苏亿博新材料科技有限公司丹阳分公司 | A kind of compound net materials specific complex coating paste of high-strength anti-flaming type glass and its preparation method and application |
| CN109518475A (en) * | 2018-11-28 | 2019-03-26 | 海宁卓益篷盖材料有限公司 | A kind of manufacture craft of matt grid cloth |
| CN112480565A (en) * | 2020-11-27 | 2021-03-12 | 江苏华信新材料股份有限公司 | Phosphorus-containing cardanol-based flame-retardant plasticizer for modified polyvinyl chloride and preparation method and application thereof |
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| WO2005061607A1 (en) * | 2003-12-19 | 2005-07-07 | Supresta Llc | Arylalkylsilyls used as flame retardant additives |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286498A (en) * | 2017-05-16 | 2017-10-24 | 安徽中意胶带有限责任公司 | The Fabric Solid-woven Fire-resistant Conveyer Belt and its manufacture method of a kind of high abrasion |
| CN108864830A (en) * | 2018-05-31 | 2018-11-23 | 江苏亿博新材料科技有限公司丹阳分公司 | A kind of compound net materials specific complex coating paste of high-strength anti-flaming type glass and its preparation method and application |
| CN109518475A (en) * | 2018-11-28 | 2019-03-26 | 海宁卓益篷盖材料有限公司 | A kind of manufacture craft of matt grid cloth |
| CN112480565A (en) * | 2020-11-27 | 2021-03-12 | 江苏华信新材料股份有限公司 | Phosphorus-containing cardanol-based flame-retardant plasticizer for modified polyvinyl chloride and preparation method and application thereof |
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