CN109280368A - A kind of highly effective flame-retardant acoustic material - Google Patents

A kind of highly effective flame-retardant acoustic material Download PDF

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CN109280368A
CN109280368A CN201811098465.XA CN201811098465A CN109280368A CN 109280368 A CN109280368 A CN 109280368A CN 201811098465 A CN201811098465 A CN 201811098465A CN 109280368 A CN109280368 A CN 109280368A
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mass ratio
added
takes
mixing
highly effective
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俞小峰
陈建春
卢星
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes
    • C08L75/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/46—Polycondensates having carboxylic or carbonic ester groups in the main chain having heteroatoms other than oxygen
    • C08G18/4676—Polycondensates having carboxylic or carbonic ester groups in the main chain having heteroatoms other than oxygen containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
    • C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
    • C08G63/6884—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/6886—Dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78—Preparation processes
    • C08G63/82—Preparation processes characterised by the catalyst used
    • C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/262—Alkali metal carbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

Abstract

The present invention relates to a kind of highly effective flame-retardant acoustic materials, belong to Material Field.The present invention carries out silane coupled processing to basalt fibre, improves surface-active, mixed and modified with the sepiolite and reagent B of demagnetization, improve the adsorptivity of its component, low-temperature plasma is handled again, improves the quantity of the polar group on its surface, improves the absorbability to noise；The tricyclic phenanthrene skeleton of rosin is introduced into the polyurethane material that maleopimaric acid processed is modified in polyester polyol, the introducing in two activated centres of carboxyl and unsaturated double-bond in its structure, the heat resistance of system can be improved, more gap labyrinths again can good sound-absorbing, reach good soundproof effect, the boric acid contained can provide flame retardant effect by being reached circulation by thermal decomposition and moisture absorption；Using calcium bicarbonate, sodium bicarbonate as inorganic filler, decomposes in carbonic acid calcipexy this system of generation, further increase system flame retardant effect.The present invention solves the problem that common acoustic material soundproof effect is bad and inflammable at present.

Description

A kind of highly effective flame-retardant acoustic material
Technical field
The invention belongs to field of material technology, in particular to a kind of highly effective flame-retardant acoustic material.
Background technique
Now, in order to effectively separate noise, common settling mode is using acoustic material.Existing acoustic material one As for cement concrete, glass plate etc., the soundproof effect of these acoustic materials is not that very well, therefore common solution is The thickness of acoustic material is increased, the problem of causing in this way is that acoustic material quality is overweight, and cost is excessively high, and installation process is very not Just.Containing components such as a large amount of sulphur, lime in Industry Waste ash, giving up to this part, there are as below methods for grey processing: direct emission method, Terminal processes method, cycling and reutilization method etc..Wherein, direct emission method, untreated sulphur and lime etc. can be serious dirty in the ash that gives up Contaminate environment；Terminal processes method needs to collect all useless ashes and focuses on again, and investment is big；And cycling and reutilization method be one more Effective processing method.Acoustic material is a kind of material for acting on soundproof effect, and present acoustic material majority is at two pieces Install what rubber layer, damping material or deadening felt etc. were made between plate, the material one side service life is short, and soundproof effect is with making Declined with the time limit, another aspect anti-flammability is not high, bad practicality.
Summary of the invention
The technical problems to be solved by the invention: for commonly using at present, acoustic material soundproof effect is bad and inflammable to be asked Topic, provides a kind of highly effective flame-retardant acoustic material.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of highly effective flame-retardant acoustic material, according to the mass fraction, including following component: 3 ~ 7 parts of calcium bicarbonates, 5 ~ 10 parts of bicarbonates Sodium, 6 ~ 10 parts of silane finish, 10 ~ 15 parts of epoxy resin, 1 ~ 4 part of lubricant, 1 ~ 4 part of plasticizer, further includes: 25 ~ 40 parts multiple Close sound isolating and flame-retardant ingredient, 15 ~ 30 parts of composite polyurethane material.
The preparation method of the composite sound-insulation inflaming-retarding ingredient, includes the following steps:
(1) it takes Black Warrior mineral wool 1:12 in mass ratio ~ 20 that reagent A is added to be mixed, filtering takes filter residue to be washed with ethanol solution It washs, it is dry, dried object is obtained, takes dried object 5 ~ 8:1:20 in mass ratio ~ 30 that pretreatment sepiolite is added, reagent B is mixed, mistake Filter, takes filter residue and drying, must pre-process Black Warrior mineral wool；
(2) it takes pretreatment Black Warrior mineral wool to vacuumize, is passed through nitrogen and adjusts intraventricular pressure, carry out Low Temperature Plasma Treating, discharge, Plasma treatment material, in mass ratio 7:2 ~ 5:1:10 take NaNO2、NH4Cl, water, starch mixing, are added by 20 ~ 30:1 of ball material mass ratio Enter the mixing of zirconium oxide ball milling pearl, ball milling obtains ball milling material, takes ball milling material to be granulated, bead 5:1 ~ 3 in mass ratio is taken to take plasma treatment Material is wrapped up, dry to get composite flame-proof ingredient.
Reagent A in the step (1): 1:15 ~ 25 take silane coupling A PS that ethanol solution mixing is added in mass ratio, Up to reagent A.
Pretreatment sepiolite in the step (1): taking sepiolite to wash, dry, pulverize sieving, takes sieving particle by matter Water mixing is added than 1:15 ~ 25 in amount, obtains ore pulp, takes ore pulp high-speed stirred, is evaporated in vacuo, obtains concentrate, take concentrate superconduction Magnetic separation processing, is stored at room temperature, and filter-press dehydration is to get pretreatment sepiolite.
Reagent B: 12 ~ 16:1:5 in mass ratio in the step (1) takes acetic acid solution, sodium citrate, boric acid mixing, i.e., Obtain reagent B.
The preparation method of the composite polyurethane material, includes the following steps:
S1. in 30 ~ 45 DEG C, 6 ~ 10:4:0.1 in mass ratio takes neopentyl glycol, 5-sodium sulfo isophthalate, sad two tin mixed It closes, leads to nitrogen protection, be warming up to 200 ~ 210 DEG C, heat preservation obtains urethane intermediates, is cooled to 140 ~ 160 DEG C, and polyurethane is added The maleopimaric acid of intermediate weight 20 ~ 35%, the isophthalic acid of urethane intermediates quality 10 ~ 25%, urethane intermediates matter The trimethylolpropane of amount 6 ~ 12% is mixed, and is warming up to 165 ~ 175 DEG C, heat preservation is warming up to 220 ~ 240 DEG C, and heat preservation obtains instead It should expect, take reaction material 10:1 in mass ratio ~ 3 that dimethylbenzene mixing is added, heat preservation reflux is cooled to 145 ~ 160 DEG C, it is warming up to 190 ~ 210 DEG C, decompression vacuum pumping, cooling discharging obtains maleopimaric acid modified polyalcohol；
S2. in 60 ~ 80 DEG C, take maleopimaric acid modified polyalcohol 5 ~ 10:1:10 in mass ratio that diethylene glycol monoethyl ether vinegar is added Acid esters, deionized water mixing, shearing dispersion obtain dispersion liquid, take dispersion liquid 15:1:3 in mass ratio ~ 6 that auxiliary agent, isophorone is added Diisocyanate is mixed, and the water that dispersion liquid quality 20 ~ 35% is added is mixed, cooling to get composite polyurethane material.
Auxiliary agent in the step S2: any one in polyurethane levelling agent RJ-600, DH-205, RM-2020.
The silane finish: any one in silane resin acceptor kh-550, KH-560, KH-570.
The lubricant: 4:1 ~ 3 take magnesium stearate, silicone oil mixing to get lubricant in mass ratio.
The plasticizer: 7 ~ 10:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticising Agent.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention carries out silane coupled processing to basalt fibre, improves surface-active, then with the sepiolite of demagnetization And reagent B is mixed and modified, improves the adsorptivity of its component, then low-temperature plasma processing, significantly improves the polar group on its surface Quantity, improve to the absorbability of noise, ball milling material wrapped up, so that noise is by the same of solid dispersion conduction sound insulation When, reduction noise can be carried out while fire-retardant, with starch to NaNO2、NH4Cl is mixed, is coated, is granulated, then by plasma Processing material package, may make NaNO when this material system is heated2And NH4Cl reaction generates nitrogen, forms gas conduction, reduces Whole heat and noise conductivity, while N2It can slowly be discharged with the raising of temperature, not only achieve the effect that heat dissipation, but also can avoid Inflammable problem；
(2) the tricyclic phenanthrene skeleton of rosin is introduced into the polyurethane material that maleopimaric acid processed is modified in polyester polyol by the present invention, The introducing in two activated centres of carboxyl and unsaturated double-bond in its structure, can be improved the heat resistance of system, more gap complexity knots Structure again can good sound-absorbing, reach good soundproof effect, the boric acid contained in system can periodically improve resistance when heated Heat dissipation effect is fired, lose a molecular water when being heated to 100 ~ 105 DEG C and forms metaboric acid, and is heated when 105 ~ 160 DEG C and changes For pyroboric acid, then complete dehydration forms anhydride boron oxide to higher temperature, and boron oxide has water imbibition, in use Can moisture absorption formed boric acid, and then can reach iterative cycles provide flame retardant effect；
(3) present invention is using calcium bicarbonate, sodium bicarbonate as inorganic filler, as the temperature rises, calcium bicarbonate, sodium bicarbonate meeting It decomposes and generates carbon dioxide and water, play the role of that oxygen is isolated, reach flame retardant effect, and can cooperate and generate other components generations Nitrogen, formed gas puigging, improve soundproof effect, and calcium bicarbonate generate CaCO3The heat transfer of system can be reduced again Rate, in addition, can be contacted with aqueous vapor and partial hydrolysis occurs during the silane coupling agent dispersed in system is used in this material, During high temperature, it can promote its hydrolysis and generate silanol, it is heated to be dehydrated generation siloxanes, the carbonic acid calcipexy generated will be decomposed In this system, system flame retardant effect is further increased.
Specific embodiment
Lubricant: 4:1 ~ 3 take magnesium stearate, silicone oil mixing to get lubricant in mass ratio.
Plasticizer: 7 ~ 10:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
Auxiliary agent: any one in polyurethane levelling agent RJ-600, DH-205, RM-2020.
Reagent A: 1:15 ~ 25 take silane coupling A PS that the ethanol solution that volume fraction is 95% is added and mix in mass ratio, Up to reagent A.
Reagent B: 12 ~ 16:1:5 in mass ratio take mass fraction 10% acetic acid solution, sodium citrate, boric acid mix to get Reagent B.
Pretreatment sepiolite: sepiolite is taken to wash with water 3 ~ 5 times, after moving to 60 ~ 80 DEG C of oven dryings to constant weight, in crushing Machine crushed 150 meshes, takes sieving particle 1:15 in mass ratio ~ 25 that water mixing is added, obtains ore pulp, take ore pulp with 2000 ~ After 1 ~ 3h of 3000r/min high-speed stirred, it is evaporated in vacuo to the 35 ~ 50% of original volume, obtains concentrate, take concentrate with 4.8 ~ 5.8T The superconducting magnetic separator of the high magnetic field intensity of magnetic field strength carries out 30 ~ 50min of processing, removes magnetisable material therein, is stored at room temperature 2 After ~ 5h, 120m is used2It is 4 ~ 8% to get pretreatment sepiolite that filter press, which carries out filter-press dehydration to water content,.
Silane finish: any one in silane resin acceptor kh-550, KH-560, KH-570.
The preparation method of composite sound-insulation inflaming-retarding ingredient, includes the following steps:
(1) it takes Black Warrior mineral wool 1:12 in mass ratio ~ 20 that reagent A mixing is added, 1 ~ 3h is stirred with 400 ~ 700r/min, is filtered, After taking filter residue wash 3 ~ 5 times with the ethanol solution that volume fraction is 90%, 20 are dried in 75 ~ 90 DEG C of vacuum ovens ~ for 24 hours, it obtains dry Dry object takes dried object 5 ~ 8:1:20 in mass ratio ~ 30 that pretreatment sepiolite, reagent B mixing is added, with 500 ~ 800r/min stirring 40 ~ 60min, filtering, takes filter residue in 70 ~ 90 DEG C of oven dryings, must pre-process Black Warrior mineral wool；
(2) it takes pretreatment Black Warrior mineral wool in vacuum chamber, is evacuated to 3.0 × 10-2Pa is then passed through nitrogen and adjusts intraventricular pressure To 6.0 × 10-2Pa, with the discharge frequency of dielectric barrier discharge for 190 ~ 220MHz, the air velocity of working gas is 45 ~ Under the conditions of 55FPM, 15 ~ 25min of Low Temperature Plasma Treating, discharging, plasma treatment material, in mass ratio 7:2 ~ 5:1:10 are carried out Take NaNO2、NH4Cl, deionized water, starch are mixed in ball milling device, and it is mixed that zirconium oxide ball milling pearl is added by ball 20 ~ 30:1 of material mass ratio It closes, with 350 ~ 550r/min, 1 ~ 3h of ball milling, obtains ball milling material, taking ball milling material to be granulated is 2 ~ 5mm radius bead, takes bead in mass ratio 5:1 ~ 3 take plasma treatment material to wrap up it, in 40 ~ 60 DEG C of vacuum drying ovens dry 20 ~ for 24 hours to get composite flame-proof ingredient.
The preparation method of composite polyurethane material, includes the following steps:
S1. in 30 ~ 45 DEG C, 6 ~ 10:4:0.1 in mass ratio take neopentyl glycol, 5-sodium sulfo isophthalate, sad two tin in Reaction kettle mixing, leads to nitrogen protection, is warming up to 200 ~ 210 DEG C, keeps the temperature 25 ~ 40min, obtains urethane intermediates, it is cooled to 140 ~ 160 DEG C, the maleopimaric acid of urethane intermediates quality 20 ~ 35%, the isophthalic two of urethane intermediates quality 10 ~ 25% is added The trimethylolpropane mixing of acid, urethane intermediates quality 6 ~ 12%, is warming up to 165 ~ 175 DEG C, keeps the temperature 30 ~ 50min, 220 ~ 240 DEG C are warming up to 4 ~ 8 DEG C/min rate, 55 ~ 70min is kept the temperature, obtains reaction material, reaction material 10:1 ~ 3 in mass ratio is taken to add Entering dimethylbenzene mixing, heat preservation flows back after 2 ~ 4h, 145 ~ 160 DEG C are cooled to, then be warming up to 190 ~ 210 DEG C with 3 ~ 6 DEG C/min rate, 20 ~ 45min of decompression vacuum pumping, natural cooling discharging, obtains maleopimaric acid modified polyalcohol；S2. in 60 ~ 80 DEG C, Ma Laihai is taken Diethylene glycol ether acetate alone, deionized water mixing is added in pine acid modified polyalcohol 5 ~ 10:1:10 in mass ratio, with 2000 ~ 3000r/min shearing 15 ~ 30min of dispersion, obtains dispersion liquid, takes dispersion liquid 15:1:3 in mass ratio ~ 6 that auxiliary agent, isophorone is added Diisocyanate mixing stirs 12 ~ 25min with 500 ~ 800r/min, the deionized water of dispersion liquid quality 20 ~ 35% is added, with 2000 ~ 3000r/min stirs 15 ~ 25min, and cooled to room temperature is to get composite polyurethane material.
A kind of highly effective flame-retardant acoustic material, according to the mass fraction, including following component: 3 ~ 7 parts of calcium bicarbonates, 5 ~ 10 parts of carbon Sour hydrogen sodium, 6 ~ 10 parts of silane finish, 10 ~ 15 parts of epoxy resin, 1 ~ 4 part of lubricant, 1 ~ 4 part of plasticizer, 25 ~ 40 parts it is compound every Sound flame-retardant composition, 15 ~ 30 parts of composite polyurethane material.
A kind of preparation method of highly effective flame-retardant acoustic material, includes the following steps:
(1) according to the mass fraction, including following component: 3 ~ 7 parts of calcium bicarbonates, 5 ~ 10 parts of sodium bicarbonates, 6 ~ 10 parts of silane treatments Agent, 10 ~ 15 parts of epoxy resin, 1 ~ 4 part of lubricant, 1 ~ 4 part of plasticizer, 25 ~ 40 parts of composite sound-insulation inflaming-retarding ingredients, 15 ~ 30 parts it is multiple Close polyurethane material；
(2) in 60 ~ 80 DEG C, first take silane finish, lubricant, plasticizer, composite polyurethane material, epoxy resin mixed in batch mixer It closes, after stirring 1 ~ 3h with 500 ~ 800r/min, moves to dual-screw pelletizer melting extrusion at 170 ~ 190 DEG C, dropped naturally to it Temperature is added composite sound-insulation inflaming-retarding ingredient, silane finish mixing, bicarbonate is added when being cooled to 25 ~ 45 DEG C to 50 ~ 70 DEG C Calcium, sodium bicarbonate mixing, moulding is to get highly effective flame-retardant acoustic material.
Embodiment 1
Lubricant: 4:1 in mass ratio takes magnesium stearate, silicone oil mixing to get lubricant.
Plasticizer: 7:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
Auxiliary agent: polyurethane levelling agent RJ-600.
Reagent A: 1:15 in mass ratio take silane coupling A PS be added volume fraction be 95% ethanol solution mixing to get Reagent A.
Reagent B: 12:1:5 in mass ratio takes the acetic acid solution, sodium citrate, boric acid of mass fraction 10% to mix to get examination Agent B.
Pretreatment sepiolite: sepiolite is taken to wash with water 3 times, after moving to 60 DEG C of oven dryings to constant weight, in pulverizer powder Broken 150 mesh of mistake takes sieving particle 1:15 in mass ratio that water mixing is added, obtains ore pulp, take ore pulp with 2000r/min high-speed stirred After 1h, it is evaporated in vacuo to the 35% of original volume, obtains concentrate, take the superconduction of the high magnetic field intensity of concentrate 4.8T magnetic field strength Magnetic separator carries out processing 30min, removes magnetisable material therein, after being stored at room temperature 2h, uses 120m2Filter press carries out filter-press dehydration It is 4% to get pretreatment sepiolite to water content.
Silane finish: silane resin acceptor kh-550.
The preparation method of composite sound-insulation inflaming-retarding ingredient, includes the following steps:
(1) it takes Black Warrior mineral wool 1:12 in mass ratio that reagent A mixing is added, 1h is stirred with 400r/min, filtering takes filter residue body After the ethanol solution that fraction is 90% washs 3 times, in the dry 20h of 75 DEG C of vacuum ovens, dried object is obtained, takes dried object by matter Pretreatment sepiolite, reagent B mixing is added than 5:1:20 in amount, stirs 40min with 500r/min, filtering takes filter residue to dry in 70 DEG C Case is dry, must pre-process Black Warrior mineral wool；
(2) it takes pretreatment Black Warrior mineral wool in vacuum chamber, is evacuated to 3.0 × 10-2Pa is then passed through nitrogen and adjusts intraventricular pressure To 6.0 × 10-2Pa, the discharge frequency with dielectric barrier discharge are 190MHz, and the air velocity of working gas is 45FPM condition Under, Low Temperature Plasma Treating 15min is carried out, discharging, plasma treatment material, in mass ratio 7:2:1:10 take NaNO2、NH4Cl、 Deionized water, starch are mixed in ball milling device, the mixing of zirconium oxide ball milling pearl are added by ball material mass ratio 20:1, with 350r/min ball milling 1h obtains ball milling material, and taking ball milling material to be granulated is 2mm radius bead, takes bead 5:1 in mass ratio that plasma treatment material is taken to carry out it Package, in the dry 20h of 40 DEG C of vacuum drying ovens to get composite flame-proof ingredient.
The preparation method of composite polyurethane material, includes the following steps:
S1. in 30 DEG C, 6:4:0.1 in mass ratio takes neopentyl glycol, 5-sodium sulfo isophthalate, sad two tin in reaction kettle Nitrogen protection is led in mixing, is warming up to 200 DEG C, is kept the temperature 25min, is obtained urethane intermediates, is cooled to 140 DEG C, is added in polyurethane Between the maleopimaric acid of weight 20%, the isophthalic acid of urethane intermediates quality 10%, urethane intermediates quality 6% three Hydroxymethyl-propane is mixed, and is warming up to 165 DEG C, keeps the temperature 30min, is warming up to 220 DEG C with 4 DEG C/min rate, keeps the temperature 55min, Reaction material, take reaction material 10:1 to be in mass ratio added dimethylbenzene mixing, after heat preservation reflux 2h, be cooled to 145 DEG C, then with 3 DEG C/ Min rate is warming up to 190 DEG C, decompression vacuum pumping 20min, and natural cooling discharging obtains maleopimaric acid modified polyalcohol；S2. in 60 DEG C, take maleopimaric acid modified polyalcohol 5:1:10 in mass ratio that diethylene glycol ether acetate alone, deionized water is added mixed It closes, dispersion 15min is sheared with 2000r/min, dispersion liquid is obtained, takes dispersion liquid 15:1:3 in mass ratio that auxiliary agent, isophorone is added Diisocyanate mixing is stirred 12min with 500r/min, the deionized water of dispersion liquid quality 20% is added, is stirred with 2000r/min 15min is mixed, cooled to room temperature is to get composite polyurethane material.
A kind of highly effective flame-retardant acoustic material, according to the mass fraction, including following component: 3 parts of calcium bicarbonates, 5 parts of bicarbonates Sodium, 6 parts of silane finish, 10 parts of epoxy resin, 1 part of lubricant, 1 part of plasticizer, 25 parts of composite sound-insulation inflaming-retarding ingredients, 15 parts it is multiple Close polyurethane material.
A kind of preparation method of highly effective flame-retardant acoustic material, includes the following steps:
(1) according to the mass fraction, including following component: 3 parts of calcium bicarbonates, 5 parts of sodium bicarbonates, 6 parts of silane finish, 10 parts of rings Oxygen resin, 1 part of lubricant, 1 part of plasticizer, 25 parts of composite sound-insulation inflaming-retarding ingredients, 15 parts of composite polyurethane material；
(2) in 60 DEG C, silane finish, lubricant, plasticizer, composite polyurethane material, epoxy resin is first taken to mix in batch mixer, After stirring 1h with 500r/min, dual-screw pelletizer melting extrusion at 170 DEG C is moved to, 50 DEG C is naturally cooling to it, is added Composite sound-insulation inflaming-retarding ingredient, silane finish are mixed, and calcium bicarbonate, sodium bicarbonate mixing, modeling are added when being cooled to 25 DEG C Shape is to get highly effective flame-retardant acoustic material.
Embodiment 2
Lubricant: 4:3 in mass ratio takes magnesium stearate, silicone oil mixing to get lubricant.
Plasticizer: 10:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
Auxiliary agent: polyurethane levelling agent DH-205.
Reagent A: 1:25 in mass ratio take silane coupling A PS be added volume fraction be 95% ethanol solution mixing to get Reagent A.
Reagent B: 16:1:5 in mass ratio takes the acetic acid solution, sodium citrate, boric acid of mass fraction 10% to mix to get examination Agent B.
Pretreatment sepiolite: sepiolite is taken to wash with water 5 times, after moving to 80 DEG C of oven dryings to constant weight, in pulverizer powder Broken 150 mesh of mistake takes sieving particle 1:25 in mass ratio that water mixing is added, obtains ore pulp, take ore pulp with 3000r/min high-speed stirred After 3h, it is evaporated in vacuo to the 50% of original volume, obtains concentrate, take the superconduction of the high magnetic field intensity of concentrate 5.8T magnetic field strength Magnetic separator carries out processing 50min, removes magnetisable material therein, after being stored at room temperature 5h, uses 120m2Filter press carries out filter-press dehydration It is 8% to get pretreatment sepiolite to water content.
Silane finish: Silane coupling reagent KH-570.
The preparation method of composite sound-insulation inflaming-retarding ingredient, includes the following steps:
(1) it takes Black Warrior mineral wool 1:20 in mass ratio that reagent A mixing is added, 3h is stirred with 700r/min, filtering takes filter residue body It is dry for 24 hours in 90 DEG C of vacuum ovens after the ethanol solution that fraction is 90% washs 5 times, dried object is obtained, takes dried object by matter Pretreatment sepiolite, reagent B mixing is added than 8:1:30 in amount, stirs 60min with 800r/min, filtering takes filter residue to dry in 90 DEG C Case is dry, must pre-process Black Warrior mineral wool；
(2) it takes pretreatment Black Warrior mineral wool in vacuum chamber, is evacuated to 3.0 × 10-2Pa is then passed through nitrogen and adjusts intraventricular pressure To 6.0 × 10-2Pa, the discharge frequency with dielectric barrier discharge are 220MHz, and the air velocity of working gas is 55FPM condition Under, Low Temperature Plasma Treating 25min is carried out, discharging, plasma treatment material, in mass ratio 7:5:1:10 take NaNO2、NH4Cl、 Deionized water, starch are mixed in ball milling device, the mixing of zirconium oxide ball milling pearl are added by ball material mass ratio 30:1, with 550r/min ball milling 3h obtains ball milling material, and taking ball milling material to be granulated is 5mm radius bead, takes bead 5:3 in mass ratio that plasma treatment material is taken to carry out it Package, it is dry for 24 hours to get composite flame-proof ingredient in 60 DEG C of vacuum drying ovens.
The preparation method of composite polyurethane material, includes the following steps:
S1. in 45 DEG C, 10:4:0.1 in mass ratio takes neopentyl glycol, 5-sodium sulfo isophthalate, sad two tin in reaction kettle Nitrogen protection is led in mixing, is warming up to 210 DEG C, is kept the temperature 40min, is obtained urethane intermediates, is cooled to 160 DEG C, is added in polyurethane Between the maleopimaric acid of weight 35%, the isophthalic acid of urethane intermediates quality 25%, urethane intermediates quality 12% three Hydroxymethyl-propane is mixed, and is warming up to 175 DEG C, keeps the temperature 50min, is warming up to 240 DEG C with 8 DEG C/min rate, keeps the temperature 70min, Reaction material, take reaction material 10:3 to be in mass ratio added dimethylbenzene mixing, after heat preservation reflux 4h, be cooled to 160 DEG C, then with 6 DEG C/ Min rate is warming up to 210 DEG C, decompression vacuum pumping 45min, and natural cooling discharging obtains maleopimaric acid modified polyalcohol；S2. in 80 DEG C, take maleopimaric acid modified polyalcohol 10:1:10 in mass ratio that diethylene glycol ether acetate alone, deionized water is added mixed It closes, dispersion 30min is sheared with 3000r/min, dispersion liquid is obtained, takes dispersion liquid 15:1:6 in mass ratio that auxiliary agent, isophorone is added Diisocyanate mixing is stirred 25min with 800r/min, the deionized water of dispersion liquid quality 35% is added, is stirred with 3000r/min 25min is mixed, cooled to room temperature is to get composite polyurethane material.
A kind of highly effective flame-retardant acoustic material, according to the mass fraction, including following component: 7 parts of calcium bicarbonates, 10 parts of bicarbonates Sodium, 10 parts of silane finish, 15 parts of epoxy resin, 4 parts of lubricants, 4 parts of plasticizer, 40 parts of composite sound-insulation inflaming-retarding ingredients, 30 parts Composite polyurethane material.
A kind of preparation method of highly effective flame-retardant acoustic material, includes the following steps:
(1) according to the mass fraction, including following component: 7 parts of calcium bicarbonates, 10 parts of sodium bicarbonates, 10 parts of silane finish, 15 parts Epoxy resin, 4 parts of lubricants, 4 parts of plasticizer, 40 parts of composite sound-insulation inflaming-retarding ingredients, 30 parts of composite polyurethane material；
(2) in 80 DEG C, silane finish, lubricant, plasticizer, composite polyurethane material, epoxy resin is first taken to mix in batch mixer, After stirring 3h with 800r/min, dual-screw pelletizer melting extrusion at 190 DEG C is moved to, 70 DEG C is naturally cooling to it, is added Composite sound-insulation inflaming-retarding ingredient, silane finish are mixed, and calcium bicarbonate, sodium bicarbonate mixing, modeling are added when being cooled to 45 DEG C Shape is to get highly effective flame-retardant acoustic material.
Embodiment 3
Lubricant: 4:2 in mass ratio takes magnesium stearate, silicone oil mixing to get lubricant.
Plasticizer: 8:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
Auxiliary agent: polyurethane levelling agent RM-2020.
Reagent A: 1:17 in mass ratio take silane coupling A PS be added volume fraction be 95% ethanol solution mixing to get Reagent A.
Reagent B: 13:1:5 in mass ratio takes the acetic acid solution, sodium citrate, boric acid of mass fraction 10% to mix to get examination Agent B.
Pretreatment sepiolite: sepiolite is taken to wash with water 4 times, after moving to 65 DEG C of oven dryings to constant weight, in pulverizer powder Broken 150 mesh of mistake takes sieving particle 1:17 in mass ratio that water mixing is added, obtains ore pulp, take ore pulp with 2500r/min high-speed stirred After 2h, it is evaporated in vacuo to the 40% of original volume, obtains concentrate, take the superconduction of the high magnetic field intensity of concentrate 4.9T magnetic field strength Magnetic separator carries out processing 35min, removes magnetisable material therein, after being stored at room temperature 3h, uses 120m2Filter press carries out filter-press dehydration It is 6% to get pretreatment sepiolite to water content.
Silane finish: Silane coupling reagent KH-570.
The preparation method of composite sound-insulation inflaming-retarding ingredient, includes the following steps:
(1) it takes Black Warrior mineral wool 1:17 in mass ratio that reagent A mixing is added, 2h is stirred with 500r/min, filtering takes filter residue body After the ethanol solution that fraction is 90% washs 4 times, in the dry 22h of 85 DEG C of vacuum ovens, dried object is obtained, takes dried object by matter Pretreatment sepiolite, reagent B mixing is added than 7:1:25 in amount, stirs 50min with 600r/min, filtering takes filter residue to dry in 80 DEG C Case is dry, must pre-process Black Warrior mineral wool；
(2) it takes pretreatment Black Warrior mineral wool in vacuum chamber, is evacuated to 3.0 × 10-2Pa is then passed through nitrogen and adjusts intraventricular pressure To 6.0 × 10-2Pa, the discharge frequency with dielectric barrier discharge are 200MHz, and the air velocity of working gas is 50FPM condition Under, Low Temperature Plasma Treating 20min is carried out, discharging, plasma treatment material, in mass ratio 7:3:1:10 take NaNO2、NH4Cl、 Deionized water, starch are mixed in ball milling device, the mixing of zirconium oxide ball milling pearl are added by ball material mass ratio 25:1, with 450r/min ball milling 2h obtains ball milling material, and taking ball milling material to be granulated is 3mm radius bead, takes bead 5:2 in mass ratio that plasma treatment material is taken to carry out it Package, in the dry 22h of 50 DEG C of vacuum drying ovens to get composite flame-proof ingredient.
The preparation method of composite polyurethane material, includes the following steps:
S1. in 40 DEG C, 8:4:0.1 in mass ratio takes neopentyl glycol, 5-sodium sulfo isophthalate, sad two tin in reaction kettle Nitrogen protection is led in mixing, is warming up to 205 DEG C, is kept the temperature 30min, is obtained urethane intermediates, is cooled to 150 DEG C, is added in polyurethane Between the maleopimaric acid of weight 25%, the isophthalic acid of urethane intermediates quality 15%, urethane intermediates quality 8% three Hydroxymethyl-propane is mixed, and is warming up to 170 DEG C, keeps the temperature 35min, is warming up to 230 DEG C with 6 DEG C/min rate, keeps the temperature 65min, Reaction material, take reaction material 10:2 to be in mass ratio added dimethylbenzene mixing, after heat preservation reflux 3h, be cooled to 150 DEG C, then with 5 DEG C/ Min rate is warming up to 200 DEG C, decompression vacuum pumping 35min, and natural cooling discharging obtains maleopimaric acid modified polyalcohol；S2. in 70 DEG C, take maleopimaric acid modified polyalcohol 7:1:10 in mass ratio that diethylene glycol ether acetate alone, deionized water is added mixed It closes, dispersion 25min is sheared with 2500r/min, dispersion liquid is obtained, takes dispersion liquid 15:1:5 in mass ratio that auxiliary agent, isophorone is added Diisocyanate mixing is stirred 20min with 600r/min, the deionized water of dispersion liquid quality 25% is added, is stirred with 2500r/min 20min is mixed, cooled to room temperature is to get composite polyurethane material.
A kind of highly effective flame-retardant acoustic material, according to the mass fraction, including following component: 5 parts of calcium bicarbonates, 7 parts of bicarbonates Sodium, 8 parts of silane finish, 13 parts of epoxy resin, 3 parts of lubricants, 3 parts of plasticizer, 35 parts of composite sound-insulation inflaming-retarding ingredients, 17 parts it is multiple Close polyurethane material.
A kind of preparation method of highly effective flame-retardant acoustic material, includes the following steps:
(1) according to the mass fraction, including following component: 5 parts of calcium bicarbonates, 7 parts of sodium bicarbonates, 8 parts of silane finish, 12 parts of rings Oxygen resin, 3 parts of lubricants, 3 parts of plasticizer, 30 parts of composite sound-insulation inflaming-retarding ingredients, 17 parts of composite polyurethane material；
(2) in 70 DEG C, silane finish, lubricant, plasticizer, composite polyurethane material, epoxy resin is first taken to mix in batch mixer, After stirring 2h with 600r/min, dual-screw pelletizer melting extrusion at 180 DEG C is moved to, 60 DEG C is naturally cooling to it, is added Composite sound-insulation inflaming-retarding ingredient, silane finish are mixed, and calcium bicarbonate, sodium bicarbonate mixing, modeling are added when being cooled to 35 DEG C Shape is to get highly effective flame-retardant acoustic material.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking composite sound-insulation inflaming-retarding ingredient.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking composite polyurethane material.
Comparative example 3: the acoustic material of Linyi City company production.
The acoustic material that above-described embodiment is obtained with comparative example is detected, sound-absorbing is measured by common Alpha cabin Effect carries out anti-flammability experiment according to GB/T2408:2008 standard, the sound-absorption coefficient of the acoustic material of experimental example and comparative example with And anti-flammability obtains that the results are shown in Table 1.
Table 1:
In summary, acoustic material effect of the invention is more preferable as can be seen from Table 1, is worth of widely use.

Claims (10)

1. a kind of highly effective flame-retardant acoustic material, according to the mass fraction, including following component: 3 ~ 7 parts of calcium bicarbonates, 5 ~ 10 parts of carbonic acid Hydrogen sodium, 6 ~ 10 parts of silane finish, 10 ~ 15 parts of epoxy resin, 1 ~ 4 part of lubricant, 1 ~ 4 part of plasticizer, which is characterized in that also wrap It includes: 25 ~ 40 parts of composite sound-insulation inflaming-retarding ingredients, 15 ~ 30 parts of composite polyurethane material.
2. a kind of highly effective flame-retardant acoustic material according to claim 1, which is characterized in that the composite sound-insulation inflaming-retarding ingredient Preparation method includes the following steps:
(1) it takes Black Warrior mineral wool 1:12 in mass ratio ~ 20 that reagent A is added to be mixed, filtering takes filter residue to be washed with ethanol solution It washs, it is dry, dried object is obtained, takes dried object 5 ~ 8:1:20 in mass ratio ~ 30 that pretreatment sepiolite is added, reagent B is mixed, mistake Filter, takes filter residue and drying, must pre-process Black Warrior mineral wool；
(2) it takes pretreatment Black Warrior mineral wool to vacuumize, is passed through nitrogen and adjusts intraventricular pressure, carry out Low Temperature Plasma Treating, discharge, Plasma treatment material, in mass ratio 7:2 ~ 5:1:10 take NaNO2、NH4Cl, water, starch mixing, are added by 20 ~ 30:1 of ball material mass ratio Enter the mixing of zirconium oxide ball milling pearl, ball milling obtains ball milling material, takes ball milling material to be granulated, bead 5:1 ~ 3 in mass ratio is taken to take plasma treatment Material is wrapped up, dry to get composite flame-proof ingredient.
3. a kind of highly effective flame-retardant acoustic material according to claim 2, which is characterized in that the reagent A in the step (1): 1:15 ~ 25 take silane coupling A PS that ethanol solution mixing is added to get reagent A in mass ratio.
4. a kind of highly effective flame-retardant acoustic material according to claim 2, which is characterized in that the pretreatment in the step (1) Sepiolite: taking sepiolite to wash, and dry, pulverize sieving, takes sieving particle 1:15 in mass ratio ~ 25 that water mixing is added, obtains ore pulp, Ore pulp high-speed stirred is taken, is evaporated in vacuo, is obtained concentrate, concentrate is taken to be handled with superconducting magnetic separation, be stored at room temperature, filter-press dehydration, i.e., Sepiolite must be pre-processed.
5. a kind of highly effective flame-retardant acoustic material according to claim 2, which is characterized in that the reagent B in the step (1): 12 ~ 16:1:5 in mass ratio takes acetic acid solution, sodium citrate, boric acid mixing to get reagent B.
6. a kind of highly effective flame-retardant acoustic material according to claim 1, which is characterized in that the preparation of the composite polyurethane material Method includes the following steps:
S1. in 30 ~ 45 DEG C, 6 ~ 10:4:0.1 in mass ratio takes neopentyl glycol, 5-sodium sulfo isophthalate, sad two tin mixed It closes, leads to nitrogen protection, be warming up to 200 ~ 210 DEG C, heat preservation obtains urethane intermediates, is cooled to 140 ~ 160 DEG C, and polyurethane is added The maleopimaric acid of intermediate weight 20 ~ 35%, the isophthalic acid of urethane intermediates quality 10 ~ 25%, urethane intermediates matter The trimethylolpropane of amount 6 ~ 12% is mixed, and is warming up to 165 ~ 175 DEG C, heat preservation is warming up to 220 ~ 240 DEG C, and heat preservation obtains instead It should expect, take reaction material 10:1 in mass ratio ~ 3 that dimethylbenzene mixing is added, heat preservation reflux is cooled to 145 ~ 160 DEG C, it is warming up to 190 ~ 210 DEG C, decompression vacuum pumping, cooling discharging obtains maleopimaric acid modified polyalcohol；
S2. in 60 ~ 80 DEG C, take maleopimaric acid modified polyalcohol 5 ~ 10:1:10 in mass ratio that diethylene glycol monoethyl ether vinegar is added Acid esters, deionized water mixing, shearing dispersion obtain dispersion liquid, take dispersion liquid 15:1:3 in mass ratio ~ 6 that auxiliary agent, isophorone is added Diisocyanate is mixed, and the water that dispersion liquid quality 20 ~ 35% is added is mixed, cooling to get composite polyurethane material.
7. a kind of highly effective flame-retardant acoustic material according to claim 6, which is characterized in that the auxiliary agent in the step S2: poly- Any one in urethane levelling agent RJ-600, DH-205, RM-2020.
8. a kind of highly effective flame-retardant acoustic material according to claim 1, which is characterized in that the silane finish: silane is even Join any one in agent KH-550, KH-560, KH-570.
9. a kind of highly effective flame-retardant acoustic material according to claim 1, which is characterized in that the lubricant: 4:1 in mass ratio ~ 3 take magnesium stearate, silicone oil mixing to get lubricant.
10. a kind of highly effective flame-retardant acoustic material according to claim 1, which is characterized in that the plasticizer: in mass ratio 7 ~ 10:3 takes triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
CN201811098465.XA 2018-09-20 2018-09-20 A kind of highly effective flame-retardant acoustic material Pending CN109280368A (en)

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Application publication date: 20190129