CN110130148A - A kind of preparation method of fire retardant papers - Google Patents
A kind of preparation method of fire retardant papers Download PDFInfo
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- CN110130148A CN110130148A CN201910416410.7A CN201910416410A CN110130148A CN 110130148 A CN110130148 A CN 110130148A CN 201910416410 A CN201910416410 A CN 201910416410A CN 110130148 A CN110130148 A CN 110130148A
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- ammonium polyphosphate
- fire retardant
- diatomite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/40—Polyphosphates
- C01B25/405—Polyphosphates of ammonium
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/66—Salts, e.g. alums
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/71—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes
- D21H17/74—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes of organic and inorganic material
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/34—Ignifugeants
Abstract
The present invention relates to a kind of preparation methods of fire retardant papers, belong to paper flame-proof field of material technology.The present invention is by sol-gel method in the ammonium polyphosphate surface ammonium polyphosphate of the modified obtained microcapsule coated of methyltriethoxysilane, improve the water resistance and thermal stability of ammonium polyphosphate, fire retardant papers are improved in the thermal stability and neat coal amout of high-temperature region, the heat release in combustion process is effectively reduced, and significantly improves the flame retardant property of fire retardant papers；The present invention utilizes the features such as porosity and high adsorption of diatomite and ammonium polyphosphate modifying, antimony pentoxide and aluminium hydroxide in-situ polymerization, prepare the composite flame-retardant agent with good absorption smog, using diatomite as carrier, utilize its porosity and high adsorption, in its hole and in situ Polymerization, prepare a kind of composite flame-retardant agent with highly effective flame-retardant effect, the addition of composite flame-retardant agent makes page reach good flame retardant effect, and influence of the reduction to paper physical property, improve its quality and the scope of application.
Description
Technical field
The present invention relates to a kind of preparation methods of fire retardant papers, belong to paper flame-proof field of material technology.
Background technique
Paper and paper products, the overwhelming majority are manufactured paper with pulp by plant fiber, are all to be made of in structure fiber interweaving.But
Due to the combustibility of plant fiber, this just determines that the fire protection flame retarding of paper and paper products has special meaning.Therefore, various
Paper base material always is the emphasis of fire-fighting work including cardboard, paper package product, indoor paper decorative product etc..It is many simultaneously
Special occasions requires paper base material flame retardant property with higher, as electrical insulating material, smoke filtration bag, space flight and aviation are used
Paper can heat paper lunch-box etc., and also just to paper-based products, more stringent requirements are proposed, and anti-flammability is also increasingly taken seriously.
It is fire-retardant to paper and paper products progress, exactly try the thermal decomposition for hindering fiber, inhibits the generation of imflammable gas, or
Person is achieved the goal by isolation heat and air and dilution imflammable gas.Paper is assigned it can be seen from the combustion mechanism of paper
With anti-flammability of preventing fires, general flame-retarding means are studied from destroying flammable system.Fire retardant generally passes through a kind of or several
Kind of approach reaches fire-retardant purpose:
(1) endothermic effect；
(2) dilution effect；
(3) depression effect；
(4) blanketing effect；
(5) charcoal amount increases and volatile matter reduces theory.
Currently, the production method of paper flame-proof material mainly has following five kinds:
It (1) is that raw material is directly manufactured paper with pulp using inorfil；
(2) additive process in starching；
(3) infusion process；
(4) rubbing method；
(5) spray-on process.
In practice, fire retardant papers difference occasion, the flame retardant property and physics of paper products, the requirement of mechanical performance is not
Together, but the following are the characteristics that it has jointly:
(1) it is able to satisfy the different flame retardant properties requirement of different product proposition, especially in high-tech, high risk occasion
Material, flame retardant property will not be decreased obviously with the extension of use time.
Used fire retardant decomposition temperature is suitable for not decomposing in process, rotten candle will not being caused to equipment
And operating environment is polluted.
Influence of the fire retardant of use to the mechanical strength of product, whiteness and other performance index can receive.Make
With in the process, the hygroscopicity of product is unobvious, and brightness reversion does not occur, and strength reduction is few.
Gas that fire retardant papers generate in combustion and the cigarette emerged not harmful to human.
Fire retardant is cheap.Currently, the fire-retardant paper products that can fully meet above-mentioned requirements in the market are also seldom, it is also necessary to
Further research.
With the enhancing that people's fire protection flame retarding is realized, fire retardant papers and its product will be developed faster, and field also will
Constantly widen.
Summary of the invention
The technical problems to be solved by the invention: for the problem that existing fire retardant papers flame retardant property is poor, one kind is provided
The preparation method of fire retardant papers.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) ammonium polyphosphate is taken, the ethanol solution that mass fraction is 50%, methyltriethoxysilane, by ammonium polyphosphate and quality point
Number mixes for 50% ethanol solution, and for 5~10min of ultrasonic disperse to get dispersion liquid, it is molten to get mixing to adjust the pH value of dispersion liquid
Liquid A, is added methyltriethoxysilane in mixed solution A, is stirred to get mixed solution B, filters up to filtering
Filter residue is washed and is dried, is cooled to room temperature to get ammonium polyphosphate modifying by slag；
(2) ammonium polyphosphate modifying, diatomite, aluminium hydroxide, antimony pentoxide are taken, ammonium polyphosphate modifying and diatomite are mixed equal
It is even, carry out isothermal holding to get mixture, aluminium hydroxide and antimony pentoxide be added in the mixture, continue heat preservation 30~
40min is placed in curing process in baking oven to get semi-finished product, by semi-finished product, is cooled to room temperature, and grinds to get composite flame-retardant agent；
(3) composite flame-retardant agent and paper pulp are uniformly mixed to get mixed pulp, mixed pulp is placed in paper machine and carries out copy paper
Processing is to get fire retardant papers.
Ammonium polyphosphate described in step (1), the ethanol solution that mass fraction is 50%, between methyltriethoxysilane
Ratio is respectively as follows: according to parts by weight, weighs 10~15 parts of ammonium polyphosphate respectively, the ethyl alcohol that 40~50 parts of mass fractions are 50%
Solution, 0.3~0.5 part of methyltriethoxysilane.
The step of pH value of dispersion liquid is adjusted described in step (1) are as follows: adjust dispersion liquid with mass fraction for 2% ammonium hydroxide
PH value is 9~10.
Methyltriethoxysilane is added described in (1) in step in mixed solution A, is stirred step are as follows:
Methyltriethoxysilane is added in mixed solution A, is 40~50 DEG C in temperature, mixing speed is to stir under 100~160r/min
Mix 2~3h of reaction.
Filter residue is washed described in (1) and is dried step by step are as follows: it is washed with deionized filter residue 2~4 times,
It is placed in the baking oven that temperature is 40~60 DEG C and dries to constant weight.
Ammonium polyphosphate modifying described in step (2), diatomite, aluminium hydroxide, the ratio between antimony pentoxide are respectively as follows:
According to parts by weight, weigh respectively 20~30 parts of ammonium polyphosphate modifyings, 1~5 part of diatomite, 2~8 parts of aluminium hydroxides, 0.2~
0.5 part of antimony pentoxide.
Ammonium polyphosphate modifying and diatomite are uniformly mixed by step described in (2), carry out isothermal holding step are as follows: will be modified
Ammonium polyphosphate and diatomite are uniformly mixed, and keep the temperature 20~30min at being 130~140 DEG C in temperature.
Semi-finished product are placed in curing process step in baking oven described in step (2) are as follows: by semi-finished product be placed in temperature be 210~
Solidify 2~3h in 220 DEG C of baking oven.
Mass ratio described in step (3) between composite flame-retardant agent and paper pulp is 1: 10.
Mixed pulp is placed in progress copy paper processing step in paper machine described in step (3) are as follows: be placed in mixed pulp
It is 120gm in Substance in paper machine-2Lower copy paper.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention utilizes the features such as porosity and high adsorption of diatomite and ammonium polyphosphate modifying, antimony pentoxide and hydrogen
Aluminium oxide in-situ polymerization prepares the composite flame-retardant agent with good absorption smog, and diatomite can reduce the cost of paper, improves
Paper White Degree；Ammonium polyphosphate is a kind of phosphorous, nitrogen inorganic fire retardants, has thermal stability good, and flame-retarded efficiency is high, safety and environmental protection
The advantages that, ammonium polyphosphate is fire-retardant to have the gentle phase fire retardation of condensed phase fire retardation concurrently, and reaction of decomposing at high temperature generates
Polyphosphoric acid and poly-metaphosphoric acid dehydrating agent can promote material dehydration charing, effectively isolation temperature, flame is propagated further, simultaneously
The non-flammable gases diluent airs such as ammonia, water vapour are released, burning is prevented, in addition it may occur from being terminated instead by base under high temperature
It answers, terminates burning；Diatomite is a kind of nonmetallic mineral with porous structure, has large specific surface area, strong adsorption etc.
Feature, and it is cheap, resourceful；Diatomite is also simultaneously a kind of papermaking filler, so utilizing it using diatomite as carrier
Porosity and high adsorption prepare a kind of composite flame-proof with highly effective flame-retardant effect in its hole and in situ Polymerization
Agent, the addition of composite flame-retardant agent makes page reach good flame retardant effect, and reduces the influence to paper physical property, improves it
Quality and the scope of application；
(2) present invention is by sol-gel method in the ammonium polyphosphate surface modified obtained microcapsules packet of methyltriethoxysilane
The ammonium polyphosphate covered improves the water resistance and thermal stability of ammonium polyphosphate, improves fire retardant papers in the thermal stability of high-temperature region
And neat coal amout, the heat release in combustion process is effectively reduced, and significantly improve the flame retardant property of fire retardant papers；
(3) antimony pentoxide and aluminium hydroxide synergistic effect in the present invention, play good fire retardation, antimony pentoxide has
The advantages that permeability is strong, adhesion strength is big, good flame retardation effect, flame retardant property is lasting, aluminium hydroxide is from the material combustion smoke stage
It is the condensed phase fire retardant that release vapor is decomposed by the endothermic reaction, aluminium hydroxide thermal dehydration can inhibit to suppression cigarette effect
The heating of fire proofing；Its decompose generate vapor can dilution oxygen and fuel gas concentration, to prevent to burn；Work as hydrogen
When heating alumina, the water being released absorbs heat, makes it into the gas phase fire-retardant stage, keeps the material of burning lower than kindling
Point, meanwhile, the water released and the fire retardant gas dilution decomposited the oxygen content of combustion zone have effectively blocked fiber
Further combustion decomposition；Aluminium oxide can generate one layer of inert oxide layer, further protect fiber in further decomposable process
Material, and air-isolation and heat source.
Specific embodiment
According to parts by weight, it is molten for 50% ethyl alcohol that 10~15 parts of ammonium polyphosphate, 40~50 parts of mass fractions are weighed respectively
Liquid, 0.3~0.5 part of methyltriethoxysilane mix the ethanol solution that ammonium polyphosphate and mass fraction are 50%, ultrasound point
5~10min is dissipated to get dispersion liquid, is 9~10 to get mixed solution with the pH value that mass fraction is 2% ammonium hydroxide adjusting dispersion liquid
Methyltriethoxysilane is added in A in mixed solution A, is 40~50 DEG C in temperature, mixing speed is 100~160r/min
Under be stirred to react 2~3h to get mixed solution B, filter up to filter residue, be washed with deionized filter residue 2~4 times, be placed in temperature
Degree is cooled to room temperature to dry in 40~60 DEG C of baking oven to constant weight to get ammonium polyphosphate modifying；According to parts by weight, respectively
20~30 parts of ammonium polyphosphate modifyings, 1~5 part of diatomite, 2~8 parts of aluminium hydroxides, 0.2~0.5 part of antimony pentoxide are weighed, it will
Ammonium polyphosphate modifying and diatomite are uniformly mixed, at being 130~140 DEG C in temperature 20~30min of heat preservation to get mixture,
Aluminium hydroxide and antimony pentoxide are added in mixture, continues 30~40min of heat preservation to get semi-finished product, semi-finished product is placed in temperature
Degree is cooled to room temperature, grinds to get composite flame-retardant agent to solidify 2~3h in 210~220 DEG C of baking oven；In mass ratio 1: 10 will
Composite flame-retardant agent and paper pulp are uniformly mixed to get mixed pulp, and mixed pulp is placed in paper machine, is in Substance
120g·m-2Lower copy paper is to get fire retardant papers.
Example 1
Ammonium polyphosphate is taken, the ethanol solution that mass fraction is 50%, methyltriethoxysilane, by ammonium polyphosphate and mass fraction
It being mixed for 50% ethanol solution, ultrasonic disperse 5min adjusts the pH value of dispersion liquid to get mixed solution A to get dispersion liquid,
Methyltriethoxysilane is added in mixed solution A, is stirred to get mixed solution B, filters up to filter residue, will filter
Slag is washed and is dried, and is cooled to room temperature to get ammonium polyphosphate modifying；Take ammonium polyphosphate modifying, diatomite, hydroxide
Aluminium, antimony pentoxide, ammonium polyphosphate modifying and diatomite are uniformly mixed, and carry out isothermal holding to get mixture, in mixture
Middle addition aluminium hydroxide and antimony pentoxide continue to keep the temperature 30min to get semi-finished product, semi-finished product are placed in baking oven at solidification
Reason, is cooled to room temperature, and grinds to get composite flame-retardant agent；Composite flame-retardant agent and paper pulp are uniformly mixed to get mixed pulp, it will
Mixed pulp, which is placed in paper machine, carries out copy paper processing to get fire retardant papers.Ammonium polyphosphate, mass fraction be 50% ethanol solution,
Ratio between methyltriethoxysilane is respectively as follows: according to parts by weight, weighs 10 parts of ammonium polyphosphate, 40 parts of quality point respectively
Count the ethanol solution for 50%, 0.3 part of methyltriethoxysilane.The step of adjusting the pH value of dispersion liquid are as follows: be with mass fraction
The pH value that 2% ammonium hydroxide adjusts dispersion liquid is 9.Methyltriethoxysilane is added in mixed solution A, is stirred step
Are as follows: methyltriethoxysilane is added in mixed solution A, is 40 DEG C in temperature, mixing speed is to stir instead under 100r/min
Answer 2h.Filter residue is washed and is dried step are as follows: is washed with deionized filter residue 2 times, being placed in temperature is 40 DEG C
It dries in baking oven to constant weight.Ammonium polyphosphate modifying, diatomite, aluminium hydroxide, the ratio between antimony pentoxide are respectively as follows: by weight
Number meter is measured, weighs 20 parts of ammonium polyphosphate modifyings, 1 part of diatomite, 2 parts of aluminium hydroxides, 0.2 part of antimony pentoxide respectively.It will change
Property ammonium polyphosphate and diatomite be uniformly mixed, carry out isothermal holding step are as follows: ammonium polyphosphate modifying and diatomite are uniformly mixed,
20min is kept the temperature at being 130 DEG C in temperature.Semi-finished product are placed in curing process step in baking oven are as follows: semi-finished product, which are placed in temperature, is
Solidify 2h in 210 DEG C of baking oven.Mass ratio between composite flame-retardant agent and paper pulp is 1: 10.Mixed pulp is placed in paper machine
Carry out copy paper processing step are as follows: mixed pulp is placed in paper machine, is 120gm in Substance-2Lower copy paper.
Example 2
Ammonium polyphosphate is taken, the ethanol solution that mass fraction is 50%, methyltriethoxysilane, by ammonium polyphosphate and mass fraction
It being mixed for 50% ethanol solution, ultrasonic disperse 6min adjusts the pH value of dispersion liquid to get mixed solution A to get dispersion liquid,
Methyltriethoxysilane is added in mixed solution A, is stirred to get mixed solution B, filters up to filter residue, will filter
Slag is washed and is dried, and is cooled to room temperature to get ammonium polyphosphate modifying；Take ammonium polyphosphate modifying, diatomite, hydroxide
Aluminium, antimony pentoxide, ammonium polyphosphate modifying and diatomite are uniformly mixed, and carry out isothermal holding to get mixture, in mixture
Middle addition aluminium hydroxide and antimony pentoxide continue to keep the temperature 33min to get semi-finished product, semi-finished product are placed in baking oven at solidification
Reason, is cooled to room temperature, and grinds to get composite flame-retardant agent；Composite flame-retardant agent and paper pulp are uniformly mixed to get mixed pulp, it will
Mixed pulp, which is placed in paper machine, carries out copy paper processing to get fire retardant papers.Ammonium polyphosphate, mass fraction be 50% ethanol solution,
Ratio between methyltriethoxysilane is respectively as follows: according to parts by weight, weighs 11 parts of ammonium polyphosphate, 43 parts of quality point respectively
Count the ethanol solution for 50%, 0.4 part of methyltriethoxysilane.The step of adjusting the pH value of dispersion liquid are as follows: be with mass fraction
The pH value that 2% ammonium hydroxide adjusts dispersion liquid is 9.3.Methyltriethoxysilane is added in mixed solution A, is stirred step
Suddenly are as follows: methyltriethoxysilane is added in mixed solution A, is 43 DEG C in temperature, mixing speed is to stir under 120r/min
React 2h.Filter residue is washed and is dried step are as follows: is washed with deionized filter residue 3 times, being placed in temperature is 49 DEG C
Baking oven in dry to constant weight.Ammonium polyphosphate modifying, diatomite, aluminium hydroxide, the ratio between antimony pentoxide be respectively as follows: by
Parts by weight meter weighs 23 parts of ammonium polyphosphate modifyings, 2 parts of diatomite, 4 parts of aluminium hydroxides, 0.3 part of antimony pentoxide respectively.It will
Ammonium polyphosphate modifying and diatomite are uniformly mixed, and carry out isothermal holding step are as follows: are mixed ammonium polyphosphate modifying and diatomite equal
It is even, 23min is kept the temperature at being 133 DEG C in temperature.Semi-finished product are placed in curing process step in baking oven are as follows: semi-finished product are placed in temperature
To solidify 2h in 213 DEG C of baking ovens.Mass ratio between composite flame-retardant agent and paper pulp is 1: 10.Mixed pulp is placed in paper machine
Middle progress copy paper processing step are as follows: mixed pulp is placed in paper machine, is 120gm in Substance-2Lower copy paper.
Example 3
Ammonium polyphosphate is taken, the ethanol solution that mass fraction is 50%, methyltriethoxysilane, by ammonium polyphosphate and mass fraction
It being mixed for 50% ethanol solution, ultrasonic disperse 7min adjusts the pH value of dispersion liquid to get mixed solution A to get dispersion liquid,
Methyltriethoxysilane is added in mixed solution A, is stirred to get mixed solution B, filters up to filter residue, will filter
Slag is washed and is dried, and is cooled to room temperature to get ammonium polyphosphate modifying；Take ammonium polyphosphate modifying, diatomite, hydroxide
Aluminium, antimony pentoxide, ammonium polyphosphate modifying and diatomite are uniformly mixed, and carry out isothermal holding to get mixture, in mixture
Middle addition aluminium hydroxide and antimony pentoxide continue to keep the temperature 36min to get semi-finished product, semi-finished product are placed in baking oven at solidification
Reason, is cooled to room temperature, and grinds to get composite flame-retardant agent；Composite flame-retardant agent and paper pulp are uniformly mixed to get mixed pulp, it will
Mixed pulp, which is placed in paper machine, carries out copy paper processing to get fire retardant papers.Ammonium polyphosphate, mass fraction be 50% ethanol solution,
Ratio between methyltriethoxysilane is respectively as follows: according to parts by weight, weighs 12 parts of ammonium polyphosphate, 46 parts of quality point respectively
Count the ethanol solution for 50%, 0.4 part of methyltriethoxysilane.The step of adjusting the pH value of dispersion liquid are as follows: be with mass fraction
The pH value that 2% ammonium hydroxide adjusts dispersion liquid is 9.6.Methyltriethoxysilane is added in mixed solution A, is stirred step
Suddenly are as follows: methyltriethoxysilane is added in mixed solution A, is 46 DEG C in temperature, mixing speed is to stir under 140r/min
React 2h.Filter residue is washed and is dried step are as follows: is washed with deionized filter residue 3 times, being placed in temperature is 55 DEG C
Baking oven in dry to constant weight.Ammonium polyphosphate modifying, diatomite, aluminium hydroxide, the ratio between antimony pentoxide be respectively as follows: by
Parts by weight meter weighs 26 parts of ammonium polyphosphate modifyings, 3 parts of diatomite, 6 parts of aluminium hydroxides, 0.4 part of antimony pentoxide respectively.It will
Ammonium polyphosphate modifying and diatomite are uniformly mixed, and carry out isothermal holding step are as follows: are mixed ammonium polyphosphate modifying and diatomite equal
It is even, 26min is kept the temperature at being 136 DEG C in temperature.Semi-finished product are placed in curing process step in baking oven are as follows: semi-finished product are placed in temperature
To solidify 2h in 216 DEG C of baking ovens.Mass ratio between composite flame-retardant agent and paper pulp is 1: 10.Mixed pulp is placed in paper machine
Middle progress copy paper processing step are as follows: mixed pulp is placed in paper machine, is 120gm in Substance-2Lower copy paper.
Example 4
Ammonium polyphosphate is taken, the ethanol solution that mass fraction is 50%, methyltriethoxysilane, by ammonium polyphosphate and mass fraction
It being mixed for 50% ethanol solution, ultrasonic disperse 10min adjusts the pH value of dispersion liquid to get mixed solution A to get dispersion liquid,
Methyltriethoxysilane is added in mixed solution A, is stirred to get mixed solution B, filters up to filter residue, it will
Filter residue is washed and is dried, and is cooled to room temperature to get ammonium polyphosphate modifying；Take ammonium polyphosphate modifying, diatomite, hydrogen-oxygen
Change aluminium, antimony pentoxide, ammonium polyphosphate modifying and diatomite are uniformly mixed, carries out isothermal holding to get mixture, mixing
Aluminium hydroxide and antimony pentoxide are added in object, continues to keep the temperature 40min to get semi-finished product, semi-finished product is placed in baking oven and are solidified
Processing, is cooled to room temperature, and grinds to get composite flame-retardant agent；Composite flame-retardant agent and paper pulp are uniformly mixed to get mixed pulp,
Mixed pulp is placed in paper machine and carries out copy paper processing to get fire retardant papers.Ammonium polyphosphate, the ethyl alcohol that mass fraction is 50% are molten
Ratio between liquid, methyltriethoxysilane is respectively as follows: according to parts by weight, weighs 15 parts of ammonium polyphosphate, 50 parts of matter respectively
Measure ethanol solution, the 0.5 part of methyltriethoxysilane that score is 50%.The step of adjusting the pH value of dispersion liquid are as follows: with quality point
Number is that the pH value that 2% ammonium hydroxide adjusts dispersion liquid is 10.Methyltriethoxysilane is added in mixed solution A, is stirred
Step are as follows: methyltriethoxysilane is added in mixed solution A, is 50 DEG C in temperature, mixing speed is to stir under 160r/min
Mix reaction 3h.Filter residue is washed and is dried step are as follows: is washed with deionized filter residue 4 times, being placed in temperature is 60
DEG C baking oven in dry to constant weight.Ammonium polyphosphate modifying, diatomite, aluminium hydroxide, the ratio between antimony pentoxide are respectively as follows:
According to parts by weight, 30 parts of ammonium polyphosphate modifyings, 5 parts of diatomite, 8 parts of aluminium hydroxides, 0.5 part of antimony pentoxide are weighed respectively.
Ammonium polyphosphate modifying and diatomite are uniformly mixed, isothermal holding step is carried out are as follows: mixes ammonium polyphosphate modifying and diatomite
Uniformly, 30min is kept the temperature at being 140 DEG C in temperature.Semi-finished product are placed in curing process step in baking oven are as follows: semi-finished product are placed in temperature
Solidify 3h in the baking oven that degree is 220 DEG C.Mass ratio between composite flame-retardant agent and paper pulp is 1: 10.Mixed pulp is placed in copy paper
Copy paper processing step is carried out in machine are as follows: mixed pulp is placed in paper machine, is 120gm in Substance-2Lower copy paper.
Reference examples: the fire retardant papers of Dongguan company production.
The fire retardant papers that example and reference examples are prepared are detected, specific detection is as follows:
Flame retardant property: ASTM0777-97(2002 is used) " the standard combustibility test methods of fire retardant papers and cardboard ".
Tensile strength: the measurement of paper tensile strength is carried out according to standard GB/T/T12914-2008.
Tearability: the measurement of paper tear degree is carried out according to standard GB/T/T455-2002.
Specific test result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Reference examples |
| After flame time/s | 1.9 | 2.0 | 1.9 | 1.9 | 5 |
| Burn time/s | 4.1 | 4.5 | 5.6 | 5.5 | 6.8 |
| Tensile index/Nm/g | 58.8 | 58.6 | 58.9 | 59.0 | 51.8 |
| Tear index/mNm2/g | 10.1 | 10.5 | 10.9 | 10.8 | 8.44 |
As shown in Table 1, fire retardant papers prepared by the present invention have good flame retardant property and mechanical property.
Claims (10)
1. a kind of preparation method of fire retardant papers, it is characterised in that it is specific the preparation method comprises the following steps:
(1) ammonium polyphosphate is taken, the ethanol solution that mass fraction is 50%, methyltriethoxysilane, by ammonium polyphosphate and quality point
Number mixes for 50% ethanol solution, and for 5~10min of ultrasonic disperse to get dispersion liquid, it is molten to get mixing to adjust the pH value of dispersion liquid
Liquid A, is added methyltriethoxysilane in mixed solution A, is stirred to get mixed solution B, filters up to filtering
Filter residue is washed and is dried, is cooled to room temperature to get ammonium polyphosphate modifying by slag；
(2) ammonium polyphosphate modifying, diatomite, aluminium hydroxide, antimony pentoxide are taken, ammonium polyphosphate modifying and diatomite are mixed equal
It is even, carry out isothermal holding to get mixture, aluminium hydroxide and antimony pentoxide be added in the mixture, continue heat preservation 30~
40min is placed in curing process in baking oven to get semi-finished product, by semi-finished product, is cooled to room temperature, and grinds to get composite flame-retardant agent；
(3) composite flame-retardant agent and paper pulp are uniformly mixed to get mixed pulp, mixed pulp is placed in paper machine and carries out copy paper
Processing is to get fire retardant papers.
2. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: polyphosphoric acid described in step (1)
Ammonium, the ethanol solution that mass fraction is 50%, the ratio between methyltriethoxysilane are respectively as follows: according to parts by weight, respectively
Weigh 10~15 parts of ammonium polyphosphate, the ethanol solution that 40~50 parts of mass fractions are 50%, 0.3~0.5 part of methyltriethoxy silane
Alkane.
3. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: adjusting described in step (1) point
The step of pH value of dispersion liquid are as follows: with mass fraction be 2% ammonium hydroxide adjust dispersion liquid pH value be 9~10.
4. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: step is mixing described in (1)
Methyltriethoxysilane is added in solution A, is stirred step are as follows: methyl triethoxy is added in mixed solution A
Silane is 40~50 DEG C in temperature, and mixing speed is to be stirred to react 2~3h under 100~160r/min.
5. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: by filter residue described in step (1)
It is washed and is dried step are as follows: be washed with deionized filter residue 2~4 times, be placed in the baking oven that temperature is 40~60 DEG C
Middle drying is to constant weight.
6. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: modification described in step (2) is poly-
Ammonium phosphate, diatomite, aluminium hydroxide, the ratio between antimony pentoxide are respectively as follows: according to parts by weight, weigh 20~30 respectively
Part ammonium polyphosphate modifying, 1~5 part of diatomite, 2~8 parts of aluminium hydroxides, 0.2~0.5 part of antimony pentoxide.
7. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: step will be modified described in (2)
Ammonium polyphosphate and diatomite are uniformly mixed, and carry out isothermal holding step are as follows: ammonium polyphosphate modifying and diatomite are uniformly mixed,
Temperature is that 20~30min is kept the temperature at 130~140 DEG C.
8. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: described in step (2) will half at
Product are placed in curing process step in baking oven are as follows: semi-finished product are placed in the baking oven that temperature is 210~220 DEG C and solidify 2~3h.
9. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: compound resistance described in step (3)
Firing the mass ratio between agent and paper pulp is 1: 10.
10. a kind of preparation method of fire retardant papers according to claim 1, it is characterised in that: will mixing described in step (3)
Paper pulp is placed in progress copy paper processing step in paper machine are as follows: mixed pulp is placed in paper machine, is 120g in Substance
m-2Lower copy paper.
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Application publication date: 20190816 |