CN107586461B - A kind of preparation method of formaldehydeless flame retardant type fiberboard - Google Patents
A kind of preparation method of formaldehydeless flame retardant type fiberboard Download PDFInfo
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Abstract
The present invention relates to starch and fiber wastes application technology as the second resource field, specifically a kind of preparation method of formaldehydeless flame retardant type fiberboard.This method is by starch, sodium metaperiodate, magnesium salts carries out solid phase activation in the ball mill and prepares dialdehyde starch, then dialdehyde starch adhesive is mixed with dialdehyde starch and glue auxiliary agent, dialdehyde starch adhesive is mixed with fiber wastes, compacting obtains formaldehydeless flame retardant type fiberboard in vulcanizing press, the present invention prepares dialdehyde starch using Solid Phase Simultaneous mechanical activation oxidation reaction, sodium metaperiodate dosage is few, efficiency is high, the aldehyde radical of dialdehyde starch is up to 1.15-2.45, solubility is up to 40-50 g/100g water, the dialdehyde starch adhesive of preparation is at low cost, good dispersion, viscosity is low, adhesive strength is big, the formaldehydeless release of the fiberboard of preparation, safety and environmental protection, there is good flame retardant property simultaneously.
Description
Technical field
The present invention relates to starch and fiber wastes application technology as the second resource field, specifically a kind of formaldehydeless fire-retardant
The preparation method of fiber type plate.
Background technique
The adhesive that wood-based panel industry uses at present is mainly urea-formaldehyde resin adhesive (UF), phenolic resin glue (PF), melamine
Amine-formaldehyde resins glue (MF), they there is also significant disadvantage, that is, exist caused by Form aldehyde release while being widely applied
Toxicological hazards.Above-mentioned adhesive raw materials all derive from oil product substantially, increasingly deficient with petroleum resources, seek environmental protection,
Safety, reproducible substitute are the directions of adhesive development.In addition, the raising with modern architecture to fire protection requirement, fire-retardant
The market demand of type wood-based plate is increasing.
Starch-based adhesive is an important development direction of adhesive " Green Chemistry ".As natural adhesive, starch
Glue has long applicating history.It is easy to get with raw material, is cheap, is corrosion-free, is pollution-free, Environmental Safety, easy to use
The advantages that, it is widely used in the bonding of corrugated case, paper, trade mark, envelope etc..Dialdehyde starch as starch adhesive one
Kind, have many advantages, such as low gelatinization point, transparent, permeability and anti -precipitability it is good, it is easy film forming, adhesive property it is good, can enhance and
The bonding force of paper fiber, moreover it is possible to increase the stability and mobility of glue, and there is certain fungus-proof antisepsis ability.Numerous researchs
Scholar has inquired into the preparation of dialdehyde starch, but still generally existing using the dialdehyde starch of traditional water phase method preparation
The disadvantages such as periodate dosage is excessively high, expensive, contaminated wastewater is serious, dialdehyde content is low, and use this dialdehyde content low
Starch preparation starch adhesive storage period it is short, initial bonding strength is poor, solid content is low, moisture is high, slow drying speed, bonding strength
Low, viscosity is big, gelatin phenomenon easily occurs.Chinese patent 201610190087.2(application number) disclose a kind of dialdehyde starch and its
Preparation method, this method are that oxidant and acidolysis agent are add to deionized water and are mixed, and starch stirring is then added and matches
At starch milk, it is washed that obtained starch milk is transferred to progress acid hydrolysis oxidative reaction, the material obtained after having reacted in reaction kettle
For re-dry to get the dialdehyde starch, oxidant is sodium metaperiodate or periodic acid after to neutrality, and acidolysis agent is the salt of 36.5wt%
One or both of acid or the sulfuric acid of 98wt%, starch are cornstarch, potato starch or rice starch, oxidant 150-
257 parts, 10-300 parts of acidolysis agent, 162 parts of starch, 648-3888 parts of deionized water, i.e. sodium metaperiodate or periodic acid dosage is to form sediment
The 92.6-159% of powder dosage, it is with high costs, and a large amount of acid waste water can be generated when material washing.
Fiberboard requirement adhesive used must be good dispersion, viscosity is low, solid content is high, adhesive strength is big, simultaneously also
It is required that prepared at low cost, this is relatively difficult to achieve for general starch adhesive, and there has been no industrialized starch gluings at present
Agent production.In conclusion developing, a kind of low production cost, simple process, glue intensity is big, solid content is high, viscosity is low, environmentally friendly
Safe and pollution-free starch adhesive prepares fiberboard, can replace security risk serious plate containing formaldehyde fibers, have simultaneously
There are the good market competitiveness and economic benefit.
Summary of the invention
The purpose of the present invention is overcoming the security risk of the existing plate containing formaldehyde fibers, while solving starch adhesive cost
High, performance difference defect, provides a kind of preparation method of formaldehydeless flame retardant type fiberboard.
The scheme of the invention is realize in this way:
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprising the following steps:
(1) solid phase activation prepares dialdehyde starch: ball mill is added in the sodium metaperiodate of starch and 0.1-1.0% starch quality
Middle carry out ball milling, zirconium ball dosage are 1-3 times of starch volume, and the magnesium salts of 0.1-10% starch quality, ball milling are added in mechanical milling process
Temperature be 20-80 DEG C, revolving speed is 200-600 r/min, and the time is 10-30 min, and dialdehyde starch is obtained after the completion of ball milling；
(2) it prepares dialdehyde starch adhesive: dialdehyde starch being dissolved in the water of 1-3 times of dialdehyde starch quality, hydrogen-oxygen is added dropwise
Changing sodium solution to adjust pH value is 8-10, the glue auxiliary agent of 0.03-0.08 times of dialdehyde starch quality is added, in 70-90 DEG C, 200-
10-30 min is stirred under the revolving speed of 500 rpm and carries out addition reaction, and it is 4-6 that hydrochloric acid solution, which is then added dropwise, and adjusts pH value, is added
The glue auxiliary agent of 0.01-0.05 times of dialdehyde starch quality, under 70-90 DEG C, the revolving speed of 200-500 rpm stirring 5-20 min into
Row condensation reaction obtains dialdehyde starch adhesive；
(3) prepare formaldehydeless flame retardant type fiberboard: by the fiber wastes of dialdehyde starch adhesive and 40-80 mesh according to
The mass ratio of 0.3-1:1 mixes, and 50-80 DEG C of drying to water content is 10-15% in baking oven, then takes out mixed material and is placed in
It is hot-forming in vulcanizing press in mold, hot pressing pressure 2-10 MPa, 60-180 DEG C of hot pressing temperature, hot pressing time 5-20
Min obtains formaldehydeless flame retardant type fiberboard.
Preferably, the starch is being 3-7% using preceding drying to water content.
Preferably, the starch is any one of tapioca, potato starch, cornstarch.
Preferably, its additive amount of the sodium metaperiodate is the 0.5% of starch quality.
Preferably, its additive amount of the magnesium salts is the 0.25% of starch quality.
Preferably, the magnesium salts is any one of magnesium chloride, magnesium nitrate, magnesium sulfate, magnesium carbonate, magnesium phosphate.
Preferably, in step (2), the dialdehyde starch and the glue auxiliary agent total mass ratio are 1:0.1.
Preferably, in step (2), the glue auxiliary agent is any one of urea, phenol, melamine.
Preferably, in step (3), the dialdehyde starch adhesive and fiber wastes are mixed according to the mass ratio of 0.75:1
It closes.
Preferably, the fiber wastes are wood powder, straw powder, one kind or one kind of bagasse, manioc waste, peanut shell
Above composition.
Under the above optimum condition, formaldehydeless flame retardant type fiberboard bending strength prepared by the present invention is curved up to 14 MPa
1400 MPa of modulus in elasticity in bending, oxygen index (OI) >=30, flame retardant property reach GB8624-2006 " construction material and product burns performance
Classification " B grade standard and GB/T8625-2005 " Test method of difficultflammability for building materials " flame retardant material requirement.
The technical principle that the present invention realizes is: firstly, being reacted using synchronization mechanism active oxidation, i.e. starch, sodium metaperiodate
Solid phase, which is blended, enters mechanical activation device progress solid phase reaction, and mechanical activation is the effect by mechanical force, produces starch itself
Raw lattice defect, crystalline texture are destroyed, and starch molecular chain shortens, and reaction compartment obstacle reduces, and sodium metaperiodate is made to be easier to enter
Inside starch molecule, while some mechanical can be converted into the interior energy of molecule, and substrate reactions activation energy reduces, and sodium metaperiodate is easier
By starch oxidation, thus the dialdehyde content for improving chemical reaction rate, shortening the reaction time, increasing starch；Secondly, magnesium salts adds
Add, can produce fused salt effect, promote the destruction of crystalline structure of starch in mechanical activation process, the oxidation for facilitating periodate is made
With to obtain the dialdehyde starch of higher aldehyde group content, the dialdehyde starch viscosity in the case where periodate dosage is less
It is low, soluble easily in water, it can be configured to the starch adhesive of solid content 40-50%；Again, magnesium salts can be made micro- under mechanical activation effect
Refinement forms the inorganic salts substance with certain whisker function, to generate apparent anti-flammability in fiberboard preparation.
The present invention has following good result:
(1) present invention prepares dialdehyde starch using Solid Phase Simultaneous mechanical activation oxidation reaction, and sodium metaperiodate dosage is few, aoxidizes
Reaction efficiency is high, and the aldehyde radical of dialdehyde starch is up to 1.15-2.45, and solubility is up to 40-50 g/100g water.
(2) dialdehyde starch viscosity of the invention is low, soluble easily in water, is very beneficial to prepare starch adhesive.
(3) ureaformaldehyde starch adhesive of the invention is at low cost, good dispersion, viscosity is low, the high reachable 40-50% of solid content, glues
It is big to connect intensity.
(4) the formaldehydeless release of fiberboard of the invention, safety and environmental protection, while there is good flame retardant property.
(5) fiberboard good mechanical properties of the invention, bending strength 2-14MPa, elasticity modulus 400-1400MPa, oxygen
Index >=30, flame retardant property reach GB8624-2006 " construction material and classification of combustion properties of building materials and products " B grade standard and GB/
The requirement of T8625-2005 " Test method of difficultflammability for building materials " flame retardant material is suitble to building board intensity and fire protecting performance
Demand.
(6) present invention uses low cost starch and fiber wastes for raw material, and production cost is low, simple process, and no waste water is useless
Gas generates, and is very suitable for industrialized production.
Specific embodiment
With reference to embodiments with a kind of preparation method of formaldehydeless flame retardant type fiberboard of the description present invention, these descriptions are simultaneously
It is not to be further limited to the content of present invention.
Embodiment 1
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprising the following steps:
(1) solid phase activation prepares dialdehyde starch: by tapioca it is dry to water content be 5%, then with 0.5% tapioca
The sodium metaperiodate of quality, which is added in ball mill, carries out ball milling, and zirconium ball dosage is 2 times of tapioca volume, is added in mechanical milling process
The magnesium sulfate of 0.25% tapioca quality, the temperature of ball milling are 40 DEG C, and revolving speed is 300 r/min, and the time is 30 min, ball milling
Dialdehyde starch is obtained after the completion；
(2) it prepares dialdehyde starch adhesive: dialdehyde starch being dissolved in the water of 1.5 times of dialdehyde starch quality, hydrogen-oxygen is added dropwise
Changing sodium solution to adjust pH value is 8.5, and the urea of 0.07 times of dialdehyde starch quality is added, stirs under 85 DEG C, the revolving speed of 400 rpm
25 min carry out addition reaction, and it is 5.0 that hydrochloric acid solution, which is then added dropwise, and adjusts pH value, add the urine of 0.03 times of dialdehyde starch quality
Element stirs 20 min under 85 DEG C, the revolving speed of 400 rpm and carries out condensation reaction, obtains dialdehyde starch adhesive；
(3) formaldehydeless flame retardant type fiberboard is prepared: by the wood powder of dialdehyde starch adhesive and 60 mesh, bagasse, manioc waste
It is mixed according to the mass ratio of 0.75:1,60 DEG C of dryings to water content is 12% in baking oven, then takes out mixed material and is placed in mold
In, hot-forming in vulcanizing press, 6 MPa of hot pressing pressure, 140 DEG C of hot pressing temperature, 10 min of hot pressing time is obtained formaldehydeless
Flame retardant type fiberboard, bending strength 14.2MPa, elasticity modulus 14000MPa, oxygen index (OI) >=30.
Embodiment 2
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprising the following steps:
(1) solid phase activation prepares dialdehyde starch: by cornstarch it is dry to water content be 7%, then with 1.0% cornstarch
The sodium metaperiodate of quality, which is added in ball mill, carries out ball milling, and zirconium ball dosage is 1 times of cornstarch volume, is added in mechanical milling process
The magnesium chloride of 1% cornstarch quality, the temperature of ball milling are 60 DEG C, and revolving speed is 600 r/min, and the time is 10 min, and ball milling is completed
After obtain dialdehyde starch；
(2) it prepares dialdehyde starch adhesive: dialdehyde starch being dissolved in the water of 1 times of dialdehyde starch quality, hydroxide is added dropwise
It is 9.5 that sodium solution, which adjusts pH value, and the urea of 0.08 times of dialdehyde starch quality is added, and stirs 20 under 70 DEG C, the revolving speed of 500 rpm
Min carries out addition reaction, and it is 4 that hydrochloric acid solution, which is then added dropwise, and adjusts pH value, adds the urea of 0.05 times of dialdehyde starch quality,
70 DEG C, stir 5 min under the revolving speed of 500 rpm and carry out condensation reaction, obtain dialdehyde starch adhesive；
(3) prepare formaldehydeless flame retardant type fiberboard: by the wood powder of dialdehyde starch adhesive and 40 mesh, straw powder, bagasse,
Manioc waste, peanut shell are mixed according to the mass ratio of 0.5:1, and 80 DEG C of dryings to water content is 10% in baking oven, then take out mixing
Material is placed in mold, hot-forming in vulcanizing press, 10 MPa of hot pressing pressure, and 120 DEG C of hot pressing temperature, hot pressing time 10
Min obtains formaldehydeless flame retardant type fiberboard, bending strength 12.5MPa, elasticity modulus 1230MPa, oxygen index (OI) >=30.
Embodiment 3
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprising the following steps:
(1) solid phase activation prepares dialdehyde starch: by potato starch it is dry to water content be 3%, then with 0.5% potato
The sodium metaperiodate of starch quality, which is added in ball mill, carries out ball milling, and zirconium ball dosage is 3 times of potato starch volume, mechanical milling process
The magnesium nitrate of 3% potato starch quality of middle addition, the temperature of ball milling are 60 DEG C, and revolving speed is 300 r/min, and the time is 20 min,
Dialdehyde starch is obtained after the completion of ball milling；
(2) it prepares dialdehyde starch adhesive: dialdehyde starch being dissolved in the water of 2 times of dialdehyde starch quality, hydroxide is added dropwise
It is 10 that sodium solution, which adjusts pH value, and the phenol of 0.03 times of dialdehyde starch quality is added, and stirs 30 under 80 DEG C, the revolving speed of 300 rpm
Min carries out addition reaction, and it is 4 that hydrochloric acid solution, which is then added dropwise, and adjusts pH value, adds the phenol of 0.02 times of dialdehyde starch quality,
80 DEG C, stir 5 min under the revolving speed of 300 rpm and carry out condensation reaction, obtain dialdehyde starch adhesive；
(3) formaldehydeless flame retardant type fiberboard is prepared: by the straw powder of dialdehyde starch adhesive and 80 mesh, bagasse, peanut
Shell is mixed according to the mass ratio of 0.3:1, and 50 DEG C of dryings to water content is 15% in baking oven, is then taken out mixed material and is placed in mould
Hot-forming in vulcanizing press in tool, 4 MPa of hot pressing pressure, 90 DEG C of hot pressing temperature, 15 min of hot pressing time obtains no first
Aldehyde flame retardant type fiberboard, bending strength 8.4MPa, elasticity modulus 1020MPa, oxygen index (OI) >=30.
Embodiment 4
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprising the following steps:
(1) solid phase activation prepares dialdehyde starch: by tapioca it is dry to water content be 7%, then with 0.1% tapioca
The sodium metaperiodate of quality, which is added in ball mill, carries out ball milling, and zirconium ball dosage is 3 times of tapioca volume, is added in mechanical milling process
The magnesium carbonate of 10% tapioca starch quality, the temperature of ball milling are 20 DEG C, and revolving speed is 600 r/min, and the time is 10 min, ball
Dialdehyde starch is obtained after the completion of mill；
(2) it prepares dialdehyde starch adhesive: dialdehyde starch being dissolved in the water of 3 times of dialdehyde starch quality, hydroxide is added dropwise
It is 8 that sodium solution, which adjusts pH value, and the melamine of 0.08 times of dialdehyde starch quality is added, and is stirred under 90 DEG C, the revolving speed of 200 rpm
10 min carry out addition reaction, and it is 6 that hydrochloric acid solution, which is then added dropwise, and adjusts pH value, add the trimerization of 0.01 times of dialdehyde starch quality
Cyanamide stirs 10 min under 90 DEG C, the revolving speed of 200 rpm and carries out condensation reaction, obtains dialdehyde starch adhesive；
(3) formaldehydeless flame retardant type fiberboard is prepared: by the wood powder of dialdehyde starch adhesive and 40 mesh, straw powder, bagasse
It mixing according to the mass ratio of 1:1,80 DEG C of dryings to water content is 10% in baking oven, it then takes out mixed material and is placed in mold,
Hot-forming in vulcanizing press, 2 MPa of hot pressing pressure, 60 DEG C of hot pressing temperature, 20 min of hot pressing time is obtained formaldehydeless fire-retardant
Fiber type plate, bending strength 2.3MPa, elasticity modulus 400MPa, oxygen index (OI) >=30.
Embodiment 5
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprising the following steps:
(1) solid phase activation prepares dialdehyde starch: being 6% by wooden cornstarch drying to water content, then forms sediment with 0.3 corn
The sodium metaperiodate of silty amount, which is added in ball mill, carries out ball milling, and zirconium ball dosage is 2 times of cornstarch volume, is added in mechanical milling process
Add the magnesium phosphate of 10% cornstarch quality, the temperature of ball milling is 50 DEG C, and revolving speed is 500 r/min, and the time is 25 min, ball milling
Dialdehyde starch is obtained after the completion；
(2) it prepares dialdehyde starch adhesive: dialdehyde starch being dissolved in the water of 2 times of dialdehyde starch quality, hydroxide is added dropwise
It is 8 that sodium solution, which adjusts pH value, and the urea 5 of 0.05 times of dialdehyde starch quality is added, and stirs 30 under 75 DEG C, the revolving speed of 300 rpm
Min carries out addition reaction, and it is 4 that hydrochloric acid solution, which is then added dropwise, and adjusts pH value, adds the urea three of 0.05 times of dialdehyde starch quality
Poly cyanamid stirs 10 min under 75 DEG C, the revolving speed of 300 rpm and carries out condensation reaction, obtains dialdehyde starch adhesive；
(3) formaldehydeless flame retardant type fiberboard is prepared: the quality by the wood powder of dialdehyde starch adhesive and 80 mesh according to 0.8:1
Than mixing, 60 DEG C of dryings to water content is 10% in baking oven, then takes out mixed material and is placed in mold, in vulcanizing press
In hot-forming, 6 MPa of hot pressing pressure, 150 DEG C of hot pressing temperature, 15 min of hot pressing time obtains formaldehydeless flame retardant type fiberboard,
Bending strength 6.8MPa, elasticity modulus 960MPa, oxygen index (OI) >=30.
Claims (10)
1. a kind of preparation method of formaldehydeless flame retardant type fiberboard, which comprises the following steps:
(1) solid phase activation prepares dialdehyde starch: by the sodium metaperiodate of starch and 0.1-1.0% starch quality be added ball mill in into
Row ball milling, ball milling zirconium ball dosage are 1-3 times of starch volume, and the magnesium salts of 0.1-10% starch quality, ball milling are added in mechanical milling process
Temperature be 20-80 DEG C, revolving speed is 200-600 r/min, and the time is 10-30 min, and dialdehyde starch is obtained after the completion of ball milling；
(2) it prepares dialdehyde starch adhesive: dialdehyde starch being dissolved in the water of 1-3 times of dialdehyde starch quality, sodium hydroxide is added dropwise
It is 8-10 that solution, which adjusts pH value, the glue auxiliary agent of 0.03-0.08 times of dialdehyde starch quality is added, in 70-90 DEG C, 200-500
10-30 min is stirred under the revolving speed of rpm and carries out addition reaction, and it is 4-6 that hydrochloric acid solution, which is then added dropwise, and adjusts pH value, is added
The glue auxiliary agent of 0.01-0.05 times of dialdehyde starch quality, under 70-90 DEG C, the revolving speed of 200-500 rpm stirring 5-20 min into
Row condensation reaction obtains dialdehyde starch adhesive；
(3) formaldehydeless flame retardant type fiberboard is prepared: by the fiber wastes of dialdehyde starch adhesive and 40-80 mesh according to 0.3-1:
1 mass ratio mixing, 50-80 DEG C of drying to water content is 10-15% in baking oven, then takes out mixed material and is placed in mold,
Hot-forming in vulcanizing press, hot pressing pressure 2-10 MPa, 60-180 DEG C of hot pressing temperature, hot pressing time 5-20 min is obtained
Formaldehydeless flame retardant type fiberboard.
2. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, which is characterized in that the starch exists
It the use of preceding drying to water content is 3-7%.
3. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 2, which is characterized in that the starch is
Any one of tapioca, potato starch, cornstarch.
4. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, which is characterized in that the periodic acid
Its additive amount of sodium is the 0.5% of starch quality.
5. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, which is characterized in that the magnesium salts its
Additive amount is the 0.25% of starch quality.
6. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 5, which is characterized in that the magnesium salts is
Any one of magnesium chloride, magnesium nitrate, magnesium sulfate, magnesium carbonate, magnesium phosphate.
7. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, which is characterized in that in step (2), institute
The dialdehyde starch and the glue auxiliary agent total mass ratio stated are 1:0.1.
8. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 7, which is characterized in that in step (2), institute
The glue auxiliary agent stated is any one of urea, phenol, melamine.
9. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, which is characterized in that in step (3), institute
The dialdehyde starch adhesive stated is mixed with fiber wastes according to the mass ratio of 0.75:1.
10. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 9, which is characterized in that the fiber
Waste is one or more kinds of compositions of wood powder, straw powder, bagasse, manioc waste, peanut shell.
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| CN110922550A (en) * | 2019-11-15 | 2020-03-27 | 长春工业大学 | Preparation method of melamine resin with low free formaldehyde content |
| CN111331701A (en) * | 2020-04-07 | 2020-06-26 | 香河众旺木业有限公司 | Wax-added routing plate and preparation method thereof |
| CN113337137A (en) * | 2021-05-24 | 2021-09-03 | 山东千森木业集团有限公司 | Formaldehyde-free flame-retardant plate and production method thereof |
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