CN107586461A - 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 ball mill and prepares dialdehyde starch, then it is mixed with dialdehyde starch adhesive 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 cost of preparation is low, good dispersion, viscosity is low, adhesive strength is big, the formaldehydeless release of fiberboard of preparation, safety and environmental protection, there is good fire resistance simultaneously.
Description
Technical field
It is specifically a kind of formaldehydeless fire-retardant the present invention relates to starch and fiber wastes application technology as the second resource field
The preparation method of fiber type plate.
Background technology
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 while extensive use there is also it is notable the shortcomings that, that is, caused by Form aldehyde release being present
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, with raising of the modern architecture to fire protection requirement, it is fire-retardant
The market demand of type wood-based plate is increasing.
Starch-based glue stick is an important development direction of adhesive " Green Chemistry ".As natural adhesive, starch
Glue has long applicating history.There is raw material to be easy to get, be cheap, be corrosion-free, be pollution-free for it, 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, there is low gelatinization point, transparent, permeability and anti -precipitability is good, easy film forming, adhesive property are good, can strengthen 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
Preparation of the scholar to dialdehyde starch is inquired into, but the dialdehyde starch still generally existing prepared using traditional water phase method
The shortcomings such as periodate dosage is too high, expensive, contaminated wastewater is serious, dialdehyde content is low, and use this dialdehyde content low
Starch prepare 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 added in deionized water and mixed, and then add starch stirring and match somebody with somebody
Into starch milk, it is scrubbed that obtained starch milk is transferred to progress acid hydrolysis oxidative reaction, the material obtained after having reacted in reactor
Re-dry after to neutrality, the dialdehyde starch is produced, oxidant is sodium metaperiodate or periodic acid, and acidolysis agent is 36.5wt% salt
One or both of sulfuric acid of acid or 98wt%, starch are cornstarch, farina or rice starch, oxidant 150-
257 parts, acidolysis agent 10-300 parts, 162 parts of starch, deionized water 648-3888 parts, i.e. sodium metaperiodate or periodic acid dosage are shallow lake
The 92.6-159% of powder dosage, it is with high costs, and can produce substantial amounts of acid waste water during material washing.
Adhesive used in fiberboard requirement must be good dispersion, viscosity is low, solid content is high, adhesive strength is big, also simultaneously
Cost is low prepared by it is required that, and this is relatively difficult to achieve for general starch adhesive, and there has been no industrialized starch is gluing at present
Agent production.In summary, develop that a kind of production cost is low, technique is simple, glue intensity is big, solid content is high, viscosity is low, environmentally friendly
Safe and pollution-free starch adhesive prepares fiberboard, can replace the serious plate containing formaldehyde fibers of potential safety hazard, have simultaneously
There are the good market competitiveness and economic benefit.
The content of the invention
The purpose of the present invention is to overcome the potential safety hazard of the existing plate containing formaldehyde fibers, while solves starch adhesive cost
A kind of the defects of height, poor performance, there is provided preparation method of formaldehydeless flame retardant type fiberboard.
The solution of the present invention is by being achieved in that：
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprises the following steps：
（1）Solid phase activation prepares dialdehyde starch：The sodium metaperiodate of starch and 0.1-1.0% starch qualities is added in ball mill
Row ball milling, zirconium ball dosage are 1-3 times of starch volume, and the magnesium salts of 0.1-10% starch qualities, the temperature of ball milling are added in mechanical milling process
Spend for 20-80 DEG C, rotating 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）Prepare dialdehyde starch adhesive：Dialdehyde starch is dissolved in the water of 1-3 times of dialdehyde starch quality, sodium hydroxide is added dropwise
Solution regulation 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, 200-500
10-30 min are stirred under rpm rotating speed and carry out addition reaction, it is 4-6 that hydrochloric acid solution regulation pH value, which is then added dropwise, is added
The glue auxiliary agent of 0.01-0.05 times of dialdehyde starch quality, stirring 5-20 min enter under 70-90 DEG C, 200-500 rpm rotating speed
Row condensation reaction, obtain dialdehyde starch adhesive；
（3）Prepare formaldehydeless flame retardant type fiberboard：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 mould,
It is 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, obtain
Formaldehydeless flame retardant type fiberboard.
Preferably, it is 3-7% that described starch, which is dried before use to water content,.
Preferably, described starch is any of tapioca, farina, cornstarch.
Preferably, its addition of described sodium metaperiodate is the 0.5% of starch quality.
Preferably, its addition of described magnesium salts is the 0.25% of starch quality.
Preferably, described magnesium salts is any of magnesium chloride, magnesium nitrate, magnesium sulfate, magnesium carbonate, magnesium phosphate.
Preferably, step（2）In, described dialdehyde starch is 1 with described glue auxiliary agent total mass ratio:0.1.
Preferably, step（2）In, described glue auxiliary agent is any of urea, phenol, melamine.
Preferably, step（3）In, described dialdehyde starch adhesive is with fiber wastes according to 0.75:1 mass ratio mixes
Close.
Preferably, described fiber wastes are wood powder, powder of straw, bagasse, manioc waste, one kind or one kind of peanut shell
Composition above.
Under above optimum condition, formaldehydeless flame retardant type fiberboard bending strength prepared by the present invention is curved up to 14 MPa
The MPa of modulus in elasticity in bending 1400, oxygen index (OI) >=30, fire resistance reach GB8624-2006《Construction material and product burns performance
Classification》B levels standard and GB/T8625-2005《Test method of difficultflammability for building materials》The requirement of flame retardant material.
The technical principle that the present invention realizes is：First, reacted using synchronization mechanism active oxidation, i.e. starch, sodium metaperiodate
Solid phase blending enters mechanical activation device and carries out solid phase reaction, and mechanical activation is the effect by mechanical force, starch is produced in itself
Raw lattice defect, crystalline texture are destroyed, and starch molecular chain shortens, and reaction compartment obstacle reduces, and makes sodium metaperiodate be more easy to enter
Inside starch molecule, while some mechanical can be converted into the interior energy of molecule, and substrate reactions activation energy is reduced, and sodium metaperiodate is easier
By starch oxidation, so as to the dialdehyde content for improving chemical reaction rate, shortening the reaction time, increasing starch；Secondly, magnesium salts adds
Add, fused salt effect can be produced, promote the destruction of crystalline structure of starch in mechanical activation process, contribute to the oxidation of periodate to make
With so as in the case where periodate dosage is less, obtain the dialdehyde starch of higher aldehyde group content, the dialdehyde starch viscosity
It is low, soluble in water, it can be configured to solids content 40-50% starch adhesive；Again, under mechanical activation effect magnesium salts can be made micro-
Refinement, the inorganic salts material with certain whisker function is formed, so as to produce obvious anti-flammability when prepared by fiberboard.
The present invention possesses following good result：
（1）The present invention prepares dialdehyde starch using Solid Phase Simultaneous mechanical activation oxidation reaction, and sodium metaperiodate dosage is few, oxidation reaction
Efficiency high, the aldehyde radical of dialdehyde starch are up to 1.15-2.45, and solubility is up to 40-50 g/100g water.
（2）The dialdehyde starch viscosity of the present invention is low, soluble in water, is very beneficial to prepare starch adhesive.
（3）The present invention ureaformaldehyde starch adhesive cost is low, good dispersion, viscosity are low, high reachable the 40-50% of solid content, glues
It is big to connect intensity.
（4）The formaldehydeless release of fiberboard of the present invention, safety and environmental protection, while there is good fire resistance.
（5）The fiberboard good mechanical properties of the present invention, bending strength 2-14MPa, modulus of elasticity 400-1400MPa, oxygen
Index >=30, fire resistance reach GB8624-2006《Construction material and product burns grading performance》B levels standard and GB/
T8625-2005《Test method of difficultflammability for building materials》The requirement of flame retardant material, it is adapted to building board intensity and fire protecting performance
Demand.
（6）The present invention uses low cost starch and fiber wastes, and for raw material, production cost is low, and technique is simple, and no waste water gives up
Gas produces, and is very suitable for industrialized production.
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 that present invention is further limited.
Embodiment 1
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprises the following steps：
（1）Solid phase activation prepares dialdehyde starch：By tapioca drying to water content be 5%, then with 0.5% tapioca quality
Sodium metaperiodate add in ball mill and carry out ball milling, 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 rotating speed is 300 r/min, and the time is 30 min, ball milling
After the completion of obtain dialdehyde starch；
（2）Prepare dialdehyde starch adhesive：Dialdehyde starch is dissolved in the water of 1.5 times of dialdehyde starch quality, sodium hydroxide is added dropwise
Solution regulation pH value is 8.5, adds the urea of 0.07 times of dialdehyde starch quality, 25 are stirred under 85 DEG C, 400 rpm rotating speed
Min carries out addition reaction, and it is 5.0 that hydrochloric acid solution regulation pH value, which is then added dropwise, adds the urea of 0.03 times of dialdehyde starch quality,
20 min are stirred under 85 DEG C, 400 rpm rotating speed 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 60 mesh, bagasse, manioc waste according to
0.75:1 mass ratio mixing, 60 DEG C of dryings to water content is 12% in baking oven, then takes out mixed material and is placed in mould,
It is hot-forming in vulcanizing press, the MPa of hot pressing pressure 6,140 DEG C of hot pressing temperature, the min of hot pressing time 10, obtain formaldehydeless resistance
Fire fiber type plate, its bending strength 14.2MPa, modulus of elasticity 14000MPa, oxygen index (OI) >=30.
Embodiment 2
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprises the following steps：
（1）Solid phase activation prepares dialdehyde starch：By cornstarch drying to water content be 7%, then with 1.0% cornstarch quality
Sodium metaperiodate add in ball mill and carry out ball milling, zirconium ball dosage is 1 times of cornstarch volume, and it is beautiful that 1% is added in mechanical milling process
The magnesium chloride of rice starch quality, the temperature of ball milling is 60 DEG C, and rotating speed is 600 r/min, and the time is 10 min, is obtained after the completion of ball milling
To dialdehyde starch；
（2）Prepare dialdehyde starch adhesive：Dialdehyde starch is dissolved in the water of 1 times of dialdehyde starch quality, it is molten that sodium hydroxide is added dropwise
Liquid regulation pH value is 9.5, adds the urea of 0.08 times of dialdehyde starch quality, 20 min are stirred under 70 DEG C, 500 rpm rotating speed
Addition reaction is carried out, it is 4 that hydrochloric acid solution regulation pH value, which is then added dropwise, the urea of 0.05 times of dialdehyde starch quality is added, 70
DEG C, stir 5 min under 500 rpm rotating speed 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, powder of straw, bagasse, cassava
Slag, peanut shell are according to 0.5:1 mass ratio mixing, 80 DEG C of dryings to water content is 10% in baking oven, then takes out mixed material
It is placed in mould, hot-forming in vulcanizing press, the MPa of hot pressing pressure 10,120 DEG C of hot pressing temperature, hot pressing time 10
Min, obtains formaldehydeless flame retardant type fiberboard, its bending strength 12.5MPa, modulus of elasticity 1230MPa, oxygen index (OI) >=30.
Embodiment 3
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprises the following steps：
（1）Solid phase activation prepares dialdehyde starch：By farina drying to water content be 3%, then with 0.5% farina
The sodium metaperiodate of quality, which is added in ball mill, carries out ball milling, and zirconium ball dosage is 3 times of farina volume, is added in mechanical milling process
Add the magnesium nitrate of 3% farina quality, the temperature of ball milling is 60 DEG C, and rotating speed is 300 r/min, and the time is 20 min, ball milling
After the completion of obtain dialdehyde starch；
（2）Prepare dialdehyde starch adhesive：Dialdehyde starch is dissolved in the water of 2 times of dialdehyde starch quality, it is molten that sodium hydroxide is added dropwise
Liquid regulation pH value is 10, adds the phenol of 0.03 times of dialdehyde starch quality, 30 min are stirred under 80 DEG C, 300 rpm rotating speed
Addition reaction is carried out, it is 4 that hydrochloric acid solution regulation pH value, which is then added dropwise, the phenol of 0.02 times of dialdehyde starch quality is added, 80
DEG C, stir 5 min under 300 rpm rotating speed and carry out condensation reaction, obtain dialdehyde starch adhesive；
（3）Prepare formaldehydeless flame retardant type fiberboard：The powder of straw of dialdehyde starch adhesive and 80 mesh, bagasse, peanut shell are pressed
According to 0.3:1 mass ratio mixing, 50 DEG C of dryings to water content is 15% in baking oven, then takes out mixed material and is placed in mould,
It is hot-forming in vulcanizing press, the MPa of hot pressing pressure 4,90 DEG C of hot pressing temperature, the min of hot pressing time 15, obtain formaldehydeless fire-retardant
Fiber type plate, its bending strength 8.4MPa, modulus of elasticity 1020MPa, oxygen index (OI) >=30.
Embodiment 4
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprises the following steps：
（1）Solid phase activation prepares dialdehyde starch：By tapioca drying to water content be 7%, then with 0.1% tapioca quality
Sodium metaperiodate add in ball mill and carry out ball milling, zirconium ball dosage is 3 times of tapioca volume, and 10% is added in mechanical milling process
The magnesium carbonate of tapioca starch quality, the temperature of ball milling is 20 DEG C, and rotating speed is 600 r/min, and the time is 10 min, and ball milling is complete
Dialdehyde starch is obtained after；
（2）Prepare dialdehyde starch adhesive：Dialdehyde starch is dissolved in the water of 3 times of dialdehyde starch quality, it is molten that sodium hydroxide is added dropwise
Liquid regulation pH value is 8, adds the melamine of 0.08 times of dialdehyde starch quality, 10 are stirred under 90 DEG C, 200 rpm rotating speed
Min carries out addition reaction, and it is 6 that hydrochloric acid solution regulation pH value, which is then added dropwise, adds the melamine of 0.01 times of dialdehyde starch quality
Amine, 10 min are stirred under 90 DEG C, 200 rpm rotating speed 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, powder of straw, bagasse according to
1:1 mass ratio mixing, 80 DEG C of dryings to water content is 10% in baking oven, then takes out mixed material and is placed in mould, flat
It is hot-forming in plate vulcanizer, the MPa of hot pressing pressure 2,60 DEG C of hot pressing temperature, the min of hot pressing time 20, it is fine to obtain formaldehydeless flame retardant type
Tie up plate, its bending strength 2.3MPa, modulus of elasticity 400MPa, oxygen index (OI) >=30.
Embodiment 5
A kind of preparation method of formaldehydeless flame retardant type fiberboard, comprises the following steps：
（1）Solid phase activation prepares dialdehyde starch：By wooden cornstarch drying to water content be 6%, then with 0.3 cornstarch matter
The sodium metaperiodate of 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
The magnesium phosphate of 10% cornstarch quality, the temperature of ball milling is 50 DEG C, and rotating speed is 500 r/min, and the time is 25 min, and ball milling is complete
Dialdehyde starch is obtained after；
（2）Prepare dialdehyde starch adhesive：Dialdehyde starch is dissolved in the water of 2 times of dialdehyde starch quality, it is molten that sodium hydroxide is added dropwise
Liquid regulation pH value is 8, adds the urea 5 of 0.05 times of dialdehyde starch quality, 30 min are stirred under 75 DEG C, 300 rpm rotating speed
Addition reaction is carried out, it is 4 that hydrochloric acid solution regulation pH value, which is then added dropwise, adds the urea melamine of 0.05 times of dialdehyde starch quality
Amine, 10 min are stirred under 75 DEG C, 300 rpm rotating speed 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 80 mesh according to 0.8:1 mass ratio mixes
Close, 60 DEG C of dryings to water content is 10% in baking oven, then takes out mixed material and is placed in mould, hot in vulcanizing press
It is molded, the MPa of hot pressing pressure 6,150 DEG C of hot pressing temperature, the min of hot pressing time 15, formaldehydeless flame retardant type fiberboard is obtained, it bends
Intensity 6.8MPa, modulus of elasticity 960MPa, oxygen index (OI) >=30.
Claims (10)
1. a kind of preparation method of formaldehydeless flame retardant type fiberboard, it is characterised in that comprise the following steps：
（1）Solid phase activation prepares dialdehyde starch：The sodium metaperiodate of starch and 0.1-1.0% starch qualities is added in ball mill
Row ball milling, zirconium ball dosage are 1-3 times of starch volume, and the magnesium salts of 0.1-10% starch qualities, the temperature of ball milling are added in mechanical milling process
Spend for 20-80 DEG C, rotating 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）Prepare dialdehyde starch adhesive：Dialdehyde starch is dissolved in the water of 1-3 times of dialdehyde starch quality, sodium hydroxide is added dropwise
Solution regulation 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, 200-500
10-30 min are stirred under rpm rotating speed and carry out addition reaction, it is 4-6 that hydrochloric acid solution regulation pH value, which is then added dropwise, is added
The glue auxiliary agent of 0.01-0.05 times of dialdehyde starch quality, stirring 5-20 min enter under 70-90 DEG C, 200-500 rpm rotating speed
Row condensation reaction, obtain dialdehyde starch adhesive；
（3）Prepare formaldehydeless flame retardant type fiberboard：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 mould,
It is 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, obtain
Formaldehydeless flame retardant type fiberboard.
2. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, it is characterised in that described starch exists
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, it is characterised in that described starch is
Any of tapioca, farina, cornstarch.
4. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, it is characterised in that described periodic acid
Its addition of sodium is the 0.5% of starch quality.
5. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, it is characterised in that described magnesium salts its
Addition is the 0.25% of starch quality.
6. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 5, it is characterised in that described magnesium salts is
Any 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, it is characterised in that step（2）In, institute
The dialdehyde starch stated is 1 with described glue auxiliary agent total mass ratio:0.1.
8. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 7, it is characterised in that step（2）In, institute
The glue auxiliary agent stated is any of urea, phenol, melamine.
9. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 1, it is characterised in that step（3）In, institute
The dialdehyde starch adhesive stated is with fiber wastes according to 0.75:1 mass ratio mixing.
10. the preparation method of formaldehydeless flame retardant type fiberboard according to claim 9, it is characterised in that described fiber
Discarded object is wood powder, powder of straw, bagasse, manioc waste, one or more kinds of compositions of 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 |
| FR3102184A1 (en) * | 2019-10-22 | 2021-04-23 | Centre National De La Recherche Scientifique | Bio-based adhesive compositions |
| 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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| CN107586461B (en) | 2019-06-18 |
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