CN105694512A - Novel halogen-free flame-retardant straw powder board - Google Patents

Novel halogen-free flame-retardant straw powder board Download PDF

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Publication number
CN105694512A
CN105694512A CN201610210377.9A CN201610210377A CN105694512A CN 105694512 A CN105694512 A CN 105694512A CN 201610210377 A CN201610210377 A CN 201610210377A CN 105694512 A CN105694512 A CN 105694512A
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Prior art keywords
powder
straw
free flame
phenolic resin
novel halogen
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CN201610210377.9A
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Chinese (zh)
Inventor
余若冰
胡乐平
黄舰
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East China University of Science and Technology
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East China University of Science and Technology
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Priority to CN201610210377.9A priority Critical patent/CN105694512A/en
Publication of CN105694512A publication Critical patent/CN105694512A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00Compositions of lignin-containing materials
    • C08L97/02Lignocellulosic material, e.g. wood, straw or bagasse
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/04Condensation polymers of aldehydes or ketones with phenols only
    • C08L61/06Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/22Halogen free composition
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides a novel halogen-free flame-retardant straw powder board which comprises 100 parts of straw powder, 10-100 parts of phenolic resin, a right amount of curing agent and 0-30 parts of filler. The invention aims to provide a high-flame-retardancy low-heat-conductivity-coefficient novel halogen-free flame-retardant straw powder board and a preparation method thereof. The invention also provides a preparation method of the novel halogen-free flame-retardant straw powder board.

Description

A kind of novel halogen-free flame-retardant powder of straw plate
Technical field
The present invention relates to sheet material field, more particularly, to a kind of powder of straw plate and preparation method thereof。
Background technology
Current agricultural residues powder is atmosphere pollution when burning, and comprehensive development and utilization is faced with again that technology is immature, it is relatively larger to invest, effectiveness comparison is poor awkward situation。Phenolic resin itself has excellent anti-flammability characteristic, simultaneously not halogen-containing again, is therefore a kind of excellent environment-friendlyflame-retardant flame-retardant material。But phenolic resin causes that due to the feature of self structure its fragility is big, and people can improve its defect by all means, adding wood powder, bamboo powder, powder of straw etc. is all effective method, can reduce again the cost of phenolaldehyde moulding compound further simultaneously。
Application number be 201510094912.4 Chinese patent disclose a kind of straw fireproof warming plate and production method thereof, its fire protecting performance reaches by adding fireproof agent Borax。But this area is needed badly a kind of without adding fire retardant or fireproof agent can have the flame-retardant board of good fire resistance。
Summary of the invention
For problems of the prior art, the invention provides a kind of excellent flame retardancy and the low novel halogen-free flame-retardant powder of straw plate of heat conductivity and preparation method thereof。
The present invention utilizes the halogen-free flame retardant feature of phenolic resin, carrys out modified straw powder plate with phenolic resin, prepares the halogen-free flameproof plate of high comprehensive performance。Halogen-free flameproof powder of straw plate comprises phenolic resin, firming agent, powder of straw, glass fibre and filler。It is substantially composed as follows: powder of straw 100 parts, phenolic resin 10-100 part, and firming agent is appropriate, glass fibre 0-50 part, filler 0-30 part。Formed clamp plate on vulcanizing press。
The invention provides a kind of novel halogen-free flame-retardant powder of straw plate, including: powder of straw 100 parts, phenolic resin 10-100 part, firming agent is appropriate, filler 0-30 part。
According to the present invention, phenolic resin includes one or several in piperazine resin, Nitrogen-containing Phenolic Resins, phosphorus containing phenolic resin, nitrogenous phosphorus containing phenolic resin, boron bakelite resin, linear phenolic resin, thermosetting phenolic resin。
According to the present invention, filler includes one or several in Kaolin, kieselguhr, white carbon, montmorillonite, Pulvis Talci。
According to the present invention, firming agent includes hexamethylenetetramine, organic acid, mineral acid, epoxy resin。
According to the present invention, also include glass fibre 0-50 part。
According to the present invention, glass fibre is glass fabric。
The preparation method that present invention also offers a kind of novel halogen-free flame-retardant powder of straw plate described above, comprises the steps:
S10: treated powder of straw 100 parts is provided;
S20: adding phenolic resin 10-100 part in powder of straw, firming agent is appropriate, filler 0-30 part, and mix homogeneously obtains mixture;
S30: by mixture on vulcanizing press compressing, to obtain novel halogen-free flame-retardant powder of straw plate。
According to the present invention, step S10 execution is: dried by straw, cutting, then passes through pulverizer and pulverizes, obtains powder;Join after powder is screened in KH550 solution, stir, then filter, dry and grind, to obtain treated powder of straw。
According to the present invention, step 30 execution is: pours the mixture in mould, is put on vulcanizing press by the mould pouring mixture into, mixture applies pressure progressively temperature programming, obtains novel halogen-free flame-retardant powder of straw plate after molding。
According to the present invention, step 30 perform be: by impregnation mixture on glass fabric after, be solidified into prepreg, superposition prepreg to vulcanizing press, pressurization temperature programming, obtain novel halogen-free flame-retardant powder of straw plate after molding。
Be it is an advantage of the current invention that: the present invention joins in phenolic resin powder of straw, obtain the powder of straw plate of excellent flame retardancy。This had both taken full advantage of agricultural resource, improve the added value of straw, obtained the sheet material of a kind of high comprehensive performance simultaneously。
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of the present invention。
Detailed description of the invention
The following examples can make those skilled in the art more fully understand the present invention, but does not limit the present invention in any way。
The invention provides a kind of novel halogen-free flame-retardant powder of straw plate, including: powder of straw 100 parts, phenolic resin 10-100 part, firming agent is appropriate, filler 0-30 part。Present invention powder of straw filled phenolic resin prepares the bittern-free flame-proof material of high comprehensive performance, takes full advantage of the structure flame-retarding characteristic of phenolic resin, it is not necessary to add fire retardant or fireproof agent。The present invention had both made full use of resource, and preparation method is simple, and environmentally safe, is the flame-retardant board of a kind of high comprehensive performance。
Preferably, phenolic resin includes one or several in piperazine resin, Nitrogen-containing Phenolic Resins, phosphorus containing phenolic resin, nitrogenous phosphorus containing phenolic resin, boron bakelite resin, linear phenolic resin, thermosetting phenolic resin。
Preferably, filler includes one or several in Kaolin, kieselguhr, white carbon, montmorillonite, Pulvis Talci。
Preferably, firming agent includes hexamethylenetetramine, organic acid, mineral acid, epoxy resin。
Preferably, glass fibre 0-50 part is also included。This glass fibre is glass fabric。
With reference to Fig. 1, the preparation method that present invention also offers a kind of novel halogen-free flame-retardant powder of straw plate described above, comprise the steps:
S10: treated powder of straw 100 parts is provided;
S20: adding phenolic resin 10-100 part in powder of straw, firming agent is appropriate, filler 0-30 part, and mix homogeneously obtains mixture;
S30: by mixture on vulcanizing press compressing, to obtain novel halogen-free flame-retardant powder of straw plate。
In a preferred embodiment, step S10 execution is: dried by straw, cutting, then passes through pulverizer and pulverizes, obtains powder;Join after powder is screened in Silane coupling agent KH550 solution, stir, then filter, dry and grind, to obtain treated powder of straw。Specifically, straw is dried, cutting, then pass through pulverizer and pulverize, obtain powder of straw;Powder of straw is carried out the screening of order number, weighs a certain amount of KH550, add deionized water, be made into the solution for later use of certain solubility。Powder of straw being joined in KH550 solution, stirs, then filter, the powder of straw filtered out is put and is dried in an oven。The powder of straw of KH550 surface treatment can be obtained。Powder of straw after drying is worn into powder body, stand-by。
In a preferred embodiment, step 30 execution is: pours the mixture in mould, is put on vulcanizing press by the mould pouring mixture into, mixture applies pressure progressively temperature programming, obtains novel halogen-free flame-retardant powder of straw plate after molding。
Specifically, liquid phenolic resin or Phenolic resin powder, firming agent, filler and powder of straw mix homogeneously, pour in mould, evacuation, deaeration, the mould pouring mixture into is put on vulcanizing press, mixture is applied pressure progressively temperature programming: room temperature → 50 DEG C → 70 DEG C → 90 DEG C → 110 DEG C are (namely, it is raised to 50 from room temperature to be raised again to 70 DEG C and be raised again to 90 DEG C and be raised again to 110 DEG C), it is then turned off vacuum, continue temperature programming: 130 DEG C/30min → 150 DEG C/30min → 180 DEG C/30min (namely maintain 30min at 130 DEG C, it is raised again to 150 DEG C and maintains 30min, by that analogy)。After molding, naturally cool to room temperature, the demoulding, obtain phenolic resin plate。
In another preferred embodiment, step 30 perform be: by impregnation mixture on glass fabric after, be solidified into prepreg, superposition prepreg to vulcanizing press, pressurization and temperature programming, obtain novel halogen-free flame-retardant powder of straw plate after molding。
Specifically, first formulated phenolic resin solution, adds firming agent, filler and powder of straw, mix homogeneously in the solution, forms dipping solution;By glass fabric impregnation, dry the glass fabric of leaching phenol resin solution, make prepreg, then prepreg is stacked up, be placed in 160 DEG C of vulcanizing presses, slowly pressurization, controlling gummosis degree, go directly maximum pressure, is then warmed up to 180-200 DEG C in 10min, suppress 40min-2 hour, after molding, obtain novel halogen-free flame-retardant powder of straw plate。
It is below that it is intended to example and is not limiting for openly sufficient purpose, the multiple embodiments listed。
Embodiment one:
Take 70g linear phenolic resin, 30g Nitrogen-containing Phenolic Resins, 10g hexamethylenetetramine, put in pulverizer and pulverize, obtain powder body material, be subsequently poured in mould;The temperature of vulcanizing press is set in 160 DEG C, the mould loading onto material is put on vulcanizing press, just start not apply pressure, Deng one or two minute after-applied only small pressure, at about 1MPa, there is a small amount of gummosis, by the time after gel, rapidly pressure is made, 160 DEG C are incubated 30min, continuous temperature programming: 180 DEG C/30min。After molding, naturally cool to room temperature, the demoulding, obtain phenolic resin plate。
Embodiment two:
100 parts of powder of straw after process, 70g linear phenolic resin, 30g Nitrogen-containing Phenolic Resins, 10g hexamethylenetetramine, put in pulverizer and pulverize, obtain powder body material, be subsequently poured in mould;The temperature of vulcanizing press is set in 160 DEG C, the mould loading onto material is put on vulcanizing press, just start not apply pressure, Deng one or two minute after-applied only small pressure, at about 1MPa, there is a small amount of gummosis, by the time after gel, rapidly pressure is made, 160 DEG C are incubated 30min, continuous temperature programming: 180 DEG C/30min。
Example three:
Take 150 parts of powder of straw after process, 70g linear phenolic resin, the nitrogenous phosphorus containing phenolic resin of 30g, 10g hexamethylenetetramine, put in pulverizer and pulverize, obtain powder body material, be subsequently poured in mould;The temperature of vulcanizing press is set in 160 DEG C, the mould loading onto material is put on vulcanizing press, just start not apply pressure, Deng one or two minute after-applied only small pressure, at about 1MPa, there is a small amount of gummosis, by the time after gel, rapidly pressure is made, 160 DEG C are incubated 30min, continuous temperature programming: 180 DEG C/30min。After molding, naturally cool to room temperature, the demoulding, obtain phenolic resin plate。
Example four:
Take 10g hexamethylenetetramine and join mix homogeneously in 100g liquid piperazine resin, add part powder of straw after 400 parts of process, mixture is uniform, then pour the mixture in mould, evacuation, deaeration, progressively temperature programming: room temperature → 50 DEG C → 70 DEG C → 90 DEG C → 110 DEG C, it is then turned off vacuum, continues temperature programming;130 DEG C/30min → 150 DEG C/30min → 170 DEG C/30min → 200 DEG C/60min。After molding, naturally cool to room temperature, the demoulding, obtain the phenolic resin plate that powder of straw is filled。
Example five:
90g linear phenolic resin and 10g Nitrogen-containing Phenolic Resins are dissolved in alcoholic solution, are subsequently adding 10g hexamethylene tetramine, stir, namely obtain the glue of impregnation;Glass fabric is impregnated glue, then dries in the air 24 hours, send in baking oven and bake prepreg;The temperature of vulcanizing press is set in 160 DEG C, by prepreg superposition from level to level, puts in vulcanizing press;Just start not apply pressure, waited one or two minute after-applied only small pressure, at about 1MPa, have a small amount of gummosis, after waiting until gel, rapidly pressure has been made, 160 DEG C have been incubated 30min, continuous temperature programming: 180 DEG C/60min → 200 DEG C/60min。After molding, naturally cool to room temperature, the demoulding, obtain the phenolic resin plate of glass fiber reinforcement。
Example six:
90g linear phenolic resin and 10g Nitrogen-containing Phenolic Resins are dissolved in alcoholic solution, are subsequently adding 10g hexamethylene tetramine, stir, adding 100g powder of straw, stir, namely obtain the glue of impregnation;Glass fabric is impregnated glue, then dries in the air 24 hours, send in baking oven and bake prepreg;The temperature of vulcanizing press is set in 160 DEG C, by prepreg superposition from level to level, puts in vulcanizing press;Just start not apply pressure, waited one or two minute after-applied only small pressure, at about 1MPa, have a small amount of gummosis, after waiting until gel, rapidly pressure has been made, 160 DEG C have been incubated 30min, continuous temperature programming: 180 DEG C/60min → 200 DEG C/60min。After molding, naturally cool to room temperature, the demoulding, obtain the phenolic resin plate that the powder of straw of glass fiber reinforcement is filled。
Following table is the contrast of the fire resistance of each example and heat conductivility, and the data from table can obtain, and the fire resistance and the heat conductivility that add the sheet material of powder of straw and glass fibre are more superior comparatively speaking。
It will be understood by those skilled in the art that above example is only exemplary embodiment, when without departing substantially from the spirit and scope of the present invention, it is possible to carry out multiple change, replacement and change。

Claims (10)

1. a novel halogen-free flame-retardant powder of straw plate, it is characterised in that including:
Powder of straw 100 parts, phenolic resin 10-100 part, firming agent is appropriate, filler 0-30 part。
2. novel halogen-free flame-retardant powder of straw plate according to claim 1, it is characterized in that, described phenolic resin includes one or several in piperazine resin, Nitrogen-containing Phenolic Resins, phosphorus containing phenolic resin, nitrogenous phosphorus containing phenolic resin, boron bakelite resin, linear phenolic resin, thermosetting phenolic resin。
3. novel halogen-free flame-retardant powder of straw plate according to claim 1, it is characterised in that filler includes one or several in Kaolin, kieselguhr, white carbon, montmorillonite, Pulvis Talci。
4. novel halogen-free flame-retardant powder of straw plate according to claim 1, it is characterised in that described firming agent includes hexamethylenetetramine, organic acid, mineral acid, epoxy resin。
5. novel halogen-free flame-retardant powder of straw plate according to claim 1, it is characterised in that also include glass fibre 0-50 part。
6. novel halogen-free flame-retardant powder of straw plate according to claim 5, it is characterised in that described glass fibre is glass fabric。
7. the preparation method of the novel halogen-free flame-retardant powder of straw plate as described in any one in claim 1-6, it is characterised in that comprise the steps:
S10: treated powder of straw 100 parts is provided;
S20: adding phenolic resin 10-100 part in described powder of straw, firming agent is appropriate, filler 0-30 part, and mix homogeneously obtains mixture;
S30: by described mixture on vulcanizing press compressing, to obtain described novel halogen-free flame-retardant powder of straw plate。
8. preparation method according to claim 7, it is characterised in that described step S10 execution is:
Straw is dried, cutting, then pass through pulverizer and pulverize, obtain powder;
Join after described powder is screened in KH550 solution, stir, then filter, dry and grind, to obtain described treated powder of straw。
9. preparation method according to claim 7, it is characterized in that, described step 30 performs: pour in mould by described mixture, the described mould pouring described mixture into is put on described vulcanizing press, described mixture is applied pressure progressively temperature programming, after molding, obtains described novel halogen-free flame-retardant powder of straw plate。
10. preparation method according to claim 7, it is characterized in that, described step 30 perform be: by described impregnation mixture on glass fabric after, it is solidified into prepreg, prepreg described in superposition is to described vulcanizing press, pressurization temperature programming, obtain described novel halogen-free flame-retardant powder of straw plate after molding。
CN201610210377.9A 2016-04-06 2016-04-06 Novel halogen-free flame-retardant straw powder board Pending CN105694512A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106000368A (en) * 2016-06-27 2016-10-12 余若冰 Oil absorption material
CN106220034A (en) * 2016-07-06 2016-12-14 何维 A kind of preparation method of insulation multi-function decoration board
CN106700584A (en) * 2016-11-22 2017-05-24 湖北硅金凝节能减排科技有限公司 Aerogel density board and preparation method thereof
CN107323059A (en) * 2017-06-08 2017-11-07 合肥同创园林科技有限公司 A kind of method that garden waste produces sheeting caps

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101934679A (en) * 2010-07-16 2011-01-05 黄玉强 Non-combustible straw decorating plate and manufacturing method thereof
CN103602090A (en) * 2013-11-07 2014-02-26 任慧 Straw and thermosetting resin compound and preparation method thereof
CN104563806A (en) * 2013-10-28 2015-04-29 天津浦安防火科技有限公司 Method for manufacturing straw environment-friendly fireproof door core plate
CN104910582A (en) * 2015-06-16 2015-09-16 陕西理工学院 Preparation method of modified-straw-powder-added phenolic resin composite board

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101934679A (en) * 2010-07-16 2011-01-05 黄玉强 Non-combustible straw decorating plate and manufacturing method thereof
CN104563806A (en) * 2013-10-28 2015-04-29 天津浦安防火科技有限公司 Method for manufacturing straw environment-friendly fireproof door core plate
CN103602090A (en) * 2013-11-07 2014-02-26 任慧 Straw and thermosetting resin compound and preparation method thereof
CN104910582A (en) * 2015-06-16 2015-09-16 陕西理工学院 Preparation method of modified-straw-powder-added phenolic resin composite board

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106000368A (en) * 2016-06-27 2016-10-12 余若冰 Oil absorption material
CN106220034A (en) * 2016-07-06 2016-12-14 何维 A kind of preparation method of insulation multi-function decoration board
CN106700584A (en) * 2016-11-22 2017-05-24 湖北硅金凝节能减排科技有限公司 Aerogel density board and preparation method thereof
CN107323059A (en) * 2017-06-08 2017-11-07 合肥同创园林科技有限公司 A kind of method that garden waste produces sheeting caps

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