CN112936484A - Preparation method of high-strength flame-retardant wood - Google Patents

Preparation method of high-strength flame-retardant wood Download PDF

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Publication number
CN112936484A
CN112936484A CN202110188407.1A CN202110188407A CN112936484A CN 112936484 A CN112936484 A CN 112936484A CN 202110188407 A CN202110188407 A CN 202110188407A CN 112936484 A CN112936484 A CN 112936484A
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wood
minutes
retardant
strength flame
reactor
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CN112936484B (en
Inventor
王文亮
苗晖
任肖肖
谢旻希
高逸飞
马玉军
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27KPROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K3/00Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/02Processes; Apparatus
    • B27K3/15Impregnating involving polymerisation including use of polymer-containing impregnating agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27DWORKING VENEER OR PLYWOOD
    • B27D3/00Veneer presses; Press plates; Plywood presses
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27KPROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K5/00Treating of wood not provided for in groups B27K1/00, B27K3/00
    • B27K5/001Heating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G8/00Condensation polymers of aldehydes or ketones with phenols only
    • C08G8/28Chemically modified polycondensates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27KPROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K2240/00Purpose of the treatment
    • B27K2240/30Fireproofing

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Forests & Forestry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)

Abstract

The invention discloses a preparation method of high-strength flame-retardant wood, which comprises the steps of adding wood slices into a reactor filled with water, and stirring; adding sodium hydroxide and formaldehyde solution into a reactor, and continuously stirring; heating the reactor, uniformly raising the internal temperature to 90 ℃ within 30-40 minutes, and keeping the temperature for 15 minutes; continuing heating to enable the internal temperature to rise to 145-175 ℃, preserving the temperature for 10-40 minutes, immediately cooling, and taking out the wood slices after the reaction is finished when the internal temperature drops to below 50 ℃; and (3) carrying out hot pressing on the wood sheets along the thickness direction under a hot press, and obtaining the high-strength flame-retardant wood after the hot pressing is finished. The invention combines the processes of mild cooking of the wood and in-situ phenolic polymerization in the wood, effectively improves the strength and the flame retardance of the wood, and has obvious significance for widening the application field of the wood.

Description

Preparation method of high-strength flame-retardant wood
Technical Field
The invention belongs to the field of biomass materials, and particularly relates to a preparation method of high-strength flame-retardant wood.
Background
The wood in China has various types and wide application fields, and particularly has obvious application value in the aspects of furniture and wood structural materials. However, the wood resources are mainly fast-growing forests at present, so that certain defects exist in the wood quality, such as low strength, poor flame retardance and the like. In view of the above situation, many researchers try to improve the properties of wood materials from different angles, such as improving the flame retardant property of wood through flame retardant modification treatment, and improving the strength of wood through processes such as hot pressing. However, the existing treatment process is complex, the treatment cost is high, and it is difficult to improve the strength and the flame retardant property of the wood at the same time.
Disclosure of Invention
The invention aims to provide a preparation method of high-strength flame-retardant wood, which aims to overcome the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-strength flame-retardant wood comprises the following steps:
the method comprises the following steps: adding the wood slices into a reactor filled with water, stirring and mixing until the wood slices are fully soaked;
step two: adding sodium hydroxide and formaldehyde solution into a reactor, and continuously stirring and mixing until the mixture is fully impregnated;
step three: heating the reactor, starting stirring, uniformly heating the reactor to 90 ℃ within 30-40 minutes, and keeping the temperature for 15 minutes;
step four: continuing heating to enable the internal temperature to rise to 145-175 ℃, preserving the temperature for 10-40 minutes, immediately performing water cooling and cooling, and taking out the wood slices after the reaction is finished when the internal temperature drops to below 50 ℃;
step five: and (3) carrying out hot pressing on the wood sheets along the thickness direction under a hot press, and obtaining the high-strength flame-retardant wood after the hot pressing is finished.
Further, the stirring time in the first step was 20 minutes.
Further, the thickness of the wood flakes in the step one is 1-15 mm, and the wood flakes are coniferous wood or broad-leaved wood.
Further, the mass ratio of the wood flakes to the water in the first step is 1: (1-3).
Further, the mass concentration of the formaldehyde solution in the second step is 37%.
Further, in step two, wood flakes: sodium hydroxide: the mass ratio of the formaldehyde solution is 1: (0.2-1): (0.2-0.5).
Further, in the fourth step, the water cooling rate is 15-25 ℃/min.
Further, in the fifth step, the hot pressing temperature is 130-150 ℃, the pressure is 1-5 MPa, and the time is 1-10 minutes.
Compared with the prior art, the invention has the following beneficial technical effects:
the preparation method of the high-strength flame-retardant wood provided by the invention realizes the dual properties of high strength and flame retardance of the wood through simple treatment, greatly improves the utilization value of the wood, and has the following specific advantages:
(1) the conventional wood cooking process is a process of bond breaking and dissolving out of lignin in wood; the conventional phenolic resin preparation process is a process of addition polycondensation reaction of phenolic substances and formaldehyde. Based on the above, the two processes are skillfully combined and generate synergistic effect through technical adjustment, the aim is to realize limited fracture and softening of lignin in the wood through mild alkaline cooking of the wood, simultaneously add formaldehyde, realize addition condensation of the formaldehyde and lignin phenolic substances softened in the wood in an in-situ polymerization mode, form lignin-based phenolic resin oligomers through in-situ reaction inside the wood, and then quickly polymerize the lignin-based phenolic resin oligomers inside the wood through hot pressing to form macromolecular reticular thermosetting resin, so that the strength of the wood is greatly improved, and meanwhile, the generated thermosetting phenolic resin endows the wood with flame retardant property.
(2) The preparation method of the high-strength flame-retardant wood provided by the invention has the advantages that the alkaline environment and the proper process parameters are provided, the one-step method is realized to skillfully combine the alkaline delignification and the lignin formaldehyde in-situ polymerization in the wood, the treatment process is simple, the cost is low, the innovation of the traditional process is realized, and a good foundation is laid for preparing the high-performance wood material.
Detailed Description
The invention is further described below.
A preparation method of high-strength flame-retardant wood comprises the following steps:
(1) adding wood flakes into a reactor filled with water, and stirring for 20 minutes, wherein the mass ratio of the wood flakes to the water is 1: (1-3); the thickness of the wood sheet is 1-15 mm, and the wood comprises coniferous wood and broadleaf wood.
(2) Sodium hydroxide and formaldehyde solution were added to the reactor and stirring was continued for 5 minutes. Wood sheet: sodium hydroxide: the mass ratio of the formaldehyde solution (mass concentration 37%) is 1: (0.2-1): (0.2-0.5).
(3) And (3) heating the reactor, uniformly raising the internal temperature to 90 ℃ within 30-40 minutes, and keeping the temperature for 15 minutes.
(4) And continuously heating to raise the internal temperature to 145-175 ℃, and preserving the temperature for 10-40 minutes. And immediately carrying out water cooling at a cooling rate of 15-25 ℃/min, and taking out the wood slices after the reaction is finished when the internal temperature is reduced to below 50 ℃.
(5) And (2) carrying out hot pressing on the wood sheets under a hot press along the thickness direction, wherein the hot pressing temperature is 130-150 ℃, the pressure is 1-5 MPa, and the time is as follows: and (5) 1-10 minutes, and obtaining the high-strength flame-retardant wood after hot pressing.
The present invention will be described in detail with reference to examples. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is illustrative of the embodiments and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1
Fast-growing poplar wood was sawn into wood chips with a thickness of 15mm, 20g of the wood chips were added to a reactor containing 60g of water and stirred for 20 minutes. Then, 20g of sodium hydroxide and 10g of a formaldehyde solution (37%) were added to the reactor, and after stirring for 5 minutes, heating was started, the internal temperature was uniformly raised to 90 ℃ for 40 minutes, and the temperature was maintained for 15 minutes. Then heating is continued to raise the internal temperature to 145 ℃, the temperature is maintained for 40 minutes, then the temperature is immediately reduced, when the internal temperature is reduced to below 50 ℃, the reaction is finished, and the wood slices are taken out. And (2) carrying out hot pressing on the wood sheets along the thickness direction under a hot press, wherein the hot pressing temperature is 130 ℃, the pressure is 5MPa, and the time is as follows: after hot pressing is finished for 1 minute, the high-strength flame-retardant wood is obtained, the mechanical strength is 561.2Mpa, and the flame-retardant performance reaches the B1 grade requirement.
Example 2
Fir wood was sawed into 1mm thick wood chips, 5g of the wood chips were added to a reactor containing 5g of water and stirred for 20 minutes. Then, 1g of sodium hydroxide and 1g of a formaldehyde solution (37%) were added to the reactor, and after stirring for 5 minutes, heating was started, the internal temperature was uniformly raised to 90 ℃ for 30 minutes, and the temperature was maintained for 15 minutes. Then heating continuously to raise the internal temperature to 175 ℃, preserving the temperature for 10 minutes, immediately cooling, when the internal temperature is lowered to below 50 ℃, finishing the reaction, and taking out the wood slices. And (2) carrying out hot pressing on the wood sheets along the thickness direction under a hot press, wherein the hot pressing temperature is 150 ℃, the pressure is 1MPa, and the time is as follows: and (3) after hot pressing is finished for 10 minutes, obtaining the high-strength flame-retardant wood, wherein the mechanical strength of the high-strength flame-retardant wood is 286.9Mpa, and the flame-retardant property of the high-strength flame-retardant wood reaches the B1 grade requirement.
Example 3
Larch wood was sawn into wood chips having a thickness of 8mm, 10g of the wood chips were added to a reactor containing 20g of water and stirred for 20 minutes. Then, 5g of sodium hydroxide and 4g of a formaldehyde solution (37%) were added to the reactor, and after stirring for 5 minutes, heating was started, and the internal temperature was uniformly raised to 90 ℃ for 35 minutes, and the temperature was maintained for 15 minutes. Then heating continuously to raise the internal temperature to 160 deg.C, after 25 min of heat-insulating, immediately cooling, when the internal temperature is reduced to below 50 deg.C, reaction is completed, and the wood sheet is taken out. And (2) carrying out hot pressing on the wood sheets along the thickness direction under a hot press, wherein the hot pressing temperature is 140 ℃, the pressure is 3MPa, and the time is as follows: and 5 minutes, after hot pressing is finished, the high-strength flame-retardant wood is obtained, the mechanical strength is 433Mpa, and the flame-retardant performance reaches the B1 level requirement.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.

Claims (8)

1. The preparation method of the high-strength flame-retardant wood is characterized by comprising the following steps:
the method comprises the following steps: adding the wood slices into a reactor filled with water, stirring and mixing until the wood slices are fully soaked;
step two: adding sodium hydroxide and formaldehyde solution into a reactor, and continuously stirring and mixing until the mixture is fully impregnated;
step three: heating the reactor, starting stirring, uniformly heating the reactor to 90 ℃ within 30-40 minutes, and keeping the temperature for 15 minutes;
step four: continuing heating to enable the internal temperature to rise to 145-175 ℃, preserving the temperature for 10-40 minutes, immediately performing water cooling and cooling, and taking out the wood slices after the reaction is finished when the internal temperature drops to below 50 ℃;
step five: and (3) carrying out hot pressing on the wood sheets along the thickness direction under a hot press, and obtaining the high-strength flame-retardant wood after the hot pressing is finished.
2. The method for preparing high-strength flame-retardant wood according to claim 1, wherein the stirring time in the first step is 20 minutes.
3. The method for preparing high-strength flame-retardant wood according to claim 1, wherein the thickness of the wood flakes in the first step is 1-15 mm, and the wood flakes are coniferous wood or broadleaf wood.
4. The method for preparing high-strength flame-retardant wood according to claim 1, wherein the mass ratio of the wood flakes to the water in the first step is 1: (1-3).
5. The method for preparing high-strength flame-retardant wood according to claim 1, wherein the mass concentration of the formaldehyde solution in the second step is 37%.
6. The method for preparing high-strength flame-retardant wood according to claim 5, wherein in the second step, the wood sheet: sodium hydroxide: the mass ratio of the formaldehyde solution is 1: (0.2-1): (0.2-0.5).
7. The preparation method of high-strength flame-retardant wood according to claim 1, wherein the water cooling rate in the fourth step is 15-25 ℃/min.
8. The preparation method of high-strength flame-retardant wood according to claim 1, wherein in the fifth step, the hot pressing temperature is 130-150 ℃, the pressure is 1-5 MPa, and the time is 1-10 minutes.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114536487A (en) * 2022-02-22 2022-05-27 陕西科技大学 Method for gluing plates without glue

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CN1252339A (en) * 1999-09-14 2000-05-10 山东省曹县祥福木业有限公司 Modified tung board treatment method
CN1333113A (en) * 2000-07-11 2002-01-30 江泽慧 Artifical forest soft wood surface compacting metho dand products thereof
CN104087219A (en) * 2014-06-09 2014-10-08 德华兔宝宝装饰新材股份有限公司 Preparation method of lignin-modified phenolic resin wood adhesive
CN110103298A (en) * 2019-04-12 2019-08-09 江山欧派门业股份有限公司 Recombinant material Component units and preparation method thereof and recombinant material
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CN1252339A (en) * 1999-09-14 2000-05-10 山东省曹县祥福木业有限公司 Modified tung board treatment method
CN1333113A (en) * 2000-07-11 2002-01-30 江泽慧 Artifical forest soft wood surface compacting metho dand products thereof
CN104087219A (en) * 2014-06-09 2014-10-08 德华兔宝宝装饰新材股份有限公司 Preparation method of lignin-modified phenolic resin wood adhesive
CN111491768A (en) * 2017-12-22 2020-08-04 斯道拉恩索公司 Modified wood product and method for producing said product
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114536487A (en) * 2022-02-22 2022-05-27 陕西科技大学 Method for gluing plates without glue

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