CN102558468A - Bamboo/wood tar-furfural thermosetting resin and preparation method thereof - Google Patents
Bamboo/wood tar-furfural thermosetting resin and preparation method thereof Download PDFInfo
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- CN102558468A CN102558468A CN2011104511318A CN201110451131A CN102558468A CN 102558468 A CN102558468 A CN 102558468A CN 2011104511318 A CN2011104511318 A CN 2011104511318A CN 201110451131 A CN201110451131 A CN 201110451131A CN 102558468 A CN102558468 A CN 102558468A
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Abstract
The invention provides bamboo/wood tar-furfural thermosetting resin, which is prepared by the following method: adding tar/wood tar and furfural to a reactor at a mass ratio of tar to furfural being 1:(1.0-1.2), uniformly stirring, and pre-heating to 68-72 DEG C; adding a basic catalyst to pH being 8-11, and reacting at 85-110 DEG C for 2-5h, wherein the amount of the basic catalyst is 7-9% the mass of the bamboo/wood tar; and naturally cooling the reaction liquid, and dewatering under reduced pressure to obtain the bamboo/wood tar-furfural thermosetting resin. According to the invention, bamboo/wood processing byproduct namely bamboo/wood tar is used for completely replacing phenol to synthesize the thermosetting resin together with furfural, not only are the problems of high raw material toxicity, environmental pollution and the like in the traditional phenolic resin preparing process solved, but also the bamboo/wood charcoal byproduct namely bamboo/wood tar is changed into valuables, and the resources are sufficiently utilized. Therefore, the preparation method is a green and environment-friendly new way for preparing phenolic resin.
Description
(1) technical field
The present invention relates to a kind of bamboo/wood tar oil-furfural thermosetting resin and preparation method thereof.
(2) background technology
Resol is the resin that is formed by phenols and aldehyde compound polycondensation; Wherein with phenol and formaldehyde condensation polymer and resol the most important; It has advantages such as cheap, heat-resisting, corrosion-resistant, fire-retardant, that burning fuming is few, is widely used as moulding compound, sizing agent, coating etc.But its shortcoming is a synthesis material phenol is prototype matter poisonous substance, and toxicity is big, and it can make protein degradation, and people's nerve, liver, kidney are suffered damage; Raw material formaldehyde has the carcinogenic and short cancer effect of intensive, can cause pulmonary function, liver function and immunologic dysfunction etc., and healthy and environment are all had harm.Therefore, the raw material of seeking environmental protection substitutes phenol and formaldehyde is very necessary.
Bamboo/wood tar oil is the main by product in bamboo/charcoal production process, at present to the development and use of bamboo/wood tar oil also seldom, many times as waste treatment, causes the wasting of resources.Containing in bamboo/wood tar oil with the phenols is nearly hundred kinds of main organic cpds, and these phenolic cpds have a lot of adjacency pairs position not have substituting group (like 4-ethylphenol, 2,6-syringol etc.), all might with aldehydes generation crosslinking reaction; Furfural has active aldehyde radical, can be that raw material makes by starch.Therefore utilizing bamboo/wood tar oil and furfural to substitute the method for phenol and formaldehyde novolak resin, help to solve the shortcoming that existing resol raw material exists, is a kind of practicable resins approach than environmental protection.
(3) summary of the invention
The objective of the invention is to utilize bamboo (wood) the charcoal main by product bamboo of production (wood) tar replacing whole phenol and furfural to synthesize thermosetting resin.
The technical scheme that the present invention adopts is:
A kind of bamboo/wood tar oil-furfural thermosetting resin is prepared by following method:
(1) by tar and furfural mass ratio 1: 1.0~1.2 bamboo/wood tar oil and furfural are placed reactor drum, stir, be preheated to 65 ℃~75 ℃;
(2) adding basic catalyst, to make pH be 8~11, in 85 ℃~110 ℃ reaction 2~5h down; Said basic catalyst quality consumption is 7~9% of bamboo/wood tar oil quality;
(3) reaction end afterreaction liquid naturally cools to 45~55 ℃, and decompression dehydration gets said bamboo/wood tar oil-furfural thermosetting resin.
Tar is a kind of thick liquid of black, is the pyrogenous product of organism process heating, and bamboo/wood tar oil of the present invention is the product of bamboo or wood distillation process, and wherein the mol ratio of phenols and furfural is less than 1.
Bamboo/wood tar oil of the present invention-furfural thermosetting resin, solids content are 64~72%, and viscosity is 4700~7000mPas (25 ℃), and the pH value is 8~11, and furfural content is 0.9~1.20% (mass percent), and solidification value is 150~160 ℃.
The invention still further relates to the preparation method of described bamboo/wood tar oil-furfural thermosetting resin, said method is following:
(1) by tar and furfural mass ratio 1: 1.0~1.2 bamboo/wood tar oil and furfural are placed reactor drum, stir, be preheated to 65 ℃~75 ℃;
(2) adding basic catalyst, to make pH be 8~11, in 85 ℃~110 ℃ reaction 2~5h down; Said basic catalyst quality consumption is 7~9% of bamboo/wood tar oil quality; Said basic catalyst can be alkali metal hydroxide, like sodium hydroxide, Pottasium Hydroxide etc., can aqueous solution form add in the reactor drum, and aqueous solution mass concentration is 30~50%;
(3) reaction end afterreaction liquid naturally cools to 45~55 ℃, and decompression dehydration gets said bamboo/wood tar oil-furfural thermosetting resin.
Preferably, said basic catalyst is the aqueous sodium hydroxide solution of mass concentration 40%, and the sodium hydroxide quality is 7~9% of bamboo/wood tar oil quality in the aqueous solution.
Preferably, said aqueous sodium hydroxide solution adds in the reactor drum in batches: at first add 70~80% of catalyzer total mass, be heated to 85 ℃~110 ℃ reaction 0.5h after, add remaining catalyzer again, in 85 ℃~110 ℃ reaction 1.5~4h.
Preferably, said step (3) decompression dehydration carries out dewatering time 2~3h under vacuum tightness 0.08~0.09MPa.
Chief value of the present invention is mainly reflected in: the present invention utilizes the whole fortified phenols of by product bamboo/wood tar oil and the synthetic thermosetting resin of furfural of bamboo/wood working; Not only help to solve existing resol and prepare problems such as the material toxicity that process exists is big, environmental pollution; And bamboo/charcoal by product bamboo/wood tar oil turned waste into wealth; Having made full use of resource, is a new way than environmental protection of preparation phenolic resinoid.
(4) description of drawings
The bamboo tar that Fig. 1 makes for embodiment-furfural resol IR collection of illustrative plates.
(5) embodiment
Below in conjunction with specific embodiment the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
Take by weighing 66.58g bamboo tar (from certain bamboo charcoal source mill by product; Analyze through FTIR; Mainly contain phenolic cpds such as phenol, 4-ethylphenol, 2-ethylphenol, 6-syringol) place the 250mL there-necked flask; Take by weighing the 66.57g furfural again and mix with above-mentioned bamboo tar, taking by weighing 4.663g NaOH then, to be made into massfraction be 40% the aqueous solution.Above-mentioned there-necked flask is put into magnetic agitation, put into 70 ℃ oil bath preheating and stir 30min, be warming up to 85 ℃ then; Add for the first time 9.32g NaOH solution; Add remaining NaOH solution behind the 30min, reaction 4h stops heating, naturally cooling under 85 ℃ of temperature afterwards.
When the reaction product temperature is reduced to 50 ℃, be decompression dehydration under the 0.09MPa in vacuum tightness, decompression dehydration 2h gets product.Its product solids content is 67.7%, and viscosity is 6099mPas, and the pH value is 9.7, and furfural content is 1.17%.
Embodiment 2:
Take by weighing 66.60g bamboo tar (with embodiment 1) and place the 250mL there-necked flask, take by weighing the 79.00g furfural again and mix with above-mentioned bamboo tar, taking by weighing 5.322g NaOH then, to be made into massfraction be 40% the aqueous solution.Above-mentioned there-necked flask is put into magnetic agitation, put into 70 ℃ oil bath preheating and stir 30min, be warming up to 95 ℃ then; Add for the first time 10.64g NaOH solution; Add remaining NaOH solution behind the 30min again, reaction 2h stops heating, naturally cooling under 95 ℃ of temperature afterwards.
After the reaction product temperature is reduced to 50 ℃, be decompression dehydration under the 0.09MPa in vacuum tightness, decompression dehydration 2h gets product.Its product solids content is 64.3%, and viscosity is 4766mPas, and the pH value is 9.7, and furfural content is 1.14%, and its IR collection of illustrative plates is referring to Fig. 1.
Embodiment 3:
Take by weighing the 64.73g wood tar oil (from certain charcoal source mill by product; Analyze through FTIR; Mainly contain phenolic cpds such as phenol, 4-ethylphenol, 2-ethylphenol, 6-syringol) place the 250mL there-necked flask; Take by weighing the 71.20g furfural again and mix with above-mentioned wood tar oil, taking by weighing 5.176g NaOH then, to be made into massfraction be 40% the aqueous solution.Above-mentioned there-necked flask is put into magnetic agitation, put into 70 ℃ oil bath preheating and stir 30min, be warming up to 105 ℃ then; Add for the first time 10.35g NaOH solution; Add remaining NaOH catalyzer behind the 30min, reaction 3h stops heating, naturally cooling under 105 ℃ of temperature afterwards.
When the reaction product temperature drops to 50 ℃, beginning in vacuum tightness is decompression dehydration under the 0.09MPa, and decompression dehydration 2h gets product.Its product solids content is 71.4%, and viscosity is 6987mPas, and the pH value is 10.1, and furfural content is 0.94%.
Embodiment 4:
Take by weighing 40.00g embodiment 1 prepared bamboo tar-furfuryl resin and be uniformly coated on the plank of three layers of (on four sides) 25cm * 25cm, adopt pressure sintering glue plywood.Hot pressing condition: gluing precompressed 0.5h, pressure are 2.7MPa, and temperature is 140~150 ℃, and hot pressing time is 4min (1min/mm).The gained wood veneer detects the bonding strength of test specimen according to the requirement of GB/T 17657-1999 " Test methods of evaluating the properties of woodbased panels and surface decorated woodbased panels ", and gained wood veneer gummed is functional.
Claims (5)
1. bamboo/wood tar oil-furfural thermosetting resin is prepared by following method:
(1) by tar and furfural mass ratio 1: 1.0~1.2 bamboo/wood tar oil and furfural are placed reactor drum, stir, be preheated to 65 ℃~75 ℃;
(2) adding basic catalyst, to make pH be 8~11, in 85 ℃~110 ℃ reaction 2~5h down; Said basic catalyst quality consumption is 7~9% of bamboo/wood tar oil quality;
(3) reaction solution naturally cools to 45~55 ℃, and decompression dehydration gets said bamboo/wood tar oil-furfural thermosetting resin.
2. the preparation method of bamboo/wood tar oil as claimed in claim 1-furfural thermosetting resin, said method is following:
(1) by tar and furfural mass ratio 1: 1.0~1.2 bamboo/wood tar oil and furfural are placed reactor drum, stir, be preheated to 65 ℃~75 ℃;
(2) adding basic catalyst, to make pH be 8~11, in 85 ℃~110 ℃ reaction 2~5h down; Said basic catalyst quality consumption is 7~9% of bamboo/wood tar oil quality;
(3) reaction solution naturally cools to 45~55 ℃, and decompression dehydration gets said bamboo/wood tar oil-furfural thermosetting resin.
3. method as claimed in claim 2 is characterized in that said basic catalyst is the aqueous sodium hydroxide solution of mass concentration 40%, and the sodium hydroxide quality is 7~9% of bamboo/wood tar oil quality in the aqueous solution.
4. method as claimed in claim 3; It is characterized in that said aqueous sodium hydroxide solution adds in the reactor drum in batches: at first add 70~80% of catalyzer total mass; After being heated to 85 ℃~110 ℃ reaction 0.5h, add remaining catalyzer again, in 85 ℃~110 ℃ reaction 1.5~4h.
5. method as claimed in claim 2 is characterized in that said step (3) decompression dehydration carries out dewatering time 2~3h under vacuum tightness 0.08~0.09MPa.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103289718A (en) * | 2013-07-02 | 2013-09-11 | 西北大学 | Method for preparing dephenolized oil and phenolic resin through medium and low temperature coal tar oil |
CN109609111A (en) * | 2018-12-27 | 2019-04-12 | 长江大学 | A kind of wood tar resin sand consolidation agent and its preparation method and application |
CN111793488A (en) * | 2019-04-08 | 2020-10-20 | 中国石油化工股份有限公司 | Chemical sand prevention agent for wood tar, preparation method and application thereof |
CN111852362A (en) * | 2019-04-28 | 2020-10-30 | 中国石油化工股份有限公司 | Chemical sand prevention method for heavy oil thermal recovery |
Citations (2)
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CN101058628A (en) * | 2007-05-25 | 2007-10-24 | 中国林业科学研究院林产化学工业研究所 | Lignin modified phenol furfural resin for moulding material and preparation method thereof |
CN101717491A (en) * | 2009-11-20 | 2010-06-02 | 北京化工大学 | Method for preparing and condensing polyaromatic hydrocarbon resin by using bamboo tar |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101058628A (en) * | 2007-05-25 | 2007-10-24 | 中国林业科学研究院林产化学工业研究所 | Lignin modified phenol furfural resin for moulding material and preparation method thereof |
CN101717491A (en) * | 2009-11-20 | 2010-06-02 | 北京化工大学 | Method for preparing and condensing polyaromatic hydrocarbon resin by using bamboo tar |
Non-Patent Citations (1)
Title |
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陈盛明等: "酚醛树脂的绿色化研究", 《塑料工业》 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103289718A (en) * | 2013-07-02 | 2013-09-11 | 西北大学 | Method for preparing dephenolized oil and phenolic resin through medium and low temperature coal tar oil |
CN103289718B (en) * | 2013-07-02 | 2015-09-09 | 西北大学 | A kind of middle coalite tar prepares the method for dephenolize oil and resol |
CN109609111A (en) * | 2018-12-27 | 2019-04-12 | 长江大学 | A kind of wood tar resin sand consolidation agent and its preparation method and application |
CN109609111B (en) * | 2018-12-27 | 2021-04-06 | 长江大学 | Wood tar resin sand consolidation agent and preparation method and application thereof |
CN111793488A (en) * | 2019-04-08 | 2020-10-20 | 中国石油化工股份有限公司 | Chemical sand prevention agent for wood tar, preparation method and application thereof |
CN111852362A (en) * | 2019-04-28 | 2020-10-30 | 中国石油化工股份有限公司 | Chemical sand prevention method for heavy oil thermal recovery |
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