CN107325244A - Preparation method for the enzymolysis xylogen base phenolic resin of Plywood - Google Patents
Preparation method for the enzymolysis xylogen base phenolic resin of Plywood Download PDFInfo
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- CN107325244A CN107325244A CN201710690016.3A CN201710690016A CN107325244A CN 107325244 A CN107325244 A CN 107325244A CN 201710690016 A CN201710690016 A CN 201710690016A CN 107325244 A CN107325244 A CN 107325244A
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- enzymolysis xylogen
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- phenolic resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/12—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
- C08G14/08—Ureas; Thioureas
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C09J161/04, C09J161/18 and C09J161/20
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Phenolic Resins Or Amino Resins (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides the preparation method of the enzymolysis xylogen base phenolic resin for Plywood, method includes 75 80 grams of addition containers of phenol and started to warm up in 55 60 DEG C of water-bath, 145 grams of 60 64 grams of formalin, 6.0 6.5 grams of alkali lye, 75 80 grams of enzymolysis xylogen and water are added into the container successively, and 80 DEG C are warming up to, then insulation reaction 75 80 minutes；Formalin is added in two times, 45 48 grams are added every time, after reacting 55 60 minutes, is cooled to 65 70 DEG C；Then 22 25 grams of aqueous slkali is added again, and adds 12.0 12.8 grams of urea, insulation reaction 38 40 minutes under the conditions of 65 70 DEG C；Cool to 45 DEG C of dischargings, prepare enzymolysis xylogen base phenolic resin adhesive.After Plywood is prepared, burst size of methanal is less than 0.3 mg/litre, reaches E1 grades of levels of national standard.
Description
Technical field
Embodiments of the invention are related to the preparation method of the enzymolysis xylogen base phenolic resin for Plywood.
Background technology
Phenolic resin is one of big glue kind of wood adhesive three (Lauxite, phenolic resin and melmac), three
Kind of adhesive with it is respective the characteristics of and advantage be widely used in wood working industry, its main raw material(s) both is from non-renewable
Petrochemicals, as people constantly strengthen the consciousness of shortage of resources crisis and environmental pollution increasingly serious concern, make wood
The expanding production and expansion application field of material processing industry synvaren (outdoor material must be used) are by price
Raise the serious challenge that control is superintended and directed with pollution.Enzymolysis xylogen derives from what is extracted after reproducible fermentation of plant straws in remaining residue
Lignin, due to lignin is in itself natural aldehydes matter and property with phenol, and the relatively good guarantor of enzymolysis xylogen
The chemism of lignin has been stayed, rich in phenolic hydroxyl group, expensive and poisonous phenol synthesis phenolic aldehyde tree can be partly replaced using it
Fat adhesive, therefore the manufacturing process research and application study of Efforts To Develop lignin phenol formaldehyde resin adhesive are phenolic resin
Development trend, with important social benefit and significant economic benefit.
The content of the invention
The invention provides a kind of method for preparing the enzymolysis xylogen base phenolic resin for Plywood, method bag
Include：Start to warm up 75-80 grams of addition container of phenol and in 55-60 DEG C of water-bath, successively by 60-64 grams of formalin,
145 grams of 6.0-6.5 grams of alkali lye, 75-80 grams of enzymolysis xylogen and water add the container, and are warming up to 80 DEG C, are then incubated anti-
Answer 75-80 minutes；Formalin is added in two times, 45-48 grams is added every time, after reacting 55-60 minutes, is cooled to 65-70
℃；Then 22-25 grams of aqueous slkali is added again, and adds 12.0-12.8 grams of urea, the insulation reaction under the conditions of 65-70 DEG C
38-40 minutes；Cool to 45 DEG C of dischargings, prepare enzymolysis xylogen base phenolic resin adhesive.
In the above-mentioned methods, wherein, the container be three-necked flask.
In the above-mentioned methods, wherein, the purity of the phenol is 98%.
In the above-mentioned methods, wherein, the mass concentration of the formalin is 37%.
In the above-mentioned methods, wherein, the alkali lye is sodium hydroxide solution, and the quality of the sodium hydroxide in the alkali lye is dense
Spend for 50%.
The enzymolysis xylogen base phenolic resin adhesive that the present invention is prepared is after for preparing Plywood, first
Aldehyde burst size is less than 0.3 mg/litre, reaches E1 grades of national standard (≤1.5 mg/litre) level.In addition, the bonding strength of sheet material is also high
In national standard I class bonding strengths.In addition, enzymolysis xylogen, which is made, using discarded object fermentation of plant straws turns waste into wealth, it is made
Phenolic resin adhesive cost reduction by 45% or so, and be conducive to environmental protection, and generate huge economic benefit.
Embodiment
The following examples can make those skilled in the art that the present invention is more fully understood, but not limit in any way
The present invention.
In order to equably be heated, the present invention uses water-bath, first by heat collecting type constant-temperature heating magnetic stirring apparatus water
Bath is warming up to 55-60 DEG C；Afterwards by 75-80 grams of the phenol of thawing (purity of phenol is 98%) add three-necked flask and
Started to warm up in 55-60 DEG C of water-bath, slowly (about 15-20 minutes, too urgent or addition simultaneously easily produced secondary anti-successively
Should) by 60-64 grams of formalin (mass concentration is 37%), 6.0-6.5 grams of alkali lye (mass concentration of sodium hydroxide be 50%),
145 grams of addition three-necked flasks of 75-80 grams of enzymolysis xylogen and water, and 80 DEG C are warming up to, then insulation reaction 75-80 minutes；Point
Slowly (every time about 3 minutes) add each 45-48 grams of reaction 55-60 of second, third batch of formalin (concentration is 37%) twice
After minute, 65-70 DEG C is cooled to；Then slowly adding within (about 3 minutes) second batch aqueous slkali, (mass concentration of sodium hydroxide is
50%) 22-25 grams, and 12.0-12.8 grams of urea is added, insulation reaction 38-40 minutes under the conditions of 65-70 DEG C；It is last cold
But 45 DEG C of dischargings are cooled to, enzymolysis xylogen base phenolic resin adhesive is prepared.
The pH of the enzymolysis xylogen base phenolic resin adhesive prepared by method measurement commonly used in the art and trip
From the amount of formaldehyde.In addition, obtained enzymolysis xylogen base phenolic resin adhesive is used to prepare Plywood, and assay plate
Material bonding strength and burst size of methanal.
Embodiment 1
1) heat collecting type constant-temperature heating magnetic stirring apparatus water-bath is warming up to 60 DEG C；
2) 80 grams of the phenol (purity of phenol is 98%) of thawing is added into three-necked flask and started to warm up in water-bath,
Successively slowly (about 15 minutes) by 64 grams of formalin (concentration is 37%), alkali lye (mass concentration of sodium hydroxide be 50%)
145 grams of 6.5 grams, 80 grams of enzymolysis xylogen and water add three-necked flasks, and are warming up to 80 DEG C, then insulation reaction 80 minutes；
3) slowly (every time about 3 minutes) add each 48 grams of second, third batch of formalin (concentration 37%) instead in two times
Answer after 60 minutes, be cooled to 70 DEG C；
4) 25 grams of second batch aqueous slkali (mass concentration of sodium hydroxide is 50%) and then is slowly added within (about 3 minutes),
And add 12.8 grams of urea, insulation reaction 40 minutes under the conditions of 70 DEG C；
5) cool to 45 DEG C of dischargings, prepare enzymolysis xylogen base phenolic resin adhesive.
Enzymolysis xylogen base synvaren leading indicator made from the above method：PH=10.32, free formaldehyde contains
Measure as 0.19%.
Above-mentioned adhesive is used to prepare Plywood, glue-spread about 150g/m2, detected by 8 test specimens, with
Reduce accidental error, average sheet material bonding strength is 0.937MPa (being shown in Table 1), and burst size of methanal is 0.28 mg/litre, reaches state
Mark E1 grades of (≤1.5 mg/litre) levels.
The Plywood shear strength of table 1 is detected
Note：The class bonding strength of national standard I >=0.75MPa
Embodiment 2
1) heat collecting type constant-temperature heating magnetic stirring apparatus water-bath is warming up to 55 DEG C；
2) 75 grams of the phenol (purity of phenol is 98%) of thawing is added into three-necked flask and started to warm up in water-bath,
Successively slowly (about 20 minutes) by 60 grams of formalin (concentration is 37%), alkali lye (mass concentration of sodium hydroxide be 50%)
145 grams of 6.0 grams, 75 grams of enzymolysis xylogen and water add three-necked flasks, and are warming up to 80 DEG C, then insulation reaction 75 minutes；
3) slowly (every time about 3 minutes) add each 45 grams of second, third batch of formalin (concentration 37%) instead in two times
Answer after 55 minutes, be cooled to 65 DEG C；
4) 22 grams of second batch aqueous slkali (mass concentration of sodium hydroxide is 50%) and then is slowly added within (about 3 minutes),
And add 12.0 grams of urea, insulation reaction 38 minutes under the conditions of 65 DEG C；
5) cool to 45 DEG C of dischargings, prepare enzymolysis xylogen base phenolic resin adhesive.
Enzymolysis xylogen base synvaren leading indicator made from the above method：PH=10.41, free formaldehyde contains
Measure as 0.27%.
Above-mentioned adhesive is used to prepare Plywood, glue-spread about 120g/m2, detected by 8 test specimens, with
Reduce accidental error, average sheet material bonding strength is 0.931MPa (being shown in Table 1), and burst size of methanal is 0.29 mg/litre, reaches state
Mark E1 grades of (≤1.5 mg/litre) levels.
The Plywood shear strength of table 2 is detected
Note：The class bonding strength of national standard I >=0.75MPa
From the foregoing, it will be observed that the enzymolysis xylogen base phenolic resin adhesive that the present invention is prepared is for preparing wood gluing
After plate, burst size of methanal is less than 0.3 mg/litre, reaches E1 grades of national standard (≤1.5 mg/litre) level.In addition, the glue of sheet material
Intensity is closed also above national standard I class bonding strengths, is the structure and decorative material of the indoor and outdoor purposes of environment-friendly type high-quality.In addition, making
Enzymolysis xylogen, which is made, with discarded object fermentation of plant straws turns waste into wealth, made enzymolysis xylogen base phenolic resin gluing
Agent cost reduction by 45% or so, not only expands the purposes of product, and is conducive to environmental protection, and generates huge economy
Benefit.
It will be understood by those skilled in the art that above example is only exemplary embodiment, in the spirit without departing substantially from the present invention
In the case of scope, a variety of changes can be carried out, replaces and changes.
Claims (5)
1. a kind of method for preparing enzymolysis xylogen base phenolic resin adhesive, including：
Start to warm up 75-80 grams of addition container of phenol and in 55-60 DEG C of water-bath, successively by 60-64 grams of formalin,
145 grams of 6.0-6.5 grams of alkali lye, 75-80 grams of enzymolysis xylogen and water add the container, and are warming up to 80 DEG C, are then incubated anti-
Answer 75-80 minutes；
Formalin is added in two times, 45-48 grams is added every time, after reacting 55-60 minutes, is cooled to 65-70 DEG C；
Then 22-25 grams of aqueous slkali is added again, and adds 12.0-12.8 grams of urea, the insulation reaction under the conditions of 65-70 DEG C
38-40 minutes；
Cool to 45 DEG C of dischargings, prepare enzymolysis xylogen base phenolic resin adhesive.
2. according to the method described in claim 1, wherein, the container be three-necked flask.
3. according to the method described in claim 1, wherein, the purity of the phenol is 98%.
4. according to the method described in claim 1, wherein, the mass concentration of the formalin is 37%.
5. according to the method described in claim 1, wherein, the alkali lye is sodium hydroxide solution, the hydroxide in the alkali lye
The mass concentration of sodium is 50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710690016.3A CN107325244A (en) | 2017-08-14 | 2017-08-14 | Preparation method for the enzymolysis xylogen base phenolic resin of Plywood |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710690016.3A CN107325244A (en) | 2017-08-14 | 2017-08-14 | Preparation method for the enzymolysis xylogen base phenolic resin of Plywood |
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| Publication Number | Publication Date |
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| CN107325244A true CN107325244A (en) | 2017-11-07 |
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ID=60225809
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710690016.3A Pending CN107325244A (en) | 2017-08-14 | 2017-08-14 | Preparation method for the enzymolysis xylogen base phenolic resin of Plywood |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412796A (en) * | 2008-11-21 | 2009-04-22 | 福州大学 | Hot melt type phenolic resin modified by using enzymatic hydrolysis lignin or derivatives thereof, and preparation thereof |
| CN104140508A (en) * | 2013-05-09 | 2014-11-12 | 东北林业大学 | Preparation method of enzymolysis lignin-based phenolic resin |
| CN105694781A (en) * | 2016-04-05 | 2016-06-22 | 北京林业大学 | Preparation and application methods of lignin-base green adhesive |
-
2017
- 2017-08-14 CN CN201710690016.3A patent/CN107325244A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412796A (en) * | 2008-11-21 | 2009-04-22 | 福州大学 | Hot melt type phenolic resin modified by using enzymatic hydrolysis lignin or derivatives thereof, and preparation thereof |
| CN104140508A (en) * | 2013-05-09 | 2014-11-12 | 东北林业大学 | Preparation method of enzymolysis lignin-based phenolic resin |
| CN105694781A (en) * | 2016-04-05 | 2016-06-22 | 北京林业大学 | Preparation and application methods of lignin-base green adhesive |
Non-Patent Citations (1)
| Title |
|---|
| 刘纲勇等: "尿素对木质素酚醛树脂胶粘剂性能的影响", 《精细化工》 * |
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Application publication date: 20171107 |
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