CN105348460B - A kind of cellulosic ethanol lignin modification Phenolic resin wood adhesive and preparation method thereof - Google Patents
A kind of cellulosic ethanol lignin modification Phenolic resin wood adhesive and preparation method thereof Download PDFInfo
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- CN105348460B CN105348460B CN201510827672.4A CN201510827672A CN105348460B CN 105348460 B CN105348460 B CN 105348460B CN 201510827672 A CN201510827672 A CN 201510827672A CN 105348460 B CN105348460 B CN 105348460B
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Abstract
The invention discloses a kind of cellulosic ethanol lignin modification Phenolic resin wood adhesive and preparation method thereof, belongs to environment-friendly type based Wood Adhesives preparing technical field.Heretofore described preparation method comprises the following steps：Cellulosic ethanol lignin, phenol, piece alkali, water are added into reactor, insulation reaction, formalin, first liquid caustic soda and second batch water, second batch formalin and second batch liquid caustic soda are then added successively, and carry out isothermal holding respectively, then urea is added, is obtained through cooling discharging.This method substitutes 40% phenol using cellulose with Vinsol, the timber of preparation is only 0.37% with free formaldehyde content in lignin-base phenolic resin adhesive, free phenol content is 0.28%, the glued board bonding strength prepared using the adhesive is 1.12MPa, reach national I class plate intensity requirement, burst size of methanal is 0.28mg/L, reaches national E0 levels standard.
Description
Technical field
The present invention relates to environment-friendly type based Wood Adhesives preparing technical field, and in particular to a kind of cellulosic ethanol lignin changes
Property Phenolic resin wood adhesive and preparation method thereof.
Background technology
China's wood-based plate consumes substantial amounts of petrochemical material with based Wood Adhesives every year, by cost of material and environmental factor shadow
Sound is larger, in great demand for low cost, high-performance environmentally-friendly based Wood Adhesives.On the other hand, using forest and agricultural biomass as raw material
Prepare bio-ethanol by biorefinery has turned into the important development direction of biomass energy, is generated during biorefinery
Substantial amounts of high activity lignin, these accessory substances fail well to be utilized all the time, are mainly taken as fuel burn-up.By
Research finds that the high activity lignin contained in this part accessory substance, molecular structure is similar to phenol, available for replacement part benzene
Phenol prepares timber phenolic resin adhesive.By the theoretical research to cellulosic ethanol lignin component and molecular structure,
The fundamental research of the molecule synthesis, Mechanism of Copolymerization that are carried out to cellulosic ethanol lignin-base phenolic resin adhesive, can
To realize making full use of for biomass resource, the integrated cost of bio-ethanol and wood-based plate secondary industry is reduced, promotes biology refining
The coordinated development of industry processed and wood-based plate industry.
The substitution rate that existing biorefinery lignin substitutes phenol is generally relatively low, and lignin raw material need purification in advance or
Person is used further to prepare lignin phenol formaldehyde resin adhesive after chemical modification is handled, when producing glued board, sheet material precompressed
It is poor, using limited in produce reality.
The content of the invention
For biorefinery accessory substance --- cellulosic ethanol lignin utilization rate it is not high to caused by environment pollution and
The caused wasting of resources, realize the higher value application of cellulosic ethanol lignin；And for wood-based plate based Wood Adhesives
High to petrochemical material dependency degree, there is certain environmental issue to health in veneered product, primary and foremost purpose of the invention is
A kind of preparation method of cellulosic ethanol lignin modification Phenolic resin wood adhesive is provided.The present invention utilizes cellulosic ethanol
Lignin substitutes part phenol and prepares biomass-based environment-friendly type based Wood Adhesives, can reduce production cost, lifts environmental protection quality,
Realize the Green Development of wood-based plate industry.
The cellulosic ethanol lignin modification phenolic aldehyde tree obtained another object of the present invention is to provide above-mentioned preparation method
Fat based Wood Adhesives.
The purpose of the present invention is achieved through the following technical solutions：A kind of cellulosic ethanol lignin modification phenol resin timber
The preparation method of adhesive, comprises the following steps：
(1) phenol 72g, cellulosic ethanol lignin 48g, liquid caustic soda 2.7g, first water 40mL are added in reactor,
90~92 DEG C are warming up to, is incubated 30~50 minutes；
(2) after insulation terminates, first formaldehyde 156g is added, 30~50 minutes are incubated under the conditions of 70~75 DEG C；
(3) first liquid caustic soda 14.4g, second batch water 40mL are added, 30~50 minutes are incubated under the conditions of 80~85 DEG C；
(4) after insulation terminates, second batch formaldehyde 72g is added, second batch liquid caustic soda 14.4g, is incubated under the conditions of 80~85 DEG C
30~50 minutes；
(5) the 3rd crowd of liquid caustic soda 14.4g is added, under the conditions of 90~92 DEG C, is reacted to 0.15~0.20Pas of viscosity, drop
Temperature adds urea 20g to 80 DEG C, then is cooled to 50 DEG C, cooling discharging.
The preparation method of cellulosic ethanol lignin described in step (1) is：During cellulosic ethanol production, straw
Stalk is after steam blasting and soda acid processing, then passes through enzymolysis, and carbohydrate therein is fermented and distills caused solid later
Discarded object main component is exactly cellulose ethanol lignin, and its molecular structure also contains in addition to lignin hydrophobic structure in itself
Phenolic hydroxyl group, alcoholic extract hydroxyl group, carboxyl isoreactivity group, it is different to prepare the lignin of paper pulp from traditional sulphite or alkaline-heating method, fine
The chemism that plain ethanol lignin preferably remains lignin is tieed up, than alkali lignin, lignosulfonates etc. containing more
Lignin component.
A kind of cellulosic ethanol lignin modification Phenolic resin wood adhesive is obtained by above-mentioned preparation method.
The present invention is had the following advantages relative to prior art and effect：
A kind of preparation method of cellulosic ethanol lignin modification Phenolic resin wood adhesive provided by the invention, the party
Method substitutes 40% phenol using cellulose with Vinsol, the timber of preparation lignin-base phenolic resin adhesive have compared with
Good combination property, its free formaldehyde content is only 0.37%, free phenol content 0.28%, is prepared using the adhesive
Glued board bonding strength is 1.12MPa, reaches national I class plate intensity requirement, burst size of methanal 0.28mg/L, reaches national E0
Level standard.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
(1) phenol 72g, cellulosic ethanol lignin 48g, liquid caustic soda 2.7g, first water 40mL are added in reactor,
90 DEG C are warming up to, is incubated 50 minutes；
(2) after insulation terminates, first formaldehyde 156g is added, 50 minutes are incubated under the conditions of 70 DEG C；
(3) first liquid caustic soda 14.4g, second batch water 40mL are added, 50 minutes are incubated under the conditions of 80 DEG C；
(4) after insulation terminates, second batch formaldehyde 72g, second batch liquid caustic soda 14.4g are added, 50 points are incubated under the conditions of 80 DEG C
Clock；
(5) the 3rd crowd of liquid caustic soda 14.4g is added, under the conditions of 90 DEG C, reacts to 0.15~0.20Pas of viscosity, is cooled to
80 DEG C, urea 20g is added, then is cooled to 50 DEG C, cooling discharging.
Embodiment 2
(1) phenol 72g, cellulosic ethanol lignin 48g, liquid caustic soda 2.7g, first water 40mL are added in reactor,
92 DEG C are warming up to, is incubated 30 minutes；
(2) after insulation terminates, first formaldehyde 156g is added, 30 minutes are incubated under the conditions of 75 DEG C；
(3) first liquid caustic soda 14.4g, second batch water 40mL are added, 30 minutes are incubated under the conditions of 85 DEG C；
(4) after insulation terminates, second batch formaldehyde 72g, second batch liquid caustic soda 14.4g are added, 30 points are incubated under the conditions of 85 DEG C
Clock；
(5) the 3rd crowd of liquid caustic soda 14.4g is added, under the conditions of 92 DEG C, reacts to 0.15~0.20Pas of viscosity, is cooled to
80 DEG C, urea 20g is added, then is cooled to 50 DEG C, cooling discharging.
Embodiment 3
(1) phenol 72g, cellulosic ethanol lignin 48g, liquid caustic soda 2.7g, first water 40mL are added in reactor,
91 DEG C are warming up to, is incubated 40 minutes；
(2) after insulation terminates, first formaldehyde 156g is added, 40 minutes are incubated under the conditions of 73 DEG C；
(3) first liquid caustic soda 14.4g, second batch water 40mL are added, 40 minutes are incubated under the conditions of 83 DEG C；
(4) after insulation terminates, second batch formaldehyde 72g, second batch liquid caustic soda 14.4g are added, 40 points are incubated under the conditions of 83 DEG C
Clock；
(5) the 3rd crowd of liquid caustic soda 14.4g is added, under the conditions of 91 DEG C, reacts to 0.15~0.20Pas of viscosity, is cooled to
80 DEG C, urea 20g is added, then is cooled to 50 DEG C, cooling discharging.
The preparation method of cellulosic ethanol lignin modification Phenolic resin wood adhesive in above-described embodiment 1~3, utilize
Cellulose substitutes 40% phenol with Vinsol, and the timber of preparation lignin-base phenolic resin adhesive has preferably comprehensive
Performance is closed, the free formaldehyde content in the cellulosic ethanol lignin modification Phenolic resin wood adhesive prepared is only
0.37%, free phenol content 0.28%, the glued board bonding strength prepared using the adhesive is 1.12MPa, reaches state
I class plate intensity requirement of family, burst size of methanal 0.28mg/L, reaches national E0Level standard.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (2)
- A kind of 1. preparation method of cellulosic ethanol lignin modification Phenolic resin wood adhesive, it is characterised in that：Including with Lower step：(1) phenol 72g, cellulosic ethanol lignin 48g, liquid caustic soda 2.7g, first water 40mL are added in reactor, heated up To 90~92 DEG C, 30~50 minutes are incubated；(2) after insulation terminates, first formaldehyde 156g is added, 30~50 minutes are incubated under the conditions of 70~75 DEG C；(3) first liquid caustic soda 14.4g, second batch water 40mL are added, 30~50 minutes are incubated under the conditions of 80~85 DEG C；(4) insulation terminate after, add second batch formaldehyde 72g, second batch liquid caustic soda 14.4g, under the conditions of 80~85 DEG C be incubated 30~ 50 minutes；(5) the 3rd crowd of liquid caustic soda 14.4g is added, under the conditions of 90~92 DEG C, reacts to 0.15~0.20Pas of viscosity, is cooled to 80 DEG C, urea 20g is added, then is cooled to 50 DEG C, cooling discharging.
- A kind of 2. cellulosic ethanol lignin modification phenol resin timber gluing that preparation method as claimed in claim 1 obtains Agent.
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| CN106854264A (en) * | 2016-12-02 | 2017-06-16 | 江南大学 | A kind of rice husk sill quality modified phenolic resin adhesive preparation method |
| CN109679044A (en) * | 2018-12-21 | 2019-04-26 | 上海昶法新材料有限公司 | A kind of preparation method of the modified phenolic resin adhesive suitable for bond paper |
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| CN103555237B (en) * | 2013-10-24 | 2015-04-15 | 嘉善中林胶粘剂科技有限公司 | Method for preparing environment-friendly adhesive for biomass wood materials |
| CN103980858B (en) * | 2014-05-26 | 2016-06-08 | 北华大学 | Laccase activated cellulose ethanol lignin is utilized to prepare biomass-based adhesive and method thereof |
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Application publication date: 20160224 Assignee: JIANGSU LANDIS WOOD CO., LTD. Assignor: Beihua University Contract record no.: 2019320000030 Denomination of invention: Cellulosic ethanol lignin modified phenolic resin wood adhesive and preparation method thereof Granted publication date: 20171117 License type: Common License Record date: 20190314 |
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