CN114350314A - Waste molasses-based high-performance environment-friendly adhesive and preparation method and application thereof - Google Patents
Waste molasses-based high-performance environment-friendly adhesive and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a waste molasses-based high-performance environment-friendly adhesive and a preparation method thereof, wherein the adhesive is prepared from the following raw materials in parts by weight: 150 parts of waste molasses, 30-40 parts of maleic anhydride modified polyethylene, 20-40 parts of silicon dioxide nano powder, 10-20 parts of ammonium polyphosphate, 2-4 parts of KH560 silane coupling agent, 2-4 parts of sodium hexametaphosphate, 0.5-0.8 part of oxalic acid and 5-15 parts of distilled water; the solid content of the environment-friendly adhesive for the plywood is 86.3-87.5%, and the viscosity range is 880-1420mPa & s. The adhesive provided by the invention has good weather resistance, bonding strength and moderate viscosity, overcomes the defect that the solid content of the traditional natural adhesive for the plywood can not be increased due to overlarge viscosity, and improves the thermosetting speed and bonding strength.
Description
Technical Field
The invention belongs to the technical field of adhesive preparation, and particularly relates to a waste molasses-based high-performance environment-friendly adhesive as well as a preparation method and application thereof.
Background
The glue used in the wood industry is mainly urea-formaldehyde glue. The urea-formaldehyde adhesive is urea and formaldehyde which are condensed into initial urea-formaldehyde resin under the action of an acidic or alkaline catalyst, and then the initial urea-formaldehyde resin is formed into infusible and insoluble urea-formaldehyde adhesive under the action of a curing agent or an auxiliary agent. The urea-formaldehyde adhesive has the advantages of low price, easily available raw materials, high bonding strength, simple manufacture, convenient use and the like, occupies a large proportion in the adhesives for wood processing production, and becomes the main adhesive species for wood production in China, wherein the urea-formaldehyde adhesive accounts for more than 90% of the adhesive amount for artificial boards in the wood industry. However, the urea-formaldehyde adhesive is prepared by using formaldehyde as a main raw material, so that formaldehyde is released from the adhesive and products thereof, and if the formaldehyde release exceeds the standard, the harm to the health of human bodies can be caused, so that the low-toxicity wood adhesive which is in line with the international market is important to research and development of organization strength. Although, there are a number of researchers thought on trying to reduce the free formaldehyde content in phenolic resins, such as optimizing the synthesis process; the proportion of reactants is changed, and the content of phenol is increased; the addition of formaldehyde trapping agent, etc. has certain effect on reducing the content of free formaldehyde, but the method cannot eliminate the influence of formaldehyde fundamentally, and only the method for completely eliminating the influence of formaldehyde is a method without formaldehyde.
The traditional natural adhesive for the plywood is modified by adopting isolated soy protein or starch mostly, the adhesive has poor heat conductivity, high viscosity and poor technological performance, hot pressing is carried out immediately after gluing, and the use is inconvenient, so that the development of the high-performance environment-friendly adhesive has important practical significance.
Therefore, in order to solve the technical problems, the invention provides an adhesive using waste molasses as a main raw material, a preparation method of the adhesive and application of the adhesive in preparation of plywood.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the waste molasses-based high-performance environment-friendly adhesive and the preparation method thereof, the adhesive has good weather resistance, bonding strength and moderate viscosity, the defect that the solid content cannot be increased due to overlarge viscosity of the traditional natural adhesive for plywood is overcome, and the thermosetting rate and bonding strength are increased.
In order to achieve the purpose, the invention provides the following technical scheme:
the waste molasses-based high-performance environment-friendly adhesive is prepared from the following raw materials in parts by weight:
preferably, the waste molasses-based high-performance environment-friendly adhesive is prepared from the following raw materials in parts by weight:
preferably, the waste molasses-based high-performance environment-friendly adhesive is prepared from the following raw materials in parts by weight:
preferably, the solid content of the waste molasses is 85%; the solid content of the environment-friendly adhesive for the plywood is 86.3-87.5%, and the viscosity range is 880-1420 mPa.
The invention also provides a preparation method of the waste molasses-based high-performance environment-friendly adhesive, which comprises the following steps:
(1) mixing the waste molasses, oxalic acid and distilled water, stirring at a low speed at a temperature of between 25 and 90 ℃ for reaction for 0.5 to 2 hours, and obtaining a mixed solution A after the reaction is finished;
(2) stirring the mixed solution A obtained in the step (1) of ammonium polyphosphate at a low speed at a temperature of between 25 and 100 ℃ for reaction for 0.5 to 3 hours to obtain a mixed solution B after the reaction is finished;
(3) stirring and reacting the mixed solution B obtained in the step (2) for 0.5-1h at 25-90 ℃ to obtain a mixed solution C after the reaction is finished;
(4) stirring the mixed solution C obtained in the step (3) of the silicon dioxide nano powder at a low speed for 10-30min at 20-30 ℃, and obtaining a mixed solution D after the reaction is finished;
(5) stirring the mixed solution D obtained in the KH560 silane coupling agent step (4) at a low speed for 10min at a temperature of between 20 and 30 ℃ until the mixture is uniform, and obtaining a mixed solution E after the reaction is finished;
(6) and (3) stirring the mixed solution E obtained in the step (5) of sodium hexametaphosphate at a high speed for 20-30min at the temperature of 20-30 ℃, and obtaining the waste molasses-based high-performance environment-friendly adhesive after the reaction is finished.
Preferably, the low-speed stirring is 180-220r/min, and the high-speed stirring is 380-420 r/min.
Preferably, the stirring speed in the step (3) is 180-420 r/min.
The invention also protects the application of the waste molasses-based high-performance environment-friendly adhesive in preparing plywood.
Preferably, in the application of preparing the plywood, the method comprises the following steps: coating the veneer with an environment-friendly adhesive on a veneer, assembling 3 layers of veneers based on a vertical texture mode, and performing hot press molding, wherein the double-side adhesive applying amount is 140-220g/m2The hot pressing temperature is 130-.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the aldehyde-free high-performance high-heat-conductivity adhesive provided by the invention, the catalysis effect of ammonium polyphosphate on molasses hydrolysis and caramelization reaction under an acidic condition is utilized, the chemical structure rearrangement of waste molasses hydrolysis products is realized, and KH560 is used as a coupling agent, so that the generation of high molecular polymers is effectively promoted, and a low molecular weight prepolymer is formed;
(2) according to the formaldehyde-free high-performance high-heat-conductivity adhesive provided by the invention, the problems of poor water resistance, poor weather resistance, low bonding strength and the like of the waste molasses-based adhesive can be solved by adding the silicon dioxide nanopowder, so that the bonding strength of the adhesive and a plywood is greatly improved;
(3) the aldehyde-free high-performance high-heat-conductivity adhesive provided by the invention utilizes a Maillard reaction to generate a chemical crosslinking reaction in the curing process, the viscosity of the adhesive is moderate, the solid content can reach 86.3-87.5%, the viscosity range is 880-1420mPa & s, the defect that the solid content cannot be increased due to overlarge viscosity of the traditional natural adhesive for plywood is overcome, and the heat curing rate and the bonding strength are increased.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a waste molasses-based high-performance environment-friendly adhesive comprises the following steps:
(1) mixing 150 parts of waste molasses, 1 part of oxalic acid and 40 parts of distilled water, stirring at a low speed of 180r/min at 25 ℃ for reaction for 0.5h, and obtaining a mixed solution A after the reaction is finished;
(2) stirring 15 parts of the mixed solution A obtained in the step (1) of ammonium polyphosphate at a low speed of 180r/min at 25 ℃ for reaction for 0.5h to obtain a mixed solution B after the reaction is finished;
(3) stirring 35 parts of the mixed solution B obtained in the step (2) of maleic anhydride modified polyethylene at 25 ℃ at the speed of 200r/min for reaction for 0.5h to obtain a mixed solution C after the reaction is finished;
(4) stirring 30 parts of the mixed solution C obtained in the step (3) of silicon dioxide nano powder at a low speed of 200r/min for 10min at 25 ℃, and obtaining a mixed solution D after the reaction is finished;
(5) 2 parts of KH560 silane coupling agent, stirring the mixed solution D obtained in the step (4) at a low speed of 200r/min at 30 ℃ for 10min until the mixture is uniform, and obtaining a mixed solution E after the reaction is finished;
(6) and (3) stirring 1 part of the mixed solution E obtained in the step (5) of sodium hexametaphosphate at a high speed of 400r/min for 20min at the temperature of 30 ℃, and obtaining the waste molasses-based high-performance environment-friendly adhesive after the reaction is finished.
Example 2
A preparation method of a waste molasses-based high-performance environment-friendly adhesive comprises the following steps:
(1) mixing 150 parts of waste molasses, 0.5 part of oxalic acid and 35 parts of distilled water, stirring at a low speed of 180r/min at the temperature of 30 ℃ for reaction for 20min, and obtaining a mixed solution A after the reaction is finished;
(2) stirring 20 parts of the mixed solution A obtained in the step (1) of ammonium polyphosphate at a low speed of 180r/min at the temperature of 30 ℃ for 10min to react to obtain a mixed solution B after the reaction is finished;
(3) stirring 30 parts of the mixed solution B obtained in the step (2) of maleic anhydride modified polyethylene at the temperature of 30 ℃ at the speed of 200r/min for reaction for 1h to obtain a mixed solution C after the reaction is finished;
(4) stirring 20 parts of the mixed solution C obtained in the step (3) of the silicon dioxide nano powder at a low speed of 200r/min for 30min at the temperature of 30 ℃, and obtaining a mixed solution D after the reaction is finished;
(5) stirring 1 part of KH560 silane coupling agent in the mixed solution D obtained in the step (4) at a low speed of 200r/min at 30 ℃ for 10min until the mixture is uniform, and obtaining a mixed solution E after the reaction is finished;
(6) and (3) stirring 2 parts of the mixed solution E obtained in the step (5) of sodium hexametaphosphate at a high speed of 400r/min for 20min at the temperature of 30 ℃, and obtaining the waste molasses-based high-performance environment-friendly adhesive after the reaction is finished.
Example 3
A preparation method of a waste molasses-based high-performance environment-friendly adhesive comprises the following steps:
(1) mixing 150 parts of waste molasses, 0.5 part of oxalic acid and 35 parts of distilled water, stirring at a low speed of 180r/min at 80 ℃ for reaction for 2 hours to obtain a mixed solution A after the reaction is finished;
(2) adding 10 parts of ammonium polyphosphate into the mixed solution A obtained in the step (1), stirring at a low speed of 220r/min at 90 ℃ for reaction for 3 hours to obtain a mixed solution B after the reaction is finished;
(3) adding 30 parts of maleic anhydride modified polyethylene into the mixed solution B obtained in the step (2), stirring and reacting at 80 ℃ at the speed of 380r/min for 1h, and obtaining a mixed solution C after the reaction is finished;
(4) after the temperature of the mixed solution C obtained in the step (3) is reduced to 20 ℃, adding 20 parts of silicon dioxide nano powder, stirring at a low speed of 220r/min for 30min, and obtaining a mixed solution D after the reaction is finished;
(5) adding 1 part of KH560 silane coupling agent into the mixed solution D obtained in the step (4), stirring at a low speed of 180r/min at 20 ℃ for 10min until the mixture is uniform, and obtaining a mixed solution E after the reaction is finished;
(6) and (3) adding 1 part of sodium hexametaphosphate into the mixed solution E obtained in the step (5), stirring at a high speed of 400r/min for 20min at the temperature of 20 ℃, and obtaining the waste molasses-based high-performance environment-friendly adhesive after the reaction is finished.
Example 4
A preparation method of a waste molasses-based high-performance environment-friendly adhesive comprises the following steps:
(1) mixing 150 parts of waste molasses, 1 part of oxalic acid and 45 parts of distilled water, stirring at a low speed of 220r/min at 90 ℃ for reaction for 1 hour to obtain a mixed solution A after the reaction is finished;
(2) adding 20 parts of ammonium polyphosphate into the mixed solution A obtained in the step (1), stirring at a low speed of 220r/min at 100 ℃ for reaction for 1h, and obtaining a mixed solution B after the reaction is finished;
(3) adding 40 parts of maleic anhydride modified polyethylene into the mixed solution B obtained in the step (2), stirring and reacting at the temperature of 90 ℃ at the speed of 380r/min for 0.5h, and obtaining a mixed solution C after the reaction is finished;
(4) after the temperature of the mixed solution C obtained in the step (3) is reduced to 30 ℃, adding 40 parts of silicon dioxide nano powder, stirring at a low speed of 220r/min for 30min, and obtaining a mixed solution D after the reaction is finished;
(5) adding 2 parts of KH560 silane coupling agent into the mixed solution D obtained in the step (4), stirring at a low speed of 220r/min at 30 ℃ for 10min until the mixture is uniform, and obtaining a mixed solution E after the reaction is finished;
(6) and (3) adding 2 parts of sodium hexametaphosphate into the mixed solution E obtained in the step (5), stirring at a high speed of 220r/min for 20min at the temperature of 30 ℃, and obtaining the waste molasses-based high-performance environment-friendly adhesive after the reaction is finished.
Comparative example 1
A preparation method of a waste molasses-based high-performance environment-friendly adhesive comprises the following steps:
(1) mixing 150 parts of fructose with 40 parts of distilled water, stirring at a low speed of 180r/min at room temperature for 20min, and obtaining a mixed solution A after the reaction is finished;
(2) stirring 35 parts of maleic anhydride modified polyethylene in the mixed solution A obtained in the step (1) at a low speed of 200r/min at room temperature for reaction for 0.5h to obtain a mixed solution B after the reaction is finished;
(3) stirring 30 parts of the mixed solution B obtained in the step (2) of silicon dioxide nano powder at a low speed of 200r/min for 10min at room temperature, and obtaining a mixed solution D after the reaction is finished;
(4) and (3) stirring 2 parts of the mixed solution C obtained in the step (3) of the KH560 silane coupling agent at a low speed of 200r/min at room temperature for 10min until the mixture is uniform, and obtaining the high-performance environment-friendly adhesive after the reaction is finished.
Comparative example 2
A preparation method of a waste molasses-based high-performance environment-friendly adhesive comprises the following steps:
(1) mixing 150 parts of waste molasses, 1 part of oxalic acid and 40 parts of distilled water, stirring at a low speed of 180r/min at room temperature for 20min, and obtaining a mixed solution A after the reaction is finished;
(2) stirring 15 parts of the mixed solution A obtained in the step (1) of ammonium polyphosphate at a low speed of 180r/min at room temperature for 10min to react to obtain a mixed solution B;
(3) stirring 35 parts of the mixed solution B obtained in the step (2) of maleic anhydride modified polyethylene at a low speed of 200r/min at room temperature for reaction for 0.5h to obtain a mixed solution C after the reaction is finished;
(4) and (3) stirring 1 part of the mixed solution C obtained in the step (3) of sodium hexametaphosphate at a high speed of 400r/min for 20min at room temperature, and obtaining the waste molasses-based high-performance environment-friendly adhesive after the reaction is finished.
The waste molasses-based high-performance environment-friendly adhesive prepared in the examples 1-4 and the comparative examples 1-2 is used for preparing a plywood for performance test, and the preparation of the plywood comprises the following steps:
the eucalyptus plywood is prepared by hot pressing according to the GB/T9846.7-2015 standard, and the technological parameters of the pressing plate are as follows: the adhesive prepared in the examples 1-4 and the comparative examples 1-2 is respectively and uniformly coated on eucalyptus single plates by adopting a manual brushing mode, 3 layers of plywood are assembled based on a vertical texture mode, hot press molding is carried out, and the double-side adhesive applying amount is 180g/m2The hot pressing temperature is 170 ℃, the pressure is 1.3MPa, and the hot pressing time is 7 minutes.
Performance testing and characterization
The wood breakage rate of the eucalyptus plywood prepared by the synthetic adhesive is tested according to a method for determining the wood breakage rate of LY T2720-. The bonding strength of the product meets the related standard of national II-type plywood, and the viscosity is tested by using a rotary viscometer at 25 ℃. The test results are shown in table 1:
table 1 performance test results of eucalyptus plywood prepared in examples and comparative examples
| Dry shear strength MPa | Breaking rate of dried wood% | Wet shear strength MPa | Percentage of wet wood broken% | |
| Example 1 | 1.67 | 100 | 1.38 | 79 |
| Example 2 | 1.62 | 100 | 1.29 | 75 |
| Example 3 | 1.54 | 100 | 1.35 | 76 |
| Example 4 | 1.64 | 100 | 1.33 | 71 |
| Comparative example 1 | 1.06 | 56 | 0.87 | 36 |
| Comparative example 2 | 1.19 | 62 | 0.95 | 40 |
The test results in the above table show that the waste molasses-based high-performance environment-friendly adhesive provided by the invention is used for the plywood, the shear strength and the wood breakage rate of the obtained plywood are obviously improved, the viscosity of the adhesive is moderate, the solid content of the environment-friendly adhesive for the plywood is 86.3-87.5%, the viscosity range is 880-1420mPa & s, the defect that the solid content cannot be improved due to too high viscosity of the traditional natural adhesive for the plywood is overcome, and the heat curing rate and the bonding strength are improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The high-performance environment-friendly waste molasses-based adhesive is characterized by being prepared from the following raw materials in parts by weight:
2. the waste molasses-based high-performance environment-friendly adhesive as claimed in claim 1 is characterized by being prepared from the following raw materials in parts by weight:
3. the waste molasses-based high-performance environment-friendly adhesive as claimed in claim 2, characterized by being prepared from the following raw materials in parts by weight:
4. the waste molasses-based high-performance environment-friendly adhesive as claimed in claim 1, wherein the solid content of the environment-friendly adhesive for plywood is 86.3-87.5%, and the viscosity range is 880-1420mPa · s.
5. The preparation method of the waste molasses-based high-performance environment-friendly adhesive as claimed in any one of claims 1-4, characterized by comprising the following steps:
(1) mixing the waste molasses, oxalic acid and distilled water, stirring at a low speed at a temperature of between 25 and 90 ℃ for reaction for 0.5 to 2 hours, and obtaining a mixed solution A after the reaction is finished;
(2) stirring the mixed solution A obtained in the step (1) of ammonium polyphosphate at a low speed at a temperature of between 25 and 100 ℃ for reaction for 0.5 to 3 hours to obtain a mixed solution B after the reaction is finished;
(3) stirring and reacting the mixed solution B obtained in the step (2) for 0.5-1h at 25-90 ℃ to obtain a mixed solution C after the reaction is finished;
(4) stirring the mixed solution C obtained in the step (3) of the silicon dioxide nano powder at a low speed for 10-30min at 20-30 ℃, and obtaining a mixed solution D after the reaction is finished;
(5) stirring the mixed solution D obtained in the KH560 silane coupling agent step (4) at a low speed for 10min at a temperature of between 20 and 30 ℃ until the mixture is uniform, and obtaining a mixed solution E after the reaction is finished;
(6) and (3) stirring the mixed solution E obtained in the step (5) of sodium hexametaphosphate at a high speed for 20-30min at the temperature of 20-30 ℃, and obtaining the waste molasses-based high-performance environment-friendly adhesive after the reaction is finished.
6. The method as claimed in claim 5, wherein the low-speed stirring is 220r/min and the high-speed stirring is 380-420 r/min.
7. The method as claimed in claim 5, wherein the stirring speed in step (3) is 180-420 r/min.
8. Use of the waste molasses-based high-performance environment-friendly adhesive as claimed in any one of claims 1-4 in the preparation of plywood.
9. Use according to claim 8, characterized in that it comprises the following steps: coating the veneer with an environment-friendly adhesive on a veneer, assembling 3 layers of veneers based on a vertical texture mode, and performing hot press molding, wherein the double-side adhesive applying amount is 140-220g/m2The hot pressing temperature is 130-.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106931A (en) * | 1985-09-12 | 1987-03-11 | 叶禽择 | Adhesional crushed material boards by molasses glue |
| JP2017171818A (en) * | 2016-03-25 | 2017-09-28 | パナソニックＩｐマネジメント株式会社 | Method for producing adhesive, and adhesive |
| KR20180003819A (en) * | 2016-07-01 | 2018-01-10 | 연기호 | Invention of forming binder from Molasses for powder carbon |
| CN108368399A (en) * | 2015-12-18 | 2018-08-03 | 汉高股份有限及两合公司 | Aqueous cementing compositions |
| CN112778955A (en) * | 2021-01-11 | 2021-05-11 | 黄山学院 | Low-cost aqueous adhesive and preparation method thereof |
-
2022
- 2022-01-07 CN CN202210014741.XA patent/CN114350314B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106931A (en) * | 1985-09-12 | 1987-03-11 | 叶禽择 | Adhesional crushed material boards by molasses glue |
| CN108368399A (en) * | 2015-12-18 | 2018-08-03 | 汉高股份有限及两合公司 | Aqueous cementing compositions |
| JP2017171818A (en) * | 2016-03-25 | 2017-09-28 | パナソニックＩｐマネジメント株式会社 | Method for producing adhesive, and adhesive |
| KR20180003819A (en) * | 2016-07-01 | 2018-01-10 | 연기호 | Invention of forming binder from Molasses for powder carbon |
| CN112778955A (en) * | 2021-01-11 | 2021-05-11 | 黄山学院 | Low-cost aqueous adhesive and preparation method thereof |
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