CN110257005B - Formaldehyde-free flour-based adhesive and preparation method thereof - Google Patents
Formaldehyde-free flour-based adhesive and preparation method thereof Download PDFInfo
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- CN110257005B CN110257005B CN201910667912.7A CN201910667912A CN110257005B CN 110257005 B CN110257005 B CN 110257005B CN 201910667912 A CN201910667912 A CN 201910667912A CN 110257005 B CN110257005 B CN 110257005B
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- 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
- C09J199/00—Adhesives based on natural macromolecular compounds or on derivatives thereof, not provided for in groups C09J101/00 -C09J107/00 or C09J189/00 - C09J197/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Veneer Processing And Manufacture Of Plywood (AREA)
Abstract
The invention discloses an aldehyde-free flour-based adhesive and a preparation method thereof, wherein the aldehyde-free flour-based adhesive comprises the following components in parts by weight: 38-42 parts of main agent, 60 parts of dispersion medium water, 0.4-0.8 part of reinforcing agent, 0.1-0.3 part of viscosity regulator, 8-12 parts of cross-linking agent and 0.5-1 part of catalyst; the preparation method comprises the following steps: weighing the components according to the weight ratio, adding the reinforcing agent into dispersion medium water, carrying out ultrasonic treatment for 15 minutes, then adding half weight of the main agent, and carrying out homogeneous emulsification for 20 minutes by using a high-pressure homogenizer under the pressure of 30MPa and the emulsifying force of 0.5 MPa; adding the rest main agent into the obtained mixture, uniformly mixing, adding the cross-linking agent and the rest catalyst, reacting at 80 ℃ for 30min, cooling to 30 ℃, and discharging; the adhesive disclosed by the invention is easy to form a cross-linked structure, high in cross-linking density, low in reaction temperature, simple in preparation method, stable in prepared adhesive performance, obviously reduced in weak interface layer, reduced in cost, good in dry/wet strength and stably improved in product quality.
Description
Technical Field
The invention relates to the field of plywood preparation, in particular to an aldehyde-free flour-based adhesive and a preparation method thereof.
Background
The precious wood resources in China are relatively deficient, the artificial forest resources are rich, the artificial boards prepared from the fast growing wood of the artificial forest through the adhesive are main raw materials for furniture floors and indoor decoration in human living environments, in 2017, the total yield of the artificial boards in China is 2.95 billion cubic meters, which accounts for 50% of the total world yield, and more than 60% of the artificial boards are plywood products. Calculated by producing 9 cubic meters of artificial boards per ton of adhesive on average, the consumption of the adhesive for the plywood in 2017 in China is about 1800 ten thousand tons (solid content is 50%), wherein the urea-formaldehyde resin and modified products thereof account for more than 90% of the total output of the adhesive and dominate. The urea-formaldehyde resin adhesive is widely used in the wood industry due to the advantages of sufficient raw materials, low price, good water solubility and the like, but has the problem of formaldehyde release of products.
With the improvement of living standard of people, the problem of human living environmental pollution is concerned, the problem of the release amount of free formaldehyde of the artificial board can be solved by adopting the biomass adhesive, the artificial board is an important way for solving the problem, but most biomass adhesives have the problem of poor water-resistant adhesive bonding performance, and the industrial application of the biomass adhesive is limited.
Disclosure of Invention
The invention overcomes the defects of the prior art, and provides the aldehyde-free flour-based adhesive and the preparation method thereof.
In order to achieve the purpose, the first technical scheme adopted by the invention is as follows: the formula of the aldehyde-free flour-based adhesive comprises the following components in parts by weight:
38-42 parts of main agent, 60 parts of dispersion medium water, 0.4-0.8 part of reinforcing agent, 0.1-0.3 part of viscosity regulator, 8-12 parts of cross-linking agent and 0.5-1 part of catalyst.
In a preferred embodiment of the invention, the main agent is modified flour, the flour protein content is 7.2% by mass, and the grain sizes are all 50-80 meshes.
In a preferred embodiment of the invention, the reinforcing agent is surface-modified nano attapulgite.
In a preferred embodiment of the present invention, the viscosity modifier is polyacrylamide, anion, and has an average molecular weight of 1800 ten thousand.
In a preferred embodiment of the present invention, the crosslinking agent is a self-made polyfunctional epoxy compound.
In a preferred embodiment of the invention, the catalyst is 50% sodium hydroxide solution by mass fraction.
In a preferred embodiment of the invention, the dispersion medium water is selected from common tap water or softened water.
The second technical scheme adopted by the invention is as follows: a preparation method of the aldehyde-free flour-based adhesive comprises the following steps:
(1) weighing the components according to the weight ratio, adding the reinforcing agent into dispersion medium water, carrying out ultrasonic treatment for 15 minutes, uniformly dividing the main agent of the weighed components into two parts, adding one part of the main agent, and carrying out homogeneous emulsification for 20 minutes by using a high-pressure homogenizer under the pressure of 30MPa and the emulsifying force of 0.5 MPa;
(2) and (2) adding the rest of the main agent into the mixture obtained in the step (1), uniformly mixing, adding the cross-linking agent and the rest of the catalyst, reacting at 80 ℃ for 30min, cooling to 30 ℃, and discharging.
In a preferred embodiment of the present invention, the primary agent is modified flour, 35 parts by weight of flour is mixed with 65 parts by weight of water, the pH is adjusted to 4.8, 10 parts by weight of sodium periodate is added, and the mixture is reacted at 55 ℃ for 3 hours to obtain the primary treatment liquid A. Reacting 0.8mol of succinic anhydride, 0.1mol of phthalic acid and 1mol of diethylenetriamine at 160 ℃ for 1 hour, then distilling the water at 160 ℃ under negative pressure for 3 hours, cooling to 110 ℃, and adding water to adjust to a 60% solution, namely B; mixing the components in parts by weight of A: B =1:1.2, adjusting the pH value to 9, reacting for 1 hour at normal temperature, heating to 60 ℃ for reacting for 20 minutes, and then spray-drying or concentrating to obtain the modified flour.
In a preferred embodiment of the invention, the reinforcing agent is nano-attapulgite, 10gKH560 is dissolved in 40g of alcohol, 10g of nano-attapulgite is added, ultrasonic dispersion is carried out for 20 minutes, the pH value of the solution is adjusted to be 3.8, the reaction is carried out for 2 hours at 80 ℃, centrifugal cleaning is carried out, and the reinforcing agent is obtained by drying.
In a preferred embodiment of the invention, the cross-linking agent is a self-made polyfunctional epoxy compound, 230 parts by weight of ammonia water is dripped into 280g of epoxy chloropropane at the temperature of 55 ℃, the temperature of the reaction solution is kept between 50 and 60 ℃, 2 parts by weight of sodium carbonate is added as a catalyst when the pH is reduced to 6.5 after the dripping is finished, the reaction is stopped after the reaction temperature is not raised for 2 hours at the temperature of between 70 and 80 ℃, and the reaction is cooled and discharged.
In a preferred embodiment of the invention, the chemical reagent matching treatment method can effectively increase reactive groups in the flour and enhance the rigidity of the cross-linking agent, so that the cross-linking agent and the flour can form a hyperbranched rigid cross-linked structure, the attapulgite can be combined into the cross-linked structure by chemical bonds, and the waterproof adhesive bonding performance of the adhesive is further improved by stress conduction and dispersion.
The invention solves the defects in the background technology, and has the following beneficial effects:
(1) according to the invention, phthalic acid is adopted to prepare the hyperbranched amino polymer with a rigid structure, and the grafted modified flour is used as a main agent, so that the activity of the flour is improved, and a branched crosslinking structure can be formed to improve the water-resistant bonding performance of the adhesive.
(2) The surface-modified fiber rod-shaped nano attapulgite is utilized to uniformly mix the nano attapulgite with a flour system, and a rod-shaped high-strength structure of the attapulgite and a relatively soft structure of a flour matrix form chemical bond connection, so that a structure with separated hardness and hardness is formed, and stress balance and improvement of the adhesive property of prepared plywood are facilitated.
(3) The modified nano-attapulgite is uniformly dispersed by utilizing a high-pressure homogenizing process, and spherical aggregates of protein and starch in the flour can be opened, so that the contact area between the modified nano-attapulgite and a cross-linking agent is increased, the performance can be synergistically improved, and the uniform and stable adhesive system is facilitated.
(4) The cross-linking agent disclosed by the invention is simple in synthesis process, efficient and water-soluble, raw materials can be derived from biomass resources, the cross-linking agent is compatible with nano-attapulgite, modified flour and other components, a chemical reaction is carried out at a lower temperature, the rigidity of an adhesive cross-linking structure is effectively improved by the introduced rigid structure, and the cross-linking agent can better react with flour under the catalytic action of sodium hydroxide, so that the cross-linking density of the adhesive is improved, the bonding performance is enhanced, the uniformity of the adhesive is good, and the technological performance of the adhesive is good.
(5) The pre-reaction process in the invention can effectively improve the molecular weight of the adhesive system, improve the prepressing performance and the cementing performance of the adhesive, reduce the hot-pressing temperature and time of the adhesive and enhance the manufacturability of the adhesive.
(6) The flour adhesive is synthesized from nano attapulgite, an environment-friendly cross-linking agent and modified flour without adding toxic substances, has high efficiency, no release of harmful substances, high reaction activity of products, good manufacturability and low cost, and can be industrially applied.
(7) The adhesive disclosed by the invention is easy to form a cross-linked structure, high in cross-linking density, low in reaction temperature, stable in performance of the prepared adhesive, good in dry/wet strength and stable and improved in product quality, and a weak interface layer is obviously reduced, and the cost is reduced.
Detailed Description
The present invention will now be described in further detail with reference to examples, which are provided to illustrate the present invention but are not intended to limit the scope of the present invention. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention.
Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Further, all the component materials used in the examples are known commercially available products.
The percent in the present invention means mass percent unless otherwise specified; but the percentage of the solution, unless otherwise specified, means that 100ml of the solution contains several grams of solute; the percentage between the liquids refers to the ratio of the volumes at 20 ℃.
The formula of the aldehyde-free flour-based adhesive comprises the following components in parts by weight:
38-42 parts of main agent, 60 parts of dispersion medium water, 0.4-0.8 part of reinforcing agent, 0.1-0.3 part of viscosity regulator, 8-12 parts of cross-linking agent and 0.5-1 part of catalyst.
The main agent is modified flour, the protein content of the flour is 7.2 percent by mass, the grain diameters are all 50-80 meshes, and the flour can be purchased in the market, such as from Beijing ancient boat food Co., Ltd; the reinforcing agent is surface-modified nano attapulgite; the viscosity regulator is polyacrylamide, anion and has the average molecular weight of 1800 ten thousand, and can be purchased from Ningquan chemical Co., Ltd; the cross-linking agent is a self-made polyfunctional epoxy compound; the catalyst is 50 percent of sodium hydroxide solution in mass fraction, is a commercial product and can be purchased from Tianjin chemical Co.Ltd; the dispersion medium water is selected from common tap water or softened water.
Example 1
The embodiment provides a preparation method of a flour adhesive, which comprises the following steps of preparing materials according to the following weight ratio:
38 kg of modified flour
Surface-modified Attapulgite 0.4 kg
0.1kg of polyacrylamide
Self-made 8kg of polyfunctional epoxy compound
0.5kg of sodium hydroxide solution
The embodiment also provides a preparation method of the adhesive, which comprises the following specific preparation steps:
(1) weighing the components according to the weight ratio, adding the surface modified attapulgite into dispersion medium water, performing ultrasonic treatment for 15 minutes, then adding half weight of modified flour, and performing homogeneous emulsification for 20 minutes by using a high-pressure homogenizer under the pressure of 30MPa and the emulsifying force of 0.5 MPa;
(2) adding the rest modified flour into the mixture obtained in the step (1), uniformly mixing, adding the self-made multifunctional epoxy compound and the rest sodium hydroxide solution, reacting at 80 ℃ for 30min, cooling at 30 ℃ and discharging.
Example 2
The embodiment provides a preparation method of a flour adhesive, which comprises the following steps of preparing materials according to the following weight ratio:
42kg of modified flour
Surface-modified Attapulgite 0.8 kg
0.3kg of polyacrylamide
Self-made polyfunctional epoxy compound 12kg
1.0kg of sodium hydroxide solution
The preparation method of the adhesive in this embodiment is the same as that in embodiment 1.
Comparative example 1
The comparative example provides a preparation method of a flour adhesive, wherein the adhesive is prepared according to the following weight ratio:
common flour 42kg
Surface-modified Attapulgite 0.8 kg
0.3kg of polyacrylamide
Self-made polyfunctional epoxy compound 12kg
1.0kg of sodium hydroxide solution
The preparation method of the adhesive in the comparative example is the same as that in example 1.
Comparative example 2
The comparative example provides a preparation method of a flour adhesive, wherein the adhesive is prepared according to the following weight ratio:
common flour 42kg
Surface-modified Attapulgite 0.8 kg
0.3kg of polyacrylamide
1.0kg of sodium hydroxide solution
The preparation method of the adhesive in the comparative example is the same as that in example 1.
Comparative example 3
The comparative example provides a preparation method of a flour adhesive, wherein the adhesive is prepared according to the following weight ratio:
common flour 42kg
0.3kg of polyacrylamide
Self-made polyfunctional epoxy compound 12kg
1.0kg of sodium hydroxide solution
The preparation method of the adhesive in the comparative example is the same as that in example 1.
Comparative example 4
Control 4 was a conventional E0 grade urea formaldehyde resin adhesive.
Comparative examples 1 to 4 were compared with examples 1 to 2, respectively, and comparative example 1 was plain flour, otherwise the same as example 2; control 2 was example 2 without crosslinker; control 3 was example 2 without enhancer; control 4 was a conventional E0 grade urea formaldehyde resin adhesive.
Test examples
Three-layer plywood was prepared by using the adhesives of examples 1-2 and comparative examples 1-4 of the present invention, respectively.
Poplar veneer: drying to 10% of water content; size 40cm by 0.15 cm.
The preparation method comprises the following normal preparation processes:
sizing: the glue coating amount is 400g/m2。
Pressure, temperature, time: 0.8MPa, 115 ℃ for 6 minutes.
The performance of the transverse spliced product is detected according to the detection method of GB/T17657-1999 test method for physical and chemical properties of artificial boards and facing artificial boards, and the detection result is shown in Table 2.
TABLE 1 plywood bond Strength
The experimental result shows that the bonding strength of the plywood prepared from the flour-based adhesive is more than 1.20MPa and the dry strength is more than 1.6 according to the detection of a II plywood, and the standard deviation calculation shows that the stability of the adhesive prepared from the flour adhesive is obviously improved and the reinforcing effect is obvious.
In light of the foregoing description of the preferred embodiment of the present invention, it is to be understood that various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (3)
1. The aldehyde-free flour-based adhesive comprises the following components in parts by weight:
38-42 parts of main agent, 60 parts of dispersion medium water, 0.4-0.8 part of reinforcing agent, 0.1-0.3 part of viscosity regulator, 8-12 parts of cross-linking agent and 0.5-1 part of catalyst; the main agent is modified flour, the flour protein content is 7.2% by mass, and the grain sizes are 50-80 meshes; the reinforcing agent is surface-modified nano attapulgite; the viscosity regulator is polyacrylamide; the cross-linking agent is a self-made polyfunctional epoxy compound, 230 parts by weight of ammonia water is dripped into 280g of epoxy chloropropane at the temperature of 55 ℃, the temperature of the reaction liquid is kept between 50 and 60 ℃, 2 parts by weight of sodium carbonate is added as a catalyst when the pH value is reduced to 6.5 after the dripping is finished, the reaction is stopped after the reaction temperature is not raised for 2 hours at the temperature of between 70 and 80 ℃, and the temperature is reduced and the material is discharged; the catalyst is 50% sodium hydroxide solution by mass fraction; the main agent is modified flour, 35 parts by weight of flour and 65 parts by weight of water are mixed, the pH value is adjusted to be 4.8, 10 parts by weight of sodium periodate is added, the mixture reacts for 3 hours at 55 ℃ to obtain an initial treatment solution A, 0.8mol of succinic anhydride, 0.1mol of phthalic acid and 1mol of diethylenetriamine react for 1 hour at 160 ℃, then the mixture is distilled under negative pressure at 160 ℃ for 3 hours, the temperature is reduced to 110 ℃, and water is added to adjust the mixture to be a 60% solution B; mixing the components in parts by weight of A: B =1:1.2, adjusting the pH value to 9, reacting for 1 hour at normal temperature, heating to 60 ℃ for reacting for 20 minutes, and performing spray drying or concentration to obtain the modified flour.
2. The method of making the aldehyde-free flour-based adhesive of claim 1, comprising the steps of:
(1) weighing the components according to the weight ratio, adding the reinforcing agent into dispersion medium water, carrying out ultrasonic treatment for 15 minutes, uniformly dividing the main agent of the weighed components into two parts, adding one part of the main agent, and carrying out homogeneous emulsification for 20 minutes by using a high-pressure homogenizer under the pressure of 30MPa and the emulsifying force of 0.5 MPa;
(2) and (2) adding the rest of the main agent into the mixture obtained in the step (1), uniformly mixing, adding the cross-linking agent and the rest of the catalyst, reacting at 80 ℃ for 30min, cooling to 30 ℃, and discharging.
3. The method of preparing the aldehyde-free flour-based adhesive of claim 2, wherein: the reinforcing agent is nano-attapulgite, 10gKH560 is dissolved in 40g of alcohol, 10g of nano-attapulgite is added, ultrasonic dispersion is carried out for 20 minutes, the pH value of the solution is adjusted to be 3.8, the reaction is carried out for 2 hours at 80 ℃, and the reinforcing agent is obtained by centrifugal cleaning, drying or concentration.
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| CN201910667912.7A CN110257005B (en) | 2019-07-23 | 2019-07-23 | Formaldehyde-free flour-based adhesive and preparation method thereof |
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| CN106085289A (en) * | 2016-07-26 | 2016-11-09 | 明辉大秦（上海）环保科技有限公司 | Environment-friendly type corrugated board low temperature laminating starch adhesive and preparation method thereof |
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Effective date of registration: 20230629 Address after: 273401 Qiansen Wood Industry, Shangye Town Industrial Park, Fei County, Linyi City, Shandong Province Patentee after: Shandong fortune Wood Industry Group Co.,Ltd. Address before: 100083 No. 35 Qinghua East Road, Beijing, Haidian District Patentee before: BEIJING FORESTRY University |