CN113403026B - Aldehyde-free adhesive synthesized from papermaking black liquor and preparation method and application thereof - Google Patents
Aldehyde-free adhesive synthesized from papermaking black liquor and preparation method and application thereof Download PDFInfo
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- CN113403026B CN113403026B CN202110659782.XA CN202110659782A CN113403026B CN 113403026 B CN113403026 B CN 113403026B CN 202110659782 A CN202110659782 A CN 202110659782A CN 113403026 B CN113403026 B CN 113403026B
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- black liquor
- aldehyde
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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
- C09J197/00—Adhesives based on lignin-containing materials
- C09J197/005—Lignin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/002—Manufacture of substantially flat articles, e.g. boards, from particles or fibres characterised by the type of binder
-
- 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
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
Abstract
The invention provides an aldehyde-free adhesive synthesized from papermaking black liquor, which comprises the raw materials of papermaking black liquor, polyvinyl alcohol, oxidized starch, an initiator, a film forming substance and a preservative. The invention utilizes lignosulfonate contained in the papermaking black liquor, and can be used as a raw material of a formaldehyde-free adhesive, thereby avoiding environmental pollution and human body injury caused by formaldehyde in the adhesive. The aldehyde-free adhesive is used for manufacturing artificial boards, and has the characteristics of high adhesive strength, good water resistance, no aldehyde and environmental protection. The invention also provides a preparation method and application of the aldehyde-free adhesive.
Description
Technical Field
The invention relates to the technical field of wood adhesives, in particular to an aldehyde-free adhesive synthesized by papermaking black liquor, a preparation method of the adhesive and application of the adhesive in preparing artificial boards.
Background
Most of the artificial board production in China is applied to furniture manufacturing and interior decoration, and adhesives used for manufacturing various indoor artificial boards are mainly urea-formaldehyde resin adhesives, so that the problem of high free formaldehyde emission is generally solved. The formaldehyde is released continuously from the products made using the urea formaldehyde resin adhesive. Formaldehyde is a toxic gas with strong irritation, which not only pollutes the environment, but also has strong irritation to the eyes, nose, throat and other organs of people, causing the abnormality of lung function, liver function and immune function.
The formaldehyde in the environment polluted by high-concentration formaldehyde can cause various diseases such as throat inflammation, respiratory tract damage and serious carcinogenesis after long-term life. Recent authoritative investigation shows that in cities of China, after the pollutants of a coal smoke type and a photochemical smog type, modern people are trapped in a third-party pollution period of indoor air pollution, and the most serious indoor air pollution is caused by the adhesives, the artificial boards and the coatings in turn. Therefore, the development of environment-friendly adhesives has become a necessary trend and a new hot spot in the field of adhesive research.
The prior art CN110885668A discloses an aldehyde-free adhesive and a preparation method thereof. The formaldehyde-free adhesive comprises the following components in parts by weight: 10 to 40 portions of soybean derivative, 0.1 to 1.5 portions of developing solvent, 80 to 160 portions of water, 0.1 to 0.8 portion of chemical modifier and 0.5 to 2.5 portions of cross-linking agent. The components are easy to obtain, the cost is low, formaldehyde is not contained, and the bonding strength of the formaldehyde-free adhesive is excellent. However, the protein macromolecular structure of the soybean protein needs to be utilized to perform various chemical reactions with the cross-linking agent, and the soybean protein has high cost, so that the popularization and the application of the type of aldehyde-free adhesive are prevented.
The prior art CN 112694582A discloses a method for synthesizing lignin-based phenolic resin adhesive by directly replacing phenol with lignin, which comprises the following steps: (1) Crushing, sieving, washing and drying the raw materials to obtain raw material powder; (2) Adding 50g of raw material powder into 500ml of acidified tetrahydrofurfuryl alcohol, controlling the reaction temperature at 135 ℃ and the reaction time at 90min to obtain a pretreatment material; (3) Carrying out non-woven fabric suction filtration on the pretreated material to obtain filtrate, slowly dripping the filtrate into 2000ml of distilled water, and carrying out sedimentation, centrifugation and drying to obtain lignin; (4) Mixing lignin and phenol to obtain a mixed solution, adding 40ml of sodium hydroxide solution and formaldehyde into the mixed solution, and carrying out two-step reaction to obtain a target product. However, in the method, the raw material needs to be extracted by acidified tetrahydrofurfuryl alcohol, and the obtained high-activity lignin is mixed with phenol to synthesize the lignin-based phenolic resin. Without being able to directly utilize the lignin.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide an aldehyde-free adhesive synthesized by papermaking black liquor.
The second purpose of the invention is to provide a preparation method of the aldehyde-free adhesive.
The third purpose of the invention is to provide the application of the aldehyde-free adhesive in the preparation of artificial boards.
In order to realize the purpose, the technical scheme of the invention is as follows:
the invention relates to an aldehyde-free adhesive synthesized by papermaking black liquor, which comprises the following components: black liquor of paper making, polyvinyl alcohol, oxidized starch, an initiator, a film forming substance and a preservative.
Preferably, the formaldehyde-free adhesive comprises the following components in parts by weight: 55-80 parts of papermaking black liquor, 5-10 parts of polyvinyl alcohol, 5-10 parts of oxidized starch, 1-20 parts of initiator, 5-10 parts of film forming substance and 0.01-0.5 part of preservative.
Preferably, the papermaking black liquor is derived from waste liquor generated in wood papermaking, bagasse papermaking, bamboo papermaking, reed papermaking, straw papermaking and fungus grass papermaking.
Preferably, the papermaking black liquor is distilled and concentrated, water with the mass content of 40% -50% is removed, then the papermaking black liquor is used as a raw material for preparing the aldehyde-free adhesive, and the solid content of the concentrated papermaking black liquor is 20% -45%.
Preferably, the initiator is selected from at least one of persulfates, sulfites, sulfates, phenolic compounds, and aldehydes.
Preferably, the persulfate is at least one selected from potassium persulfate, ammonium persulfate and sodium persulfate, the sulfite is at least one selected from sodium sulfite, potassium sulfite and calcium sulfite, and the sulfate is sodium dodecyl sulfate.
Preferably, the phenolic compound is selected from at least one of resorcinol, phenol, bisphenol a; the aldehyde is formaldehyde.
Preferably, the film forming material is selected from at least one of polyvinyl acetate emulsion, vinyl acetate-acrylic emulsion, styrene-acrylic emulsion and pure acrylic emulsion.
Preferably, the preservative is selected from at least one of borax, pentachlorophenol and zinc oxide.
Preferably, the formaldehyde-free adhesive comprises the following components in parts by weight: 5-8 parts of polyvinyl alcohol, 5-8 parts of oxidized starch, 0.01-0.05 part of persulfate, 5-8 parts of styrene-acrylic emulsion, 0.008-0.015 part of sulfite, 0.01-0.025 part of borax, 0-0.3 part of zinc oxide, 55-80 parts of papermaking black liquor, 1-5 parts of formaldehyde and 0-0.03 part of sodium dodecyl sulfate.
The invention also relates to a preparation method of the aldehyde-free adhesive, which comprises the steps of adding the components into the papermaking black liquor, uniformly stirring to fully mix the components, and then immediately using or storing in a sealed manner.
The invention also relates to application of the aldehyde-free adhesive in preparing artificial boards, wherein the artificial boards comprise plywood, shaving boards and fiber boards.
The invention has the beneficial effects that:
the invention provides an aldehyde-free adhesive synthesized from papermaking black liquor, which comprises the raw materials of papermaking black liquor, polyvinyl alcohol, oxidized starch, an initiator, a film forming substance and a preservative. The invention utilizes the lignosulfonate contained in the papermaking black liquor, and can be used as a raw material of the aldehyde-free adhesive, thereby avoiding environmental pollution and human body injury caused by formaldehyde in the adhesive. The aldehyde-free adhesive is used for manufacturing artificial boards, and has the characteristics of high adhesive strength, good water resistance, no aldehyde and environmental protection.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention relates to an aldehyde-free adhesive synthesized by papermaking black liquor, which comprises the following components: black liquor of paper making, polyvinyl alcohol, oxidized starch, an initiator, a film forming substance and a preservative.
In one embodiment of the invention, the aldehyde-free adhesive comprises the following components in parts by weight: 55-80 parts of papermaking black liquor, 5-10 parts of polyvinyl alcohol, 5-10 parts of oxidized starch, 1-20 parts of initiator, 5-10 parts of film forming substance and 0.01-0.5 part of preservative.
Wherein the papermaking black liquor is derived from waste liquor generated in wood papermaking, bagasse papermaking, bamboo papermaking, reed papermaking, straw papermaking and fungus grass papermaking. The waste liquor produced by the alkaline pulping process of the paper industry is dark brown, so the waste liquor is called black liquor. The black liquor contains a large amount of suspended solids, organic pollutants and toxic substances, and the direct discharge of the black liquor into a water body can cause serious pollution. However, the black liquor also contains a large amount of lignosulfonate, which can be used as a raw material for the aldehyde-free binder.
Because the paper-making black liquor raw pulp has high water content, the invention preferably carries out distillation concentration in advance, namely, water with the mass content of 40-50% is removed, and then the obtained product is used as a raw material for preparing the aldehyde-free adhesive. The solid content of the concentrated papermaking black liquor is 20-45%.
The oxidized starch is a modified starch obtained by oxidizing starch in acid, alkali and neutral media under the action of an oxidizing agent. The oxidized starch reduces the gelatinization temperature of the starch, reduces the viscosity of hot paste and increases the thermal stability, and the oxidized starch is a thickening agent with low viscosity and high concentration and is used for replacing soybean protein.
Because the lignosulfonate contains hydroxymethyl, the lignosulfonate can perform a cross-linking reaction with carboxyl on oxidized starch to form a cross-linked network structure, so that the water-resistant adhesive bonding performance of the aldehyde-free adhesive is enhanced. If lignin is directly used as a raw material, the lignin needs to be degraded at high temperature and high pressure so as to generate a hydroxymethylation reaction, and the content of hydroxymethyl in the lignin is increased.
In one embodiment of the present invention, the initiator is selected from at least one of persulfates, sulfites, sulfates, phenolic compounds, and aldehydes.
Furthermore, the persulfate is selected from at least one of potassium persulfate, ammonium persulfate and sodium persulfate, the sulfite is selected from at least one of sodium sulfite, potassium sulfite and calcium sulfite, and the sulfate is sodium dodecyl sulfate. Because the single persulfate is not suitable for reaction initiation, and the persulfate and the sulfate are jointly used to form a redox system, free radicals are generated through redox reaction, and the whole process only involves the transfer of free electrons, the reaction activation energy is low, and the method is suitable for reaction at low temperature. On the basis, the sulfate is added, so that the starch molecules can be depolymerized, active groups in the molecules are exposed, the crosslinking reaction is facilitated, and meanwhile, the initiator is added, so that the temperature is slowly increased, a more compact crosslinking network is obtained, and the bonding strength of the adhesive is improved.
In one embodiment of the present invention, the phenolic compound is selected from at least one of resorcinol, phenol, bisphenol a; the aldehyde is formaldehyde. Because the addition amount of formaldehyde as an initiator is less, the formaldehyde is consumed after reaction and cannot be remained in the adhesive.
In one embodiment of the present invention, the film forming material is at least one selected from the group consisting of polyvinyl acetate emulsion, vinyl acetate-acrylic emulsion, styrene-acrylic emulsion, and acrylic emulsion. The film-forming material is capable of adhering to a material to form a film, mainly contains a polymer resin and water, and can be also called as an aqueous emulsion, wherein the solid content is 40-60wt%.
In one embodiment of the invention, the preservative is selected from at least one of borax, pentachlorophenol, zinc oxide.
In one embodiment of the invention, the aldehyde-free adhesive comprises the following components in parts by weight: 5-8 parts of polyvinyl alcohol, 5-8 parts of oxidized starch, 0.01-0.05 part of persulfate, 5-8 parts of styrene-acrylic emulsion, 0.008-0.015 part of sulfite, 0.01-0.025 part of borax, 0-0.3 part of zinc oxide, 55-80 parts of papermaking black liquor, 1-5 parts of formaldehyde and 0-0.03 part of sodium dodecyl sulfate.
The embodiment of the invention also relates to a preparation method of the aldehyde-free adhesive, which comprises the steps of adding the components into the papermaking black liquor, uniformly stirring to fully mix the components, and then immediately using or hermetically storing. Specifically, the preparation method comprises the steps of adding the components except the papermaking black liquor into the papermaking black liquor, uniformly stirring, heating to 70-95 ℃, reacting for 1-3 hours, cooling to 30-60 ℃, discharging and packaging.
The embodiment of the invention also relates to application of the aldehyde-free adhesive in preparing the artificial board. The artificial board is a plate or a molded product which is made by taking wood or other non-wood plants as raw materials, separating the raw materials into various unit materials through certain mechanical processing and then gluing the unit materials with or without adhesive and other additives. The preparation method comprises the steps of cutting and drying the veneers, the wood chips and the wood shavings, then gluing, forming and pressurizing to obtain the required board.
The artificial board comprises plywood, shaving board and fiberboard.
The plywood is a board which is made by rotary cutting steamed and softened log into large sheets, then bonding the large sheets by synthetic resin adhesive with good water resistance, pressurizing, drying, sawing edges and finishing the surface. The number of layers is odd, and is generally 3-13, which are called three-ply board, five-ply board, etc. The wood used for making plywood includes basswood, birch, water ash, beech, colored wood, eucalyptus, etc.
The fiberboard is a board prepared by crushing, soaking and grinding waste materials such as barks, wood shavings, branches and the like into wood pulp, and then carrying out pressure forming and drying treatment. The molding temperature and pressure are different, so that the molding can be divided into three types, namely hard, semi-hard and soft.
Particle board is a board pressed from wood shavings or wood fiber stock with or without size applied. The shaving board has low density, uniform material quality, easy moisture absorption and low strength.
Example 1
An aldehyde-free adhesive synthesized from papermaking black liquor comprises the following components in parts by weight: 5 parts of polyvinyl alcohol, 5 parts of oxidized starch, 0.01 part of sodium persulfate, 5 parts of styrene-acrylic emulsion, 0.008 part of sodium sulfite, 0.01 part of borax, 55 parts of papermaking black liquor and 1 part of formaldehyde.
Adding the components into the papermaking black liquor, uniformly stirring, heating to 85 ℃, reacting for 1.5 hours, cooling to 30 ℃, discharging and packaging.
Example 2
An aldehyde-free adhesive synthesized from papermaking black liquor comprises the following components in parts by weight: 8 parts of polyvinyl alcohol, 8 parts of oxidized starch, 0.05 part of sodium persulfate, 8 parts of styrene-acrylic emulsion, 0.015 part of sodium sulfite, 0.025 part of borax, 0.3 part of zinc oxide, 80 parts of papermaking black liquor, 3 parts of formaldehyde and 0.03 part of sodium dodecyl sulfate.
The procedure was as in example 1.
Example 3
An aldehyde-free adhesive synthesized from papermaking black liquor comprises the following components in parts by weight: 6 parts of polyvinyl alcohol, 6 parts of oxidized starch, 0.03 part of sodium persulfate, 6 parts of styrene-acrylic emulsion, 0.010 part of sodium sulfite, 0.015 part of borax, 0.15 part of zinc oxide, 60 parts of papermaking black liquor, 5 parts of formaldehyde and 0.15 part of sodium dodecyl sulfate.
The procedure was as in example 1.
The papermaking black liquor of the above embodiment is from Yinlu Fuke technology, inc. of Shinming city, sanming province, and the solid content after evaporation concentration is 30-35%.
Comparative examples 1 to 5 were obtained by changing the raw materials and the amounts used based on example 3. The specific settings are shown in table 1.
TABLE 1
| Examples | Changed raw materials and dosage |
| Comparative example 1 | Oxidized starch was replaced with soybean flour, and other raw materials and amounts were the same as in example 3 |
| Comparative example 2 | Sodium persulfate was replaced with sodium sulfite, and the other raw materials and amounts were the same as in example 3 |
| Comparative example 3 | Sodium sulfite was replaced with sodium persulfate, and the other raw materials and amounts were the same as in example 3 |
| Comparative example 4 | No sodium lauryl sulfate was used, and the other raw materials and amounts were the same as in example 3 |
| Comparative example 5 | The black liquor is not concentrated, and other raw materials and the using amount are the same as those in example 3 |
Test example
The aldehyde-free adhesives prepared in the above examples and comparative examples are mixed with wood fibers according to the mass ratio of 1. Then placing the mixture into a hot-pressing mold frame, and paving the mixture uniformly and flatly. And cold pressing for 20s to form, then hot pressing for 8min at the temperature of 180-230 ℃ and under the pressure of 6MPa, and relieving pressure and cooling to obtain the medium-density fiberboard. The mechanical property and formaldehyde emission of the board are detected according to the method specified in the national standard GB/T11718-2009 Density fiberboard in a dry state. The mechanical properties include static bending strength, elastic modulus, internal bonding strength and water absorption thickness expansion rate.
The medium density fiberboard of example 3 had a density of 0.86g/cm 3 The static bending strength is 44.4MPa, the elastic modulus is 2965MPa, the internal bonding strength is 1.66MPa, the water absorption thickness expansion rate is 11.5 percent, and the formaldehyde release amount is 0mg/100g.
The test results for examples 1 and 2 are similar to example 3. The test results of comparative examples 1 to 5 were all lower than those of the examples.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. The aldehyde-free adhesive synthesized from the papermaking black liquor is characterized by comprising the following components in parts by weight: the paint comprises the following components in parts by weight: 6 parts of polyvinyl alcohol, 6 parts of oxidized starch, 0.03 part of sodium persulfate, 6 parts of styrene-acrylic emulsion, 0.010 part of sodium sulfite, 0.015 part of borax, 0.15 part of zinc oxide, 60 parts of papermaking black liquor, 5 parts of formaldehyde and 0.15 part of sodium dodecyl sulfate;
the papermaking black liquor is from Yuanjian Yuankagao, fuke technology, inc., of san Ming city, fujian province, and the solid content is 30-35% after evaporation and concentration.
2. The method for preparing the aldehyde-free adhesive according to claim 1, wherein the components are added into the papermaking black liquor, stirred uniformly, heated to 85 ℃, reacted for 1.5 hours, cooled to 30 ℃, discharged and packaged.
3. Use of the aldehyde-free adhesive of claim 1 in the preparation of artificial boards, including plywood, particle board, and fiber board.
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| CN202110659782.XA CN113403026B (en) | 2021-06-15 | 2021-06-15 | Aldehyde-free adhesive synthesized from papermaking black liquor and preparation method and application thereof |
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| CN113403026B true CN113403026B (en) | 2023-01-31 |
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Citations (7)
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| CN101092550A (en) * | 2007-07-27 | 2007-12-26 | 邹炎 | Adhesive prepared from paper making black liquor for forming active carbon |
| CN101191039A (en) * | 2006-11-20 | 2008-06-04 | 兰州大学 | Method for preparing paper-making black liquor adhesive |
| CN101191038A (en) * | 2006-11-20 | 2008-06-04 | 兰州大学 | Method for preparing paper-making black liquor adhesive |
| CN105018011A (en) * | 2015-08-21 | 2015-11-04 | 广西星岛科技发展有限公司 | Adhesive synthesized by using papermaking black liquor as raw material and production method thereof |
| CN106281157A (en) * | 2016-08-29 | 2017-01-04 | 南宁市创锦胶合板有限责任公司 | Moistureproof composite urea formaldehyde resin and production method thereof |
| CN109517579A (en) * | 2018-11-22 | 2019-03-26 | 丰禾新材（北京）技术有限公司 | Adhesive and fiberboard preparation method |
| CN111394025A (en) * | 2020-04-03 | 2020-07-10 | 秾源科技(北京)有限公司 | Method for preparing environment-friendly adhesive from chemi-mechanical pulp pulping waste liquid |
-
2021
- 2021-06-15 CN CN202110659782.XA patent/CN113403026B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101191039A (en) * | 2006-11-20 | 2008-06-04 | 兰州大学 | Method for preparing paper-making black liquor adhesive |
| CN101191038A (en) * | 2006-11-20 | 2008-06-04 | 兰州大学 | Method for preparing paper-making black liquor adhesive |
| CN101092550A (en) * | 2007-07-27 | 2007-12-26 | 邹炎 | Adhesive prepared from paper making black liquor for forming active carbon |
| CN105018011A (en) * | 2015-08-21 | 2015-11-04 | 广西星岛科技发展有限公司 | Adhesive synthesized by using papermaking black liquor as raw material and production method thereof |
| CN106281157A (en) * | 2016-08-29 | 2017-01-04 | 南宁市创锦胶合板有限责任公司 | Moistureproof composite urea formaldehyde resin and production method thereof |
| CN109517579A (en) * | 2018-11-22 | 2019-03-26 | 丰禾新材（北京）技术有限公司 | Adhesive and fiberboard preparation method |
| CN111394025A (en) * | 2020-04-03 | 2020-07-10 | 秾源科技(北京)有限公司 | Method for preparing environment-friendly adhesive from chemi-mechanical pulp pulping waste liquid |
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