CN115491173A - Lignin sodium sulfonate-urea formaldehyde precondensate-urea synthesized modified urea formaldehyde resin wood adhesive and preparation method thereof - Google Patents
Lignin sodium sulfonate-urea formaldehyde precondensate-urea synthesized modified urea formaldehyde resin wood adhesive and preparation method thereof Download PDFInfo
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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
- C09J187/00—Adhesives based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
Abstract
The invention discloses a lignin sodium sulfonate-urea formaldehyde precondensate liquid-urea synthesis modified urea formaldehyde resin wood adhesive, which is synthesized by taking lignin sodium sulfonate, urea formaldehyde precondensate liquid and urea as main raw materials and sodium hydroxide and formic acid or acetic acid as catalysts through an alkali-acid-alkali synthesis process through a copolycondensation reaction; wherein the mass ratio of the sodium lignosulphonate to the urea is 0.21-0.40, the molar ratio of the formaldehyde to the urea in the urea formaldehyde pre-condensation liquid is 6:1, and the final molar ratio of the formaldehyde to the urea is 1.2. Accordingly, a corresponding preparation method is also established. Compared with the earlier research, the invention increases the dosage of sodium lignosulfonate, changes the molar ratio of formaldehyde to urea in the urea formaldehyde precondensate, reduces the molar ratio of formaldehyde to urea, but has similar performance and longer storage period compared with pure Urea Formaldehyde (UF) resin, and can be widely applied to the industry of artificial boards. In a word, the invention has simple process and excellent comprehensive performance, and improves the operability in the actual production of the plywood.
Description
Technical Field
The invention belongs to the field of wood adhesives and high polymer materials in artificial board production, and particularly relates to a lignin sodium sulfonate-urea formaldehyde precondensate-urea synthesized modified urea formaldehyde resin wood adhesive and a preparation method thereof.
Background
UF resins (urea-formaldehyde resins) are prepared by transporting formaldehyde solutions to plants and then adding urea in batches for synthesis. In the resin synthesis process, formaldehyde in a glue making workshop is harmful to human bodies greatly, because the formaldehyde has serious stimulation on eyes, mucous membranes and respiratory tracts of the human bodies. In addition, during the subsequent use of the wood composite product, the wood composite product can continuously release formaldehyde to the outside, thus being harmful to human health. Therefore, the urea-formaldehyde resin adhesive synthesized by using the urea-formaldehyde precondensate is proposed by Li Jianzhang (the development direction of the raw material of the urea-formaldehyde resin for the artificial board industry, namely UFC (high concentration formaldehyde) is J48-51 and 2007-01-18 in the forest industry) for many years, so that the transportation cost can be saved, the self-polymerization of the formaldehyde can be prevented, and the low-temperature storage stability of the formaldehyde can be improved.
The lignosulfonate is a main component of black liquor produced by pulping by a sulfite method, the pulping black liquor produced by papermaking in China is more than 450 million tons every year, the utilization rate of the lignosulfonate is less than 10 percent, and how to efficiently utilize lignin and derivatives thereof becomes a research hotspot in multiple fields. The sodium lignosulfonate-urea-formaldehyde precondensate liquid-urea copolycondensation resin (SLUF) wood adhesive is a copolycondensation resin adhesive which is synthesized by using sodium lignosulfonate, urea-formaldehyde precondensate liquid and urea as main raw materials through an alkali-acid-alkali process. Compared with pure UF resin, the SLUF resin has equivalent mechanical property, good storage period and lower free formaldehyde content; and the cheap sodium lignosulfonate is used for replacing urea at a high ratio, is used for the wood adhesive industry for producing artificial boards, and can give consideration to both cost and environmental protection. Therefore, it is of great significance to intensively study the SLUF resin adhesive.
The inventor carries out preliminary research on the preparation of the modified urea-formaldehyde resin wood adhesive by using sodium lignosulfonate-urea formaldehyde pre-condensed liquid-urea in synthesis and characterization of UFC-sodium lignosulfonate-based modified urea-formaldehyde resin (forest industry, 2021, 58 (04): 53-58) and UFC-sodium lignosulfonate copolycondensation resin in kinetics of curing and thermal performance analysis (university of Guilin institute of technology, 2021,41 (4): 851-857).
Disclosure of Invention
The invention aims to solve the technical problem of providing a lignin sodium sulfonate-urea formaldehyde precondensate solution-urea synthesized modified urea formaldehyde resin wood adhesive with simple process and excellent comprehensive performance and a preparation method thereof.
In order to solve the technical problem, the invention adopts the following technical scheme:
sodium lignosulfonate-urea-formaldehyde precondensate solution-urea synthesis modified urea-formaldehyde resin wood adhesive (SLUF) is synthesized by taking sodium lignosulfonate, urea-formaldehyde precondensate solution and urea as main raw materials and sodium hydroxide and formic acid or acetic acid as catalysts through an alkali-acid-alkali synthesis process through a copolycondensation reaction; wherein the mass ratio of the sodium lignosulphonate to the urea is 0.21-0.40, the molar ratio of the formaldehyde to the urea in the urea formaldehyde pre-condensation liquid is 6:1, and the molar ratio of the formaldehyde to the urea is 1.2.
The adhesive is dark brown liquid, the content of free formaldehyde is 0.10-0.21%, the content of solid is 47.0-53.0%, the pH value is 7.0-8.0, the viscosity is 17.0-20.0 s (coating in a 4 cup, 30 ℃), the storage period is 30-60 days, and the bonding strength is more than or equal to 0.70Mpa (meeting the standard of national II-type plywood).
The preparation method of the synthetic modified urea-formaldehyde resin wood adhesive adopts distilled water, sodium hydroxide, paraformaldehyde and urea to prepare colorless and transparent urea-formaldehyde pre-condensate; the prepared urea formaldehyde pre-condensed liquid, sodium lignin sulfonate and urea are subjected to copolycondensation reaction under the condition of a catalyst.
The preparation method comprises the following steps of:
(1) Adding 2160.0 parts of 50 mass percent formaldehyde solution into a reaction kettle, starting a stirrer, adjusting the pH to 8.0-9.0 by using an alkali solution, heating to 90 ℃, uniformly dividing 360.0 parts of urea into three batches, adding the three batches of urea into the reaction kettle, reacting until the solution is clear and transparent, cooling to room temperature, adding distilled water to adjust the 50 percent formaldehyde solution into 37 percent formaldehyde solution, and blanking to obtain colorless and transparent urea-formaldehyde precondensate solution (UFC), wherein the molar ratio of formaldehyde to urea in the urea-formaldehyde precondensate solution is 6:1;
(2) Adding 291.9 parts of urea formaldehyde pre-condensation liquid and 37.8-72.0 parts of sodium lignosulfonate into a reaction kettle, starting a stirrer, adjusting the pH to 8.0-9.0 by using an alkali solution, and then adding 97.2 parts of first urea (U) 1 ) Programmed heating to 88 deg.C, keeping the temperature for 20min, and adding 61.3 parts of second urea (U) 2 ) Keeping the temperature for 20min;
(3) Adjusting pH to 5.0-5.5 with acid solution, reacting until viscosity is 17.0-20.0 s (coating in-4 cup, 30 deg.C), cooling to 60 deg.C, adjusting pH to 7.0-8.0 with alkali solution, and adding 21.5 parts of third urea (U) 3 ) Keeping the temperature for 20min, cooling to room temperature, and discharging to obtain dark brown SLUF resin, wherein the final molar ratio of formaldehyde to urea is 1.2.
The alkali solution is a sodium hydroxide solution with the mass fraction of 40%, and the acid solution is a formic acid or acetic acid solution with the mass fraction of 30%.
The temperature rise rate is 1 ℃/2min.
The inventor improves the SLUF resin on the basis of preliminary research in the earlier stage, develops a lignin sodium sulfonate-urea formaldehyde pre-shrinking liquid-urea synthesis modified urea formaldehyde resin wood adhesive, takes lignin sodium sulfonate, urea formaldehyde pre-shrinking liquid and urea as main raw materials, takes sodium hydroxide and formic acid or acetic acid as catalysts, and carries out copolycondensation synthesis through an alkali-acid-alkali synthesis process; wherein the mass ratio of the sodium lignosulphonate to the urea is 0.21-0.40, the molar ratio of the formaldehyde to the urea in the urea formaldehyde pre-condensation liquid is 6:1, and the molar ratio of the formaldehyde to the urea is 1.2. Accordingly, a corresponding preparation method is also established. The invention can effectively introduce sodium lignosulfonate into a copolymerization system to realize the copolycondensation reaction of the sodium lignosulfonate, the urea-formaldehyde precondensate and urea. Compared with the earlier research, the invention increases the dosage of sodium lignosulfonate, changes the molar ratio of formaldehyde to urea in the urea formaldehyde precondensate, reduces the molar ratio of formaldehyde to urea, but has similar performance and longer storage period compared with pure Urea Formaldehyde (UF) resin, and can be widely applied to the industry of artificial boards. In a word, the invention realizes the effective utilization of the sodium lignosulfonate in the pulping black liquor, and has wide raw material source and low price; the synthesis process is similar to UF resin, production equipment does not need to be replaced, and parameters do not need to be adjusted too much; the product effectively reduces the content of free formaldehyde in the resin, has more environmental protection advantages, and improves the operability in the actual production of the plywood.
Detailed Description
Example 1
UF, raw material ratio: the molar ratio of formaldehyde to urea in the urea formaldehyde pre-condensation liquid is 6:1, and the molar ratio of formaldehyde to urea is 1.2.
The preparation method comprises the following steps:
(1) Adding 291.9 parts of urea formaldehyde pre-condensate into a reaction kettle, and adding 97.2 parts of U 1 Adjusting the pH value to 8.0-9.0 by using an alkali solution (a sodium hydroxide solution with the mass fraction of 40%, the same applies below), heating to 88 ℃, preserving the temperature for 20min, and adding 61.3 parts of U 2 Keeping the temperature for 20min;
(2) Adjusting the pH value to 5.0-5.5 by using an acid solution (30 mass percent formic acid solution), reacting until the viscosity is 17.0-20.0 s (coating in a 4 cup, 30 ℃), cooling to 60 ℃, adjusting the pH value to 7.0-8.0 by using an alkali solution, and finally adding 21.5 parts of U 3 Keeping the temperature for 20min, cooling to room temperature, and discharging to obtain milky UF resin.
Wherein the urea formaldehyde precondensate is prepared in advance according to the following steps (similar to the following examples): adding 2160.0 parts of 50 mass percent formaldehyde solution into a reaction kettle, starting a stirrer, adjusting the pH to 8.0-9.0 by using an alkali solution, heating to 90 ℃, uniformly dividing 360.0 parts of urea into three batches, adding the three batches of urea into the reaction kettle, reacting until the solution is clear and transparent, cooling to room temperature, adding distilled water to adjust the 50 percent formaldehyde solution into 37 percent formaldehyde solution, and blanking to obtain colorless and transparent urea formaldehyde pre-condensation solution.
The product performance is as follows: the adhesive is milk white liquid, the content of free formaldehyde is 0.27 percent, the solid content is 48.92 percent, the viscosity is 17.37s (coating-4 cups, 30 ℃), the storage period is 15 days, the bonding strength is more than or equal to 0.7MPa, and the prepared plywood reaches the standard of national II-type plywood.
Example 2
SLUF-1, raw material ratio: the molar ratio of formaldehyde to urea in the urea formaldehyde pre-condensation liquid is 6:1, the mass ratio of sodium lignosulfonate to urea is 0.21.
The preparation method comprises the following steps:
(1) 291.9 parts of urea formaldehyde precondensate solution and 37.8 parts of sodium lignosulfonate are added into a reaction kettle, a stirrer is started, the pH is adjusted to 8.0-9.0 by using an alkali solution (a sodium hydroxide solution with the mass fraction of 40 percent, the same is applied below), and then 97.2 parts of U is added 1 Heating to 88 ℃, keeping the temperature for 20min, and adding 61.3 parts of U 2 Keeping the temperature for 20min;
(2) Adjusting the pH value to 5.0-5.5 by using an acid solution (30 mass percent formic acid solution), reacting until the viscosity is 17.0-20.0 s (coating in a 4 cup, 30 ℃), cooling to 60 ℃, adjusting the pH value to 7.0-8.0 by using an alkali solution, and finally adding 21.5 parts of U 3 Preserving the heat for 20min, cooling to room temperature, and discharging to obtain the dark brown SLUF resin.
The preparation method of the urea formaldehyde precondensate is the same as that of the example 1.
The product performance is as follows: the adhesive is dark brown liquid, the content of free formaldehyde is 0.21%, the content of solid is 50.40%, the viscosity is 17.12s (coating-4 cup, 30 ℃), the storage period is 40-50 days, the bonding strength is more than or equal to 0.7MPa, and the prepared plywood reaches the standard of national II-type plywood.
Example 3
SLUF-2, raw material ratio: the molar ratio of formaldehyde to urea in the urea formaldehyde precondensate solution is 6:1, the mass ratio of sodium lignosulfonate to urea is 0.27.
The preparation method comprises the following steps:
(1) Adding 291.9 parts of urea formaldehyde pre-condensate and 48.6 parts of sodium lignosulfonate into a reaction kettle, starting a stirrer, adjusting the pH to 8.0-9.0 by using an alkali solution, and then adding 97.2 parts of U 1 Heating to 88 ℃, keeping the temperature for 20min, and adding 61.3 parts of U 2 Keeping the temperature for 20min;
(2) Adjusting the pH value to 5.0-5.5 by using acid solution (30 mass percent formic acid solution), and reacting untilThe viscosity is 17.0-20.0 s (coating in a 4 cup, 30 ℃), the pH is adjusted to 7.0-8.0 by alkali solution after the temperature is reduced to 60 ℃, and finally 21.5 parts of U is added 3 Preserving heat for 20min, cooling to room temperature, and discharging to obtain dark brown SLUF resin.
The preparation method of the urea formaldehyde precondensate is the same as that of the example 1.
The product performance is as follows: the adhesive is dark brown liquid, the content of free formaldehyde is 0.17%, the content of solid is 50.84%, the viscosity is 17.36s (coated in-4 cups, 30 ℃), the storage period is 50-60 days, the bonding strength is more than or equal to 0.7MPa, and the prepared plywood reaches the standard of national II-type plywood.
Example 4
SLUF-3, raw material ratio: the molar ratio of formaldehyde to urea in the urea formaldehyde pre-condensation liquid is 6:1, the mass ratio of sodium lignosulfonate to urea is 0.33.
The preparation method comprises the following steps:
(1) 291.9 parts of urea formaldehyde pre-condensed liquid and 59.4 parts of sodium lignosulfonate are added into a reaction kettle, a stirrer is started, the pH value is adjusted to 8.0-9.0 by alkali solution, and then 97.2 parts of first batch of urea (U) is added 1 ) Heating to 88 deg.C, maintaining the temperature for 20min, and adding 61.3 parts of second urea (U) 2 ) Keeping the temperature for 20min;
(2) Adjusting pH to 5.0-5.5 with acid solution (30 wt% acetic acid solution), reacting to viscosity of 17.0-20.0 s (coating in 4 cup, 30 deg.C), cooling to 60 deg.C, adjusting pH to 7.0-8.0 with alkali solution, and adding 21.5 parts of urea of third batch (U) 3 ) Preserving heat for 20min, cooling to room temperature, and discharging to obtain dark brown SLUF resin.
The product performance is as follows: the adhesive is dark brown liquid, the content of free formaldehyde is 0.13%, the content of solid is 51.72%, the viscosity is 17.95s (coating-4 cups, 30 ℃), the storage period is 35-45 days, the bonding strength is more than or equal to 0.7MPa, and the prepared plywood reaches the standard of national II-type plywood.
Example 5
SLUF-4, raw material ratio: the molar ratio of formaldehyde to urea in the urea formaldehyde pre-condensation liquid is 6:1, the mass ratio of sodium lignosulfonate to urea is 0.40.
The preparation method comprises the following steps:
(1) 291.9 parts of urea formaldehyde pre-condensed liquid and 72.0 parts of sodium lignosulfonate are added into a reaction kettle, a stirrer is started, the pH value is adjusted to 8.0-9.0 by alkali solution, and then 97.2 parts of first batch of urea (U) is added 1 ) Heating to 88 deg.C, maintaining the temperature for 20min, and adding 61.3 parts of second urea (U) 2 ) Keeping the temperature for 20min;
(2) Adjusting pH to 5.0-5.5 with acid solution (30 wt% acetic acid solution), reacting to viscosity of 17.0-20.0 s (coating in 4 cup, 30 deg.C), cooling to 60 deg.C, adjusting pH to 7.0-8.0 with alkali solution, and adding 21.5 parts of urea of third batch (U) 3 ) Preserving heat for 20min, cooling to room temperature, and discharging to obtain dark brown SLUF resin.
The product performance is as follows: the adhesive is dark brown liquid, the content of free formaldehyde is 0.10%, the solid content is 52.42%, the viscosity is 18.12s (coating-4 cup, 30 ℃), the storage period is 30-40 days, the bonding strength is more than or equal to 0.7MPa, and the prepared plywood reaches the standard of national II-type plywood.
And (4) analyzing results: experimental results show that the SLUF wood adhesive prepared by the invention has no great difference in other performances except appearance and pure UF wood adhesive. In addition, the introduction of the sodium lignosulfonate effectively reduces the content of free formaldehyde in the resin, and has more environmental protection advantages. The sodium lignosulfonate also greatly prolongs the storage period of the resin, and improves the operability in the actual production of the plywood.
Claims (6)
1. A lignin sodium sulfonate-urea formaldehyde precondensate liquid-urea synthesis modified urea-formaldehyde resin timber adhesive is characterized in that the lignin sodium sulfonate, urea formaldehyde precondensate liquid and urea are used as main raw materials, sodium hydroxide and formic acid or acetic acid are used as catalysts, and the synthesis is carried out by the copolycondensation reaction through the synthesis process of alkali-acid-alkali; wherein the mass ratio of the sodium lignosulphonate to the urea is 0.21-0.40, the molar ratio of the formaldehyde to the urea in the urea formaldehyde pre-condensate is 6:1, and the final molar ratio of the formaldehyde to the urea is 1.2.
2. The synthetic modified urea-formaldehyde resin wood adhesive according to claim 1, characterized in that the adhesive is dark brown liquid, the content of free formaldehyde is 0.10-0.21%, the solid content is 47.0-53.0%, the pH value is 7.0-8.0, the viscosity is 17.0-20.0 s (coating-4 cup, 30 ℃), the storage period is 30-60 days, and the bonding strength is more than or equal to 0.70Mpa.
3. The method of preparing the synthetic modified urea-formaldehyde resin wood adhesive of claim 1, wherein; preparing colorless and transparent urea formaldehyde pre-condensation liquid by using distilled water, sodium hydroxide, paraformaldehyde and urea; the prepared urea formaldehyde pre-condensed liquid, sodium lignin sulfonate and urea are subjected to copolycondensation reaction under the condition of a catalyst.
4. The preparation method according to claim 3, characterized by comprising the following steps, wherein the raw materials are in parts by weight:
(1) Adding 2160.0 parts by mass of 50% formaldehyde solution into a reaction kettle, starting a stirrer, adjusting the pH to 8.0-9.0 by using an alkali solution, heating to 90 ℃, uniformly dividing 360.0 parts of urea into three batches, adding the three batches of urea into the reaction kettle, reacting until the solution is clear and transparent, cooling to room temperature, adding distilled water to adjust the 50% formaldehyde solution into 37% formaldehyde solution, and blanking to obtain a colorless and transparent urea formaldehyde pre-condensation solution;
(2) Adding 291.9 parts of urea formaldehyde pre-condensation liquid and 37.8-72.0 parts of sodium lignosulfonate into a reaction kettle, starting a stirrer, adjusting the pH to 8.0-9.0 by using an alkali solution, then adding 97.2 parts of first batch of urea, raising the temperature to 88 ℃ by program, preserving the temperature for 20min, adding 61.3 parts of second batch of urea, and preserving the temperature for 20min;
(3) Adjusting the pH value to 5.0-5.5 by using an acid solution, reacting until the viscosity is 17.0-20.0 s (coating in a 4 cup, 30 ℃), cooling to 60 ℃, adjusting the pH value to 7.0-8.0 by using an alkali solution, finally adding 21.5 parts of third batch of urea, preserving the temperature for 20min, cooling to room temperature, and blanking to obtain the dark brown SLUF resin.
5. The method of claim 4, wherein: the alkali solution is a sodium hydroxide solution with the mass fraction of 40%, and the acid solution is a formic acid or acetic acid solution with the mass fraction of 30%.
6. The method of claim 4, wherein: the temperature rise rate is 1 ℃/2min.
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