CN117417725A - Preparation process of environment-friendly weather-resistant plate adhesive - Google Patents
Preparation process of environment-friendly weather-resistant plate adhesive Download PDFInfo
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- CN117417725A CN117417725A CN202311523320.0A CN202311523320A CN117417725A CN 117417725 A CN117417725 A CN 117417725A CN 202311523320 A CN202311523320 A CN 202311523320A CN 117417725 A CN117417725 A CN 117417725A
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 30
- 239000000853 adhesive Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 108010073771 Soybean Proteins Proteins 0.000 claims abstract description 12
- 235000019710 soybean protein Nutrition 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- PYJJCSYBSYXGQQ-UHFFFAOYSA-N trichloro(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](Cl)(Cl)Cl PYJJCSYBSYXGQQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- 230000001105 regulatory effect Effects 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 7
- 238000007731 hot pressing Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 2
- 239000003292 glue Substances 0.000 abstract description 26
- 230000001502 supplementing effect Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 235000010469 Glycine max Nutrition 0.000 description 4
- 244000068988 Glycine max Species 0.000 description 4
- 239000011120 plywood Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000012975 dibutyltin dilaurate Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C09J189/00—Adhesives based on proteins; Adhesives based on derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a preparation process of environment-friendly weather-proof plate glue, which comprises the steps of adding 100 parts of soybean protein powder into 200 parts of deionized water, uniformly mixing, adjusting the pH value to 10-12, stirring and reacting for 2-6 hours at 40-60 ℃, reducing the viscosity to 500-1000cp, adjusting the pH value to be neutral, filtering flowing water, supplementing ethyl acetate, adding 5-10 parts of octadecyl trichlorosilane, heating to 50-60 ℃, and stirring and reacting for 1-2 hours; cooling to 35-45 ℃, adding 40-60 parts of 45-55% ethyl acetate solution of MDI at a constant speed within half an hour, and stirring for reacting for 1-3 hours; the viscosity reaches 1200-1500cp, 2.5-5 parts of dicyandiamide is added to continue to react for 1-1.5 hours, and the temperature is reduced to 12-15 ℃ at constant speed, so that the environment-friendly weather-proof plate adhesive is obtained.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a preparation process of an environment-friendly weather-resistant adhesive for plates.
Background
In the preparation process of the plate, the adhesive is indispensable, common adhesives such as urea-formaldehyde resin adhesive, phenolic resin adhesive and the like are easy to generate free formaldehyde in the use process, and along with the enhancement of environmental awareness of people, the use of formaldehyde-free adhesives has become a market trend.
Common formaldehyde-free adhesives include soybean glue and MDI glue, which are excellent in properties, but are expensive and high in activity Yi Nian boards. The soybean glue material is natural, has lower price, does not contain formaldehyde, but has insufficient adhesiveness, poor water resistance, poor anti-microbial degradation capability and easy mildew, and usually needs to be improved in properties by adding other components, such as formaldehyde, phenol and other chemical substances to stabilize the structure, and other adhesives to enhance the viscosity, but can introduce other pollutants, and the defects of the soybean glue cannot be completely overcome by direct mixing due to different adhesive properties. At present, soybean glue is modified and researched by utilizing a cross-linking agent to react with soybean protein to form a netlike cross-linked structure so as to improve, but glue solution is cross-linked to form a glue solution with large molecular weight, so that the prepared glue has large viscosity, poor fluidity and poor permeability, and the performances of construction and final plates are affected.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a preparation process of an environment-friendly weather-proof plate adhesive.
The preparation process of the environment-friendly weather-proof plate adhesive comprises the following steps:
(1) Adding 100 parts of soybean protein powder into 200 parts of deionized water, uniformly mixing by a high-speed stirrer, regulating the pH value of the mixture to 10-12 by sodium hydroxide, and stirring and reacting for 2-6 hours at 40-60 ℃ until the viscosity is 500-1000cp;
(2) Cooling to normal temperature, regulating pH to neutrality with hydrochloric acid, filtering to remove flowing water, adding ethyl acetate according to the filtered water, adding 5-10 parts of octadecyl trichlorosilane, heating to 50-60 ℃, stirring and reacting for 1-2 hours;
(3) Cooling to 35-45 ℃, adding 40-60 parts of 45-55% ethyl acetate solution of MDI at a constant speed within half an hour, and stirring for reacting for 1-3 hours;
(4) After the viscosity reaches 1200-1500cp and the viscosity does not change obviously within 15min, adding 2.5-5 parts of dicyandiamide to react for 1-1.5 hours continuously, and simultaneously starting to cool to 12-15 ℃ at a constant speed to obtain the environment-friendly weather-proof plate adhesive.
Preferably, the preparation process of the environment-friendly weather-proof plate adhesive comprises the following steps:
(1) Adding 100 parts of soybean protein powder into 200 parts of deionized water, uniformly mixing by a high-speed stirrer, adjusting the pH value of the mixture to 11 by sodium hydroxide, and stirring and reacting for 4 hours at 50-60 ℃ until the viscosity reaches 600-800cp;
(2) Cooling to normal temperature, regulating pH to neutrality with hydrochloric acid, filtering to remove flowing water, adding ethyl acetate according to the filtered water, adding 5-10 parts of octadecyl trichlorosilane, heating to 50-60 ℃, stirring and reacting for 1-2 hours;
(3) Cooling to 35-45 ℃, adding 50 parts of ethyl acetate solution of MDI with the concentration of 50% at a constant speed within half an hour, and stirring for reacting for 1-3 hours;
(4) After the viscosity reaches 1200-1500cp and the viscosity does not change obviously within 15min, adding 2.5-5 parts of dicyandiamide to react for 1-1.5 hours continuously, and simultaneously starting to cool to 12-15 ℃ at a constant speed to obtain the environment-friendly weather-proof plate adhesive.
Preferably, the plate glue is constructed by adopting a hot-pressing process, and the glue coating amount is 150g/m < 2 >; the hot pressing process conditions are that the pressure is 1MPa, the temperature is 110 ℃ and the time is 1min/mm.
The invention adjusts the microstructure of the adhesive by adjusting the solvent environment and the reaction temperature in different reaction stages, has low viscosity, good workability, strong permeability and high bonding strength to the plate, and improves the mildew-proof and weather-proof properties of the adhesive.
Description of the embodiments
The experimental methods used in the examples are conventional methods unless otherwise specified. Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified. The parts of the invention refer to mass percent, and the bonding strength test of the plate in the embodiment refers to the method test in the national standard GB/T4897-2015.
Examples
Adding 20g of soybean protein powder into 40g of deionized water, uniformly mixing by a high-speed stirrer, regulating the pH value of the mixture to 11 by using a 1mol/L sodium hydroxide solution, stirring and reacting for 4 hours at 55 ℃, measuring the viscosity 703cp of the mixture, reducing the temperature to normal temperature, regulating the pH value to neutrality by using hydrochloric acid, filtering flowing water, supplementing ethyl acetate according to the filtered water, adding 5-10 parts of octadecyl trichlorosilane, heating to 50 ℃, stirring and reacting for 2 hours, reducing the temperature to 45 ℃, uniformly adding 10g of 50% concentration ethyl acetate solution of MDI within half an hour, stirring and reacting for 2 hours, measuring the viscosity of the glue solution to 1346cp, measuring the viscosity of the glue solution to 1356cp after 15 minutes, adding 0.6g of dicyandiamide, starting uniform temperature reduction, continuously reacting for 1 hour, and reducing the temperature to 14 ℃ to obtain the environment-friendly weather-proof plate glue.
Examples
Adding 20g of soybean protein powder into 40g of deionized water, uniformly mixing by a high-speed stirrer, regulating the pH value of the mixture to 12 by using a 1mol/L sodium hydroxide solution, stirring and reacting for 4 hours at 50 ℃, measuring the viscosity 656cp of the mixture, reducing the pH value to neutral by using hydrochloric acid, filtering flowing water, supplementing ethyl acetate according to the filtered water, adding 5-10 parts of octadecyl trichlorosilane, heating to 55 ℃, stirring and reacting for 2 hours, reducing the temperature to 40 ℃, uniformly adding 10g of 50% ethyl acetate solution of MDI within half an hour, stirring and reacting for 2 hours, measuring the viscosity of the glue solution to 1426cp, measuring the viscosity of the glue solution to 1441cp after 15 minutes, adding 0.6g of dicyandiamide, starting uniform temperature reduction, continuously reacting for 1 hour, and reducing the temperature to 12 ℃ to obtain the environment-friendly weather-proof plate glue.
Comparative example 1
Adding 20g of soybean protein powder into 40g of deionized water, uniformly mixing by a high-speed stirrer, regulating the pH value of the mixture to 11 by using 1mol/L sodium hydroxide solution, stirring and reacting for 4 hours at 55 ℃, measuring the viscosity 694cp of the mixture, reducing the temperature to normal temperature, regulating the pH value to neutrality by using hydrochloric acid, filtering flowing water, supplementing ethyl acetate according to the filtered water, heating to 40 ℃, uniformly adding 10g of ethyl acetate solution of MDI with the concentration of 50% within half an hour, stirring and reacting for 2 hours, measuring the viscosity of the glue solution to 1106cp, measuring the viscosity of the glue solution to 1129cp after 15 minutes, adding 0.6g of dicyandiamide, starting uniform cooling, continuing reacting for 1 hour, and cooling to 12 ℃ to obtain the plate glue.
Comparative example 2
Adding 20g of soybean protein powder into 40g of deionized water, uniformly mixing by a high-speed stirrer, regulating the pH value of the mixture to 11 by using a 1mol/L sodium hydroxide solution, stirring and reacting for 4 hours at 55 ℃, measuring the viscosity 727cp of the mixture, reducing the pH value to neutral by using hydrochloric acid, filtering flowing water, supplementing ethyl acetate according to the filtered water, adding 5-10 parts of octadecyl trichlorosilane, heating to 60 ℃, stirring and reacting for 2 hours, uniformly adding 10g of 50% MDI ethyl acetate solution and 0.05g of dibutyl tin dilaurate within half an hour, stirring and reacting for 2 hours, measuring the viscosity of the glue to 2246cp, measuring the viscosity of the glue to 2316cp after 15 minutes, adding 0.6g of 1, 4-butanediol, continuously reacting for 2 hours, and reducing the temperature to 14 ℃ to obtain the plate glue.
Manufacturing a plywood: the board is made of poplar board, and is hot pressed into three-ply board, and the adhesive coating amount is 150g/m 2 The hot pressing process conditions are that the pressure is 1MPa, the temperature is 110 ℃, the time is 1min/mm, and 10 groups of plywood are manufactured in each embodiment.
And (3) detecting the bonding strength: the resulting plywood was left at room temperature for 1 week and tested for bond strength according to GB/T4897-2015.
Weather resistance test: placing all groups of plywood into a constant temperature and humidity box, setting the temperature to 35 ℃ and the relative humidity to 100%, detecting the bonding strength once every other week in the first month, detecting the bonding strength once every other month in the subsequent month, and observing the mildew condition of the plates.
The gluing test results are shown in table 1 below:
table 1 mildew conditions are shown in table 2 below:
TABLE 2
From the results, examples 1 and 2 showed a small amount of sizing of only 150g/m 2 The bonding strength can reach more than 1.1MPa, the comparative example 2 is modified by octadecyl trichlorosilane, the subsequent modification is carried out according to the conventional isocyanate modification process, the viscosity of the glue solution is obviously improved, the viscosity is obviously higher than that of the example 1, the bonding strength is about 1MPa under the same sizing amount, the bonding strength is not better than that of the example 1, the plate glue prepared by the example has better penetration and infiltration, the bonding layer is thicker, and the bonding strength is obviously improved. The subsequent high-temperature storage is carried out, the bonding strength of the comparative example 2 is obviously changed, the bonding layer is better in water resistance after the board is soaked, the better weather-proof effect is achieved, the soybean protein after hydrolysis of the comparative example 1 is not subjected to the modification treatment of octadecyl trichlorosilane, the subsequent reaction with MDI is poor, the glue solution is low in viscosity, the bonding performance is poor, the subsequent mildew points are easy to mildew, and a large number of unmodified groups are indicated to the soybean protein.
Claims (5)
1. The preparation method of the environment-friendly weather-proof plate adhesive is characterized by comprising the following steps of: the preparation method comprises the following steps:
(1) Adding 100 parts of soybean protein powder into 200 parts of deionized water, uniformly mixing by a high-speed stirrer, regulating the pH value of the mixture to 10-12, and stirring and reacting for 2-6 hours at 40-60 ℃ until the viscosity is 500-1000cp;
(2) Cooling to normal temperature, regulating pH value to neutral, filtering flowing water, adding ethyl acetate according to the filtered water, adding 5-10 parts of octadecyl trichlorosilane, heating to 50-60 ℃, stirring and reacting for 1-2 hours;
(3) Cooling to 35-45 ℃, adding 40-60 parts of 45-55% ethyl acetate solution of MDI at a constant speed within half an hour, and stirring for reacting for 1-3 hours;
(4) After the viscosity reaches 1200-1500cp and the viscosity does not change obviously within 15min, adding 2.5-5 parts of dicyandiamide to react for 1-1.5 hours continuously, and simultaneously starting to cool to 12-15 ℃ at a constant speed to obtain the environment-friendly weather-proof plate adhesive.
2. The method for preparing the environment-friendly weather-resistant plate adhesive according to claim 1, which is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) Adding 100 parts of soybean protein powder into 200 parts of deionized water, uniformly mixing by a high-speed stirrer, adjusting the pH value of the mixture to 11, and stirring and reacting for 4 hours at 50-60 ℃ until the viscosity is 600-800cp;
(2) Cooling to normal temperature, regulating pH value to neutral, filtering flowing water, adding ethyl acetate according to the filtered water, adding 5-10 parts of octadecyl trichlorosilane, heating to 50-60 ℃, stirring and reacting for 1-2 hours;
(3) Cooling to 35-45 ℃, adding 50 parts of ethyl acetate solution of MDI with the concentration of 50% at a constant speed within half an hour, and stirring for reacting for 1-3 hours;
(4) After the viscosity reaches 1200-1500cp and the viscosity does not change obviously within 15min, adding 2.5-5 parts of dicyandiamide to react for 1-1.5 hours continuously, and simultaneously starting to cool to 12-15 ℃ at a constant speed to obtain the environment-friendly weather-proof plate adhesive.
3. The method for preparing the environment-friendly weather-resistant plate adhesive according to any one of claims 1 to 2, which is characterized by comprising the following steps: the pH of the mixture in step (1) was adjusted with 1mol/L sodium hydroxide solution.
4. The method for preparing the environment-friendly weather-resistant plate adhesive according to any one of claims 1 to 2, which is characterized by comprising the following steps: in the step (2), 1mol/L hydrochloric acid is used for adjusting the pH value.
5. The method for preparing the environment-friendly weather-resistant plate adhesive according to any one of claims 1 to 2, which is characterized by comprising the following steps: the application method of the plate adhesive comprises the steps of adopting a hot pressing process for construction, wherein the adhesive coating amount is 150g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The hot pressing process conditions are that the pressure is 1MPa, the temperature is 110 ℃ and the time is 1min/mm.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311099072 | 2023-08-30 | ||
| CN2023110990721 | 2023-08-30 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117417725A true CN117417725A (en) | 2024-01-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311523320.0A Pending CN117417725A (en) | 2023-08-30 | 2023-11-15 | Preparation process of environment-friendly weather-resistant plate adhesive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117417725A (en) |
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2023
- 2023-11-15 CN CN202311523320.0A patent/CN117417725A/en active Pending
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