CN110964434B - Aldehyde-free green environment-friendly adhesive and preparation method thereof - Google Patents
Aldehyde-free green environment-friendly adhesive and preparation method thereof Download PDFInfo
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- CN110964434B CN110964434B CN201911190740.5A CN201911190740A CN110964434B CN 110964434 B CN110964434 B CN 110964434B CN 201911190740 A CN201911190740 A CN 201911190740A CN 110964434 B CN110964434 B CN 110964434B
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- aldehyde
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- friendly adhesive
- free green
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 51
- 239000000853 adhesive Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229920002873 Polyethylenimine Polymers 0.000 claims description 47
- 238000006243 chemical reaction Methods 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 9
- ZJHHPAUQMCHPRB-UHFFFAOYSA-N urea urea Chemical compound NC(N)=O.NC(N)=O ZJHHPAUQMCHPRB-UHFFFAOYSA-N 0.000 description 9
- 239000007795 chemical reaction product Substances 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 241000219000 Populus Species 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229920000587 hyperbranched polymer Polymers 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/02—Polyamines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/0206—Polyalkylene(poly)amines
Abstract
The invention discloses an aldehyde-free green environment-friendly adhesive and a preparation method thereof. The adhesive disclosed by the invention is strong in binding power, free of formaldehyde release and stable in color. The preparation method is simple, no other curing agent is added, the production cost is low, and the preparation conditions are mild. The adhesive prepared by the method is good in adhesive property, green and environment-friendly, and does not generate harmful gas in the using process.
Description
Technical Field
The invention relates to the technical field of chemical synthesis, and particularly relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof.
Background
China is a large wood consumption country, and the artificial board is one of the main ways of wood consumption, and the artificial board industry develops rapidly and has a huge market in China; at present, 90% of adhesives for artificial boards in the market contain substances harmful to human bodies, such as formaldehyde, benzene, toluene and the like. At present, the adhesive is widely used in life and production of people, and is widely used in furniture manufacturing industry and decoration industry in particular. With the development of social economy and the increasing living standard of people, the environmental awareness of people is higher and higher, and the requirements on living environment and living goods are higher and higher. Long-term inhalation of small amounts of formaldehyde also causes strong carcinogenicity. Therefore, the production of an aldehyde-free green environment-friendly adhesive is a trend of the development of adhesives in the future.
At present, a novel green, environment-friendly, formaldehyde-free, green and environment-friendly adhesive and a preparation method thereof are lacked.
Disclosure of Invention
The invention aims to provide a novel green, environment-friendly and thorough formaldehyde-free high-performance thermosetting resin adhesive and a preparation method thereof.
The technical scheme of the invention is as follows: the aldehyde-free green environment-friendly adhesive disclosed by the invention is composed of a hyperbranched polymer obtained by reacting urea and Polyethyleneimine (PEI).
Further, the molar ratio of the polyethyleneimine PEI to the urea is 1: 2-6.
The preparation method of the aldehyde-free green environment-friendly adhesive comprises the following steps:
(1) weighing polyethyleneimine PEI and Urea Urea according to the proportion;
(2) uniformly stirring, and placing the mixture in an oil bath kettle at the temperature of 120-135 ℃ for reaction for 4-10 h;
(3) and cooling to room temperature after reaction, weighing the mass of the product, and adding water according to 50-60% of solid content to completely dissolve the product to prepare the aldehyde-free green environment-friendly adhesive.
Further, in the step (2), the reaction temperature is 130 ℃.
Further, in the step (2), the reaction time is 6 h.
Further, in the step (3), the solid content of the adhesive is 55%.
Has the advantages that: the adhesive disclosed by the invention is strong in binding power, free of formaldehyde release and stable in color. The preparation method is simple, no other curing agent is added, the production cost is low, and the preparation conditions are mild. The adhesive prepared by the method is good in adhesive property, green and environment-friendly, and does not generate harmful gas in the using process.
Detailed Description
The invention is further illustrated by the following examples. It should be understood that these examples are illustrative and exemplary of the present invention, and are not intended to limit the scope of the present invention in any way.
Example 1
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps: (1) adding 39.25g PEI and 10.00g Urea to a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 2;
(2) stirring uniformly, and placing in an oil bath kettle at 130 ℃ for reaction for 10 h;
(3) and cooling to room temperature after reaction, and adding water according to the solid content of 55% to completely dissolve the mixture to prepare the aldehyde-free green environment-friendly adhesive.
Example 2
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps:
in step (1), the reactants PEI 33.00g and Urea 12.60g were added to the reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 3;
in the step (2), uniformly stirring, and placing in an oil bath kettle at 130 ℃ for reaction for 10 h;
in the step (3), after the reaction, cooling to room temperature, and adding water according to the solid content of 55% to completely dissolve the reaction product, so as to obtain the aldehyde-free green environment-friendly adhesive.
Example 3
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps:
in the step (1), 19.60g of polyethyleneimine PEI and 10.00g of Urea Urea are added into a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 4;
in the step (2), uniformly stirring, and placing in an oil bath kettle at 130 ℃ for reaction for 10 h;
in the step (3), after the reaction, cooling to room temperature, and adding water according to the solid content of 55% to completely dissolve the reaction product, so as to obtain the aldehyde-free green environment-friendly adhesive.
Example 4
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps:
in the step (1), 15.70g of polyethyleneimine PEI and 10.00g of Urea Urea are added into a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 5;
in the step (2), uniformly stirring, and placing in an oil bath kettle at 130 ℃ for reaction for 10 h;
in the step (3), after the reaction, cooling to room temperature, and adding water according to the solid content of 55% to completely dissolve the reaction product, so as to obtain the aldehyde-free green environment-friendly adhesive.
Example 5
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps:
in the step (1), 13.07g of polyethyleneimine PEI and 10.00g of Urea Urea are added into a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 6;
in the step (2), uniformly stirring, and placing in an oil bath kettle at 130 ℃ for reaction for 10 h;
in the step (3), after the reaction, cooling to room temperature, and adding water according to the solid content of 55% to completely dissolve the reaction product, so as to obtain the aldehyde-free green environment-friendly adhesive.
Example 6
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps: (1) adding 39.25g of PEI and 10.00g of Urea Urea into a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 2;
(2) stirring uniformly, and placing in an oil bath kettle at 120 ℃ for reaction for 10 h;
(3) and cooling to room temperature after reaction, and adding water according to the solid content of 55% to completely dissolve the mixture to prepare the aldehyde-free green environment-friendly adhesive.
Example 7
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps:
in the step (1), 33.00g of polyethyleneimine PEI and 12.60g of Urea Urea are added into a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 3;
in the step (2), uniformly stirring, and placing in an oil bath kettle at 125 ℃ for reaction for 10 h;
in the step (3), after the reaction, cooling to room temperature, and adding water according to the solid content of 55% to completely dissolve the reaction product, so as to obtain the aldehyde-free green environment-friendly adhesive.
Example 8
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps:
in the step (1), 19.60g of polyethyleneimine PEI and 10.00g of Urea Urea are added into a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 4;
in the step (2), uniformly stirring, and placing in a 135 ℃ oil bath for reaction for 10 h;
in the step (3), after the reaction, cooling to room temperature, and adding water according to the solid content of 55% to completely dissolve the reaction product, so as to obtain the aldehyde-free green environment-friendly adhesive.
Example 9
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps:
in the step (1), 15.70g of polyethyleneimine PEI and 10.00g of Urea Urea are added into a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 5;
in the step (2), uniformly stirring, and placing in an oil bath kettle at 120 ℃ for reaction for 8 h;
in the step (3), after the reaction, cooling to room temperature, and adding water according to the solid content of 55% to completely dissolve the reaction product, so as to obtain the aldehyde-free green environment-friendly adhesive.
Example 10
The invention relates to an aldehyde-free green environment-friendly adhesive and a preparation method thereof, which comprises the following steps:
in the step (1), 13.07g of polyethyleneimine PEI and 10.00g of Urea Urea are added into a reactor; the molar ratio is as follows: polyethyleneimine PEI: urea 1: 6;
in the step (2), uniformly stirring, and placing in an oil bath kettle at 120 ℃ for reaction for 6 h;
in the step (3), after the reaction, cooling to room temperature, and adding water according to the solid content of 55% to completely dissolve the reaction product, so as to obtain the aldehyde-free green environment-friendly adhesive.
Test example 1
In order to verify the performance characteristics of the synthesized aldehyde-free green environment-friendly adhesive, the following tests were performed:
the aldehyde-free green environment-friendly adhesive prepared in the embodiment is taken, poplar veneers with the thickness of 2mm are used for pressing three layers of plywood, the physical and mechanical properties of the board are tested according to the requirements of national standard GB/T17657 plus 2013 physicochemical property test method for artificial boards and decorative artificial boards, and the water resistance of the board is mainly tested. The method comprises the following specific steps: the synthesized aldehyde-free green environment-friendly adhesive is 160g/m according to the adhesive application amount2The test paper is coated on a single-layer poplar board, the hot pressing temperature is 200 ℃, the hot pressing is carried out for 6 minutes, then the board is cut into 36 test pieces, the dry strength, the wet strength (the test pieces are soaked in 63 ℃ water for 3 hours), the water resistance (the test pieces are soaked in boiling water for 3 hours) and the like of the 36 test pieces are respectively tested according to the average division of 3 parts, and the test results are shown in the table 1:
TABLE 1
| Test piece | Dry Strength (MPa) | Wet strength (MPa) | Water resistance (MPa) |
| Example 1 | 1.84 | 1.55 | 1.34 |
| Example 2 | 2.48 | 1.72 | 1.60 |
| Example 3 | 2.35 | 1.59 | 1.58 |
| Example 4 | 2.24 | 1.52 | 1.33 |
| Example 5 | 1.63 | 1.50 | 1.28 |
According to the measured intensity of each example, the following results are obtained by screening: when the molar ratio of each reactant is: PEI: 1: and 3, the corresponding aldehyde-free green environment-friendly adhesive has the best performance.
According to the water resistance requirement of GB/T9846-.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (4)
1. The preparation method of the aldehyde-free green environment-friendly adhesive is characterized by comprising the following steps of:
(1) according to the molar ratio of polyethyleneimine PEI to urea of 1: (2-6) weighing PEI and urea according to the proportion;
(2) uniformly stirring, and placing the mixture in an oil bath kettle at the temperature of 120-135 ℃ for reaction for 4-10 h;
(3) and cooling to room temperature after reaction, weighing the mass of the product, and adding water according to 50-60% of solid content to completely dissolve the product to prepare the aldehyde-free green environment-friendly adhesive.
2. The aldehyde-free green environment-friendly adhesive as claimed in claim 1, wherein: in step (2), the reaction temperature is 130 ℃.
3. The aldehyde-free green environment-friendly adhesive as claimed in claim 1, wherein: in the step (2), the reaction time is 6 h.
4. The aldehyde-free green environment-friendly adhesive as claimed in claim 1, wherein: in the step (3), the solid content of the adhesive is 55%.
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| CN110964434B true CN110964434B (en) | 2021-05-11 |
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