A kind of high-performance etherified bio-based resin and preparation method thereof

A technology of bio-based resins and amino resins, applied in the fields of aldehyde/ketone condensation polymer adhesives, adhesive types, papermaking, etc., can solve the problems of easy self-crosslinking reaction, poor storage stability, and low mechanical strength , to achieve the effect of improving market competitiveness and application value, high mechanical strength and hardness, and simple preparation method

Active Publication Date: 2019-06-21
JIANGNAN UNIV
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Problems solved by technology

At the same time, the imino group is very active and unstable, and it is most prone to self-crosslinking reaction, and its storage stability is poor.
Generally, industrially produced etherified melamine resins contain a certain amount of solvent, and a low degree of etherification will also reduce the solid content
It can be seen from the above that etherified melamine resin has problems such as poor storage stability, high free formaldehyde content, low solid content, and strong odor. While endangering the environment, long-term contact will also cause potential hazards to human health, making it in coatings, The application of ink is limited to a certain extent
[0004] In order to solve the above problems, some researchers chose to introduce photosensitive groups into the structure of amino resins to prepare aminoacrylates, such as "Ying Mingyou. Synthesis of new photosensitive prepolymers and their applications in inks [D]. Jiangnan University, 2008." Synthesized a light-curable petroleum-based aminoacrylic resin to improve storage stability and reduce formaldehyde content. However, the high hardness of this resin results in excess rigidity and insufficient flexibility, which limits its use in certain applications on some flexible substrates; our research group has also conducted related research before, for example, in CN 105669580 A, a photocurable resin containing a triazine ring and its preparation method are disclosed. The oleic acid structure and amino resin are modified The multi-arm bio-based aminoacrylate with hard-core and soft-shell structure can be successfully prepared. The preparation method is simple, the price is cheap, and the photosensitivity is strong. However, because the molecular structure contains long flexible fatty chains, the hardness of the cured film is low, and the mechanical strength is low. Need to further enhance the modification to enhance its application space and value

Method used

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  • A kind of high-performance etherified bio-based resin and preparation method thereof
  • A kind of high-performance etherified bio-based resin and preparation method thereof
  • A kind of high-performance etherified bio-based resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Add 23.426g high methyl etherified melamine formaldehyde resin (Jinan Sanqiang Chemical Co., Ltd., viscosity 7300mPa s), 124.034g hydroxyethyl cardanol ether, 0.468g p-toluenesulfonic acid, 12g n-octane Power stirring bar, condensing reflux tube, thermometer and 250mL four-necked flask equipped with n-octane water separator;

[0062] (2) Pass dry gas before heating up, slowly raise the temperature to 110°C and slightly reflux within 1 hour, and continue the reaction for 14 hours, so that n-octane and methanol generated in the reactant form an azeotrope to slowly remove from the reaction system Remove small alcohol molecules, react for 14 hours, then raise the temperature to 125°C and continue the reaction for 4 hours;

[0063] (3) Stop heating after the reaction is over and continue to stir and cool to room temperature, and remove residual n-heptane in the system by distillation under reduced pressure to obtain product A;

[0064] (4) Product A is washed repeatedly...

Embodiment 2

[0072] (1) Add 3.254g high-etherified melamine formaldehyde resin (Jinan Sanqiang Chemical Co., Ltd.), 17.227g hydroxyethyl cardanol ether, 0.069g p-toluenesulfonic acid, 2.146g isooctane to a power stirring bar, Condensation reflux tube, thermometer and 100mL four-neck flask equipped with n-heptane water separator;

[0073] (2) Pass dry gas before heating up, slowly raise the temperature to 105°C within 1.5 hours and reflux slightly, and continue the reaction for 13 hours, so that isooctane and butanol generated in the reactants form an azeotrope to slowly remove from the reaction system Removal of alcohol small molecules;

[0074] (3) Stop heating after the reaction is over and continue to stir and cool to room temperature, and remove residual isooctane in the system by distillation under reduced pressure to obtain product A;

[0075] (4) Product A was washed multiple times with acetonitrile to remove unreacted catalyst p-toluenesulfonic acid and raw materials, and after va...

Embodiment 3

[0080] (1) Add 23.614g of high methyl etherified urea formaldehyde resin, 137.816g of hydroxyethyl cardanol ether, 0.274g of p-toluenesulfonic acid, and 12g of n-octane into the In the 100mL four-neck flask of the alkanes water separator;

[0081] (2) Pass dry gas before heating up, slowly raise the temperature to 110°C and microreflux within 1.5 hours, and continue the reaction for 12 hours, so that n-octane and methanol generated in the reactants form an azeotrope to slowly remove from the reaction system Removal of alcohol small molecules;

[0082] (3) Stop heating after the reaction is over and continue stirring to cool to room temperature, and decompressed distillation to remove residual n-octane in the system to obtain product A;

[0083] (4) Product A was washed several times to remove unreacted catalyst and raw materials, distilled under reduced pressure, and dried in a vacuum oven for 24 hours to obtain the product modified urea-formaldehyde resin.

[0084] Highly e...

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Abstract

The invention discloses a high-performance etherified bio-based resin and a preparation method thereof, belonging to the technical field of synthetic resins. In the present invention, amino resin and hydroxyethyl cardanol ether with hydroxyl groups are used as raw materials, and ether exchange reaction is carried out under the action of a catalyst to obtain a modified amino resin with high bio-based content, and a certain amount of monohydroxyl lower ether can also be added. Mixed etherification makes mixed etherified amino resin with lower viscosity and good stability. The preparation method of the present invention is simple, low in cost, mild in reaction conditions, and strong in controllability. The synthesized novel bio-based mixed etherified amino resin has high solid content, low viscosity, good biodegradability, stable product performance, and can Used as a chemical intermediate in the field of industrial coatings.

Description

technical field [0001] The invention relates to a high-performance etherified bio-based resin and a preparation method thereof, belonging to the technical field of synthetic resins. Background technique [0002] Amino resins are amino-containing (-NH 2 ) is a kind of thermosetting resin with high cross-linking activity obtained by the methylolation reaction of the compound with formaldehyde, and then the etherification modification with the lower alcohol. Usually, the coating film obtained by using amino resin as a crosslinking agent has the advantages of high hardness, high gloss, good color retention, good chemical resistance and weather resistance, so it is widely used in the coating industry, leather tanning agent, adhesive Agents, flame retardant materials and other fields. [0003] At present, there are many etherified melamine resin products on the market, and the synthesis technology is very mature. Melamine formaldehyde resin contains a lot of -CH 2 OH and -NH- ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G12/42C08L61/32C09D161/32C09J161/32D06M15/427D21H19/26B33Y70/00
CPCC09D161/32C09J161/32D06M15/427D21H19/26C08G12/42C08G12/422C08G12/427C08L61/32B33Y70/00C08L2201/08
Inventor 刘仁陈淼刘敬成刘朋飞张丽萍刘晓亚陈明清
Owner JIANGNAN UNIV
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