CN108164697A - Asparagus fern carbamide resin new synthetic method - Google Patents
Asparagus fern carbamide resin new synthetic method Download PDFInfo
- Publication number
- CN108164697A CN108164697A CN201710914443.5A CN201710914443A CN108164697A CN 108164697 A CN108164697 A CN 108164697A CN 201710914443 A CN201710914443 A CN 201710914443A CN 108164697 A CN108164697 A CN 108164697A
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- CN
- China
- Prior art keywords
- asparagus fern
- carbamide resin
- primary amine
- semi
- finished product
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 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
- C08G71/00—Macromolecular compounds obtained by reactions forming a ureide or urethane link, otherwise, than from isocyanate radicals in the main chain of the macromolecule
- C08G71/02—Polyureas
Abstract
The invention discloses a kind of asparagus fern carbamide resin new synthetic methods, are related to chemical technology field, and this method is divided into two stages:First stage by strictly controlling the formula and technique of raw material, facilitates polyfunctional group organic primary amine to be reacted with dialkyl maleate.Second stage by strictly carrying out the reprocessing of special process to the material that the first stage synthesizes, obtains the target product asparagus fern carbamide resin of high conversion.Synthetic resin has following improvement in this way:1st, generated time is short, improves production efficiency, reduces energy consumption;2nd, conversion rate of products is high, more environmentally-friendly without organic primary amine and dialkyl maleate monomer.Film is fine and close after asparagus fern carbamide resin film forming, and barrier propterty increases substantially.Asparagus fern carbamide resin is mainly used in waterproof, anti-corrosion, and weatherability is required in harsh outdoor coatings.
Description
Technical field
The present invention relates to chemical technology field, it is more particularly related to a kind of new side of asparagus fern carbamide resin synthesis
Method.
Background technology
Present environmental pollution is serious, and country is determined to administer.Traditional oil product VOC emission is significantly exceeded, hair
Open up that aqueous, large arch dam product is very urgent.Chinese society just marches toward modernization comprehensively, and people require increasingly the quality of life
It is high.This product has excellent performance, and guard time is long, meets the direction of industry development.The similar product production of existing market
Period is long, generally at least 7 days generated times, and high energy consumption, the time of delivery is long, and cost remains high.
Invention content
Problem to be solved by this invention is to provide a kind of asparagus fern carbamide resin new synthetic method, and 100% contains admittedly, without molten
Agent and viscosity is low, meets environmental requirement, and product generated time is short, about 8 hours or so, and production efficiency is high.
To achieve the above object, the present invention provides following technical solution:
The asparagus fern carbamide resin new synthetic method includes the following steps:
(1) polyfunctional group organic primary amine is slowly added dropwise to in excessive dialkyl maleate (excessive total throwing amount
30%), cool down while stirring, be added dropwise process control temp be no more than 60 DEG C, drip 50 DEG C heat preservation 8 hours, 8 hours after sample
Detection, is considered as that the reaction was complete when the residual that can't detect primary amine, terminates synthesis, and product is as semi-finished product into next production
Workshop section;
(2) synthetic semi-finished product are added in into rotary evaporator or molecular distillation instrument, below vacuum degree 10Pa, temperature 80
By semi-finished product or painting or film is spread under conditions of~100 DEG C, the dialkyl maleate in semi-finished product is gone forward side by side by rapid vaporization
Enter in condenser, be collected in together after becoming liquid, be re-used as raw material and synthesized again, target product-poly- lucid asparagus
Ammonia acid ester resin is just purified.
It is using the advantageous effect of above technical scheme:The asparagus fern carbamide resin new synthetic method generated time is short, improves
Production efficiency reduces energy consumption.Asparagus fern carbamide resin high conversion rate, without organic primary amine and dialkyl maleate monomer, more
Add environmental protection.Film is fine and close after asparagus fern carbamide resin film forming, and barrier propterty increases substantially.Asparagus fern carbamide resin is mainly used in pair
Waterproof, anti-corrosion, weatherability are required in harsh outdoor coatings.
Description of the drawings
The specific embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the chemical constitution schematic diagram of asparagus fern carbamide resin;
Fig. 2 is the principles of chemistry figure of asparagus fern carbamide resin new synthetic method of the present invention.
Specific embodiment
The preferred embodiment of the invention will now be described in detail with reference to the accompanying drawings asparagus fern carbamide resin new synthetic method.
Fig. 1 and Fig. 2 shows the specific embodiment of asparagus fern carbamide resin new synthetic method of the present invention:
As shown in Fig. 2, the asparagus fern carbamide resin new synthetic method includes the following steps:
(1) polyfunctional group organic primary amine is slowly added dropwise to in excessive dialkyl maleate (excessive total throwing amount
30%), cool down while stirring, be added dropwise process control temp be no more than 60 DEG C, drip 50 DEG C heat preservation 8 hours, 8 hours after sample
Detection, is considered as that the reaction was complete when the residual that can't detect primary amine, terminates synthesis, and product is as semi-finished product into next production
Workshop section;
(2) synthetic semi-finished product are added in into rotary evaporator or molecular distillation instrument, below vacuum degree 10Pa, temperature 80
By semi-finished product or painting or film is spread under conditions of~100 DEG C, the dialkyl maleate in semi-finished product is gone forward side by side by rapid vaporization
Enter in condenser, be collected in together after becoming liquid, be re-used as raw material and synthesized again, target product-poly- lucid asparagus
Ammonia acid ester resin is just purified.
Fig. 1 is the chemical constitution schematic diagram of asparagus fern carbamide resin, and wherein X represents aliphatic carbon chain or cyclic aliphatic carbochain.
It is reacted by excessive dialkyl maleate with different polyfunctional group organic primary amines, by strict temperature control, sternly
Lattice detection primary amine content completes entire building-up process.Since dialkyl maleate is significantly excessive, primary amine is easy to that the reaction was complete,
Synthesis can't detect the residual of primary amine after proceeding to 8 hours.If primary amine routinely is designed with maleate equivalent proportion 1: 1,
Phase in post synthesis, reaction would become hard to continue, and can still detect that primary amine remains after 1 month.And remaining primary amine is great
Influence products application.Reaction product above is added in into rotary evaporator or molecular distillation instrument, by vacuum degree and temperature
Excessive dialkyl maleate is evaporated off in control, just obtains target product:Asparagus fern carbamide resin.
The asparagus fern carbamide resin new synthetic method generated time is short, improves production efficiency, reduces energy consumption.Asparagus fern polyureas tree
Fat high conversion rate, it is more environmentally-friendly without organic primary amine and dialkyl maleate monomer.Film causes after asparagus fern carbamide resin film forming
Close, barrier propterty increases substantially.Asparagus fern carbamide resin is mainly used in waterproof, anti-corrosion, and weatherability requires harsh open air
On coating.
Above is only the preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art,
Without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.
Claims (1)
1. a kind of asparagus fern carbamide resin new synthetic method, which is characterized in that include the following steps:
(1) polyfunctional group organic primary amine is slowly added dropwise to in excessive dialkyl maleate (the 30% of excessive total throwing amount),
Cool down while stirring, be added dropwise process control temp be no more than 60 DEG C, drip 50 DEG C heat preservation 8 hours, 8 hours after sample detection,
It is considered as that the reaction was complete when the residual that can't detect primary amine, terminates synthesis, product is as semi-finished product into next production workshop section;
(2) synthetic semi-finished product are added in into rotary evaporator or molecular distillation instrument, below vacuum degree 10Pa, temperature 80~
By semi-finished product or painting or film is spread under conditions of 100 DEG C, the dialkyl maleate in semi-finished product is by rapid vaporization and enters
In condenser, it is collected in together after becoming liquid, is re-used as raw material and is synthesized again, target product-poly-aspartic
Acid ester resin is just purified.
Priority Applications (1)
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CN201710914443.5A CN108164697A (en) | 2017-09-21 | 2017-09-21 | Asparagus fern carbamide resin new synthetic method |
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CN201710914443.5A CN108164697A (en) | 2017-09-21 | 2017-09-21 | Asparagus fern carbamide resin new synthetic method |
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CN108164697A true CN108164697A (en) | 2018-06-15 |
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CN201710914443.5A Pending CN108164697A (en) | 2017-09-21 | 2017-09-21 | Asparagus fern carbamide resin new synthetic method |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110396053A (en) * | 2019-07-30 | 2019-11-01 | 深圳市前海博扬研究院有限公司 | Asparagus fern polyureas performed polymer and preparation method and a kind of coating |
CN113307863A (en) * | 2021-05-25 | 2021-08-27 | 华南农业大学 | Preparation method and application of polyaspartic acid and salt antibody thereof |
CN113683775A (en) * | 2021-08-23 | 2021-11-23 | 衡阳拓创聚合新材料有限公司 | Preparation method of aqueous asparagus polyurea resin and aqueous asparagus polyurea resin thereof |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110396053A (en) * | 2019-07-30 | 2019-11-01 | 深圳市前海博扬研究院有限公司 | Asparagus fern polyureas performed polymer and preparation method and a kind of coating |
CN113307863A (en) * | 2021-05-25 | 2021-08-27 | 华南农业大学 | Preparation method and application of polyaspartic acid and salt antibody thereof |
CN113683775A (en) * | 2021-08-23 | 2021-11-23 | 衡阳拓创聚合新材料有限公司 | Preparation method of aqueous asparagus polyurea resin and aqueous asparagus polyurea resin thereof |
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Application publication date: 20180615 |