Production process of dendritic polyamidoamine

A technology of polyamidoamine and production process, which is applied in the chemical synthesis process field of dendritic polymers, can solve the problems of toluene residue, restriction of industrial production, and restriction of industrialization, so as to reduce the generation of by-products, reduce the multiple of monomer excess, The effect of reducing the harm to the human body

Active Publication Date: 2016-07-20
WEIHAI CY DENDRIMER TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] There are following shortcomings in the above laboratory preparation method, which limits the possibility of its suitability for industrialized production:
[0022] 1. The reactions are all carried out in laboratory flasks, and the low temperature control uses an ice bath. The temperature is not easy to control, the operation is troublesome, and the products required by the industrial scale cannot be obtained;
[0023] 2. A large excess of raw materials (generally 50-100 times the excess of raw material amines and 2-5 times the excess of acrylates in traditional processes), resulting in increased manufacturing costs, high product prices, and low production capacity, making it difficult to promote industrialization;
[0024] 3. Toluene, a toxic solvent, is used as an entrainer in the purification process, which is used in large quantities, resulting in increased purification costs, which is not good for the health of operators, and toluene residues are not environmentally friendly and affect product quality;
[0025] 4. There is no process for purification, recycling and reuse of waste liquid, resulting in a large waste of raw materials and high costs;
[0026] 5. Simply use the small rotary steamer in the traditional laboratory for purification. Repeated purification requires repeated disassembly operations, which will accelerate equipment loss, affect production efficiency, and limit its industrialization

Method used

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  • Production process of dendritic polyamidoamine
  • Production process of dendritic polyamidoamine
  • Production process of dendritic polyamidoamine

Examples

Experimental program
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Effect test

Embodiment 1

[0051] The temperature of the 1 ton reactor is controlled by a low-temperature cooling cycle machine to -5±2°C, and 14Kg of ethylenediamine (EDA) dissolved in 70Kg of methanol is added to the reactor; 112Kg of methyl acrylate is dissolved in 444Kg of methanol, And join it in the reaction kettle and mix with the methanol solution of EDA; Keep this temperature, adopt nitrogen protection and under the mechanical agitation under continuous reaction 24h, then by 200L rotary evaporator under vacuum state, excess solvent and unreacted small molecule In order to remove unreacted small molecules to obtain a product with higher purity, the rotary evaporator with continuous feeding and discharging is used for repeated purification with solvent methanol three times to obtain the G-0.5 generation dendritic polyamidoamine.

Embodiment 2

[0053]Dissolve 118.2KgEDA in 463Kg of methanol and add it to a 1-ton reactor. The cooling cycle machine precisely controls the temperature to keep it at 0±2°C; then add dropwise 9.8KgG-0.5 dendritic polyamidoamine dissolved in 49Kg of methanol , under nitrogen protection and mechanical stirring; use a low-temperature cooling cycle machine to control the temperature of the reactor at 20±2°C, and stir at a constant temperature for 48 hours. After the reaction is complete, most of the excess methanol and EDA are removed by vacuum distillation, and then the initially purified The crude product is further purified by a rotary evaporator with continuous feed and discharge at 70°C. In order to purify excess unreacted small molecules as much as possible, n-butanol is used as an entrainer for methanol and ethylenediamine. Purified by rotary steaming once, and then washed three times with methanol to finally obtain the G0 generation dendritic polyamidoamine.

Embodiment 3

[0055] The temperature of the 1 ton reactor is controlled by a low-temperature cooling cycle machine to -5±2°C, 120.5KgMA dissolved in 472Kg of methanol is added to the reactor, and then 7.5KgG0 generation dendrite dissolved in 40Kg of methanol is added dropwise to the reactor Polyamidoamine solution, under the protection of nitrogen and mechanical stirring, the reaction temperature is controlled by a low-temperature cooling cycle machine to 20±2°C, and the reaction is continued for 24 hours. After the reaction is complete, excess methanol and MA are removed by vacuum distillation, and then the preliminary purified crude The product was further purified by a 200L rotary evaporator with continuous feeding and discharging at 60°C. In order to purify the excess unreacted small molecules as much as possible, the product was purified three times with the solvent methanol to obtain the G0.5 generation dendrimer amidoamine.

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Abstract

The invention belongs to a production process of a dendritic polymer, in particular to a production process of a dendritic polyamidoamine. The reaction temperature is precisely controlled by a low-temperature circulator. The initial reaction temperature is controlled at about -5±2°C, and after the addition of materials, the reaction temperature is controlled at 20±2°C to make the reaction more stable, and the appropriate excess monomer ratio can be adjusted to reduce the generation of by-products. , cooperate with ton-scale industrial synthesis reactor to realize industrial production scale; for the first time, continuous feeding and discharging rotary evaporation equipment is used to purify dendrimeric polyamidoamine to improve purification efficiency; The raw materials are recovered and purified to obtain reusable raw materials, which further reduces the cost of raw materials in industrial production.

Description

technical field [0001] The invention belongs to a chemical synthesis process of a dendritic polymer, in particular to a production process of a dendritic polyamidoamine. Background technique [0002] Dendritic polyamidoamine is a kind of dendritic polymer, which has a highly branched molecular structure and a large number of surface functional groups. With the increase of algebra, the molecular structure becomes spherical, and there are cavities in the molecule. The molecule has a nanometer size, and its special The synthetic method makes it have a monodisperse molecular weight distribution. [0003] Synthesis of dendritic polyamidoamines in the prior art is in the laboratory with amines (such as ethylenediamine, ammonia, hexamethylenediamine, diethylenetriamine, etc.), acrylates (such as methyl acrylate, ethyl acrylate, etc.) ) as the raw material through Michael addition reaction and amidation alternating reaction to prepare dendrimers with different algebraic numbers and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
Inventor 李武松刘聪聪
Owner WEIHAI CY DENDRIMER TECH
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