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Polydodecalactam and multistage-series polymerization method for polydodecalactam modified resin

A technology of polylaurolactam and laurolactam, which is applied in the field of polyamide materials, can solve the problems of unfavorable polycondensation molecular weight, poor flexibility, short residence time, etc., so as to avoid unfavorable polycondensation process and molecular weight growth, and ensure stability and stability. Reliability, resistance to bumping and clogging

Active Publication Date: 2017-06-20
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But find from actual operation, existing similar continuous process also has some problems: 1) laurolactam and water miscibility are relatively poor, during continuous reaction, the residence time of material in mixer is short, it is difficult to mix the two Uniformity, thereby affecting the polymerization effect in the tubular / tower reactor, in the above two patents, the residual monomer content of laurolactam in the final product is above 0.2wt%; 2) If you need to produce different batch numbers and specifications It is also difficult to flexibly add various additives and comonomers in the continuous process of polyamide 12 resin products; 3) In the patents of these continuous processes, they all enter the normal pressure section directly from the high pressure section, and there is no pressure The gradient drops, and the viscosity of the material rises too fast, which is not conducive to the smooth progress of polycondensation and the increase of molecular weight. It takes a long time for polycondensation, and it is also easy to cause the above-mentioned material bumping and pipeline blockage.
[0005] Therefore, in order to solve the shortcomings of the current conventional batch process, such as low efficiency, unstable product quality, poor mixing effect and poor flexibility of the continuous process, it is necessary to develop a new continuous polymerization process to prepare polylaurolactam and its modified resin.

Method used

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  • Polydodecalactam and multistage-series polymerization method for polydodecalactam modified resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] The preparation of PA12 pure resin products adopts a 5-stage series polymerization process

[0068] 500kg of molten monomer laurolactam and 75kg of water are input into the reactor R1 (anchor stirring) from the raw material inlet, and 1kg of terephthalic acid is added from the feed inlet A1 as a molecular weight stabilizer, and the working temperature of the kettle is maintained at 300°C. Airtight reaction, the pressure (gauge pressure) is 5.0MPa, and the residence time is 1h; then the valve V1 is opened, and the material is transported to R2 (anchor stirring), where the pressure (gauge pressure) in the kettle is stabilized at 3MPa, the reaction temperature is 290°C, and the residence time is 1h. The material is further prepolymerized here, and the monomer conversion rate is increased to 99.95% (that is, the residual order is 0.05%); then the valve V3 is opened, and the material is transported to R3 (screw Belt stirring), where the pressure (gauge pressure) in the kettl...

Embodiment 2

[0070] The preparation of PA12 additive compound products adopts a 5-stage series polymerization process

[0071] 500kg of molten monomer laurolactam and 25kg of water are input into the reactor R1 (anchor stirring) from the raw material port, and 4kg of dodecanedioic acid is added from the feeding port A1 as a molecular weight stabilizer, and the working temperature of the kettle is maintained at 280°C , airtight reaction, the pressure (gauge pressure) range is 4.0MPa, and the residence time is 3h; then the valve V1 is opened, the material is transported to R2 (anchor stirring), and 0.75kg IRGANOX 1098 and 0.75kg IRGAFOS 168 are added from A2 as antioxidant agent, the pressure (gauge pressure) in the kettle is stabilized at 1MPa through the pressure regulating valve V2, the reaction temperature is 270°C, and the residence time is 3h. The material is further prepolymerized here, and the monomer conversion rate is raised to 99.92% (ie Residual list is 0.08%); Then open valve V3...

Embodiment 3

[0073] Preparation of PA6 / 66 / 12 copolymer resin, using 5-stage series polymerization process

[0074]200kg of molten monomer laurolactam and 30kg of water are input into the reactor R1 (anchor stirring) from the raw material port, and 100kg of caprolactam is added from the feed port A1 as a comonomer, and 2kg of hexamethylenediamine is added as a molecular weight stabilizer. Keep the working temperature of 290°C, seal the reaction, the pressure (gauge pressure) is 4.5MPa, and the residence time is 2h; then open the valve V1, transfer the material to R2 (anchor stirring), and add 0.8kg IRGANOX245 and 0.8kg IRGAFOS126 from A2 as Antioxidant, add the 60% aqueous solution that 200kg nylon 66 salt prepares as comonomer, the pressure (gauge pressure) in the kettle is stabilized at 2MPa by pressure regulating valve V2, and reaction temperature is 280 ℃, and residence time is 2h, and material Further pre-polymerization and copolymerization here, the monomer conversion rate is brought ...

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Abstract

The invention provides a method for hydrolysis polymerization of laurolactam. According to the invention, through multistage-series operation, smooth transition of a high-pressure hydrolysis stage and a pressure-reducing condensation polymerization stage and highly-efficient production are realized, and the conversion rate of a laurolactam monomer is 99.9% or above; meanwhile, the process has high flexibility, can realize addition and uniform dispersion of an additive and / or a copolymerization monomer in all stages of a reaction according to needs of a product, and prepares polydodecalactam modified resin.

Description

technical field [0001] The invention relates to a multistage series polymerization method of polylaurolactam and its modified resin, belonging to the field of polyamide materials. Background technique [0002] Polyamide 12 (also known as polylaurolactam or nylon 12) is a high-performance and high-value-added long carbon chain polyamide material, which is polymerized from laurolactam. The preparation of polylaurolactam can usually adopt the hydrolytic polymerization process, using water as the ring-opening agent, under the condition of high temperature and high pressure, the laurolactam is ring-opened and an oligomer with a certain degree of polymerization is formed, and then the polylaurolactam is decomposed under normal pressure or vacuum. Under certain conditions, water should be removed as much as possible, and the molecular weight can be further increased to reach the required degree of polymerization through polycondensation, so that the polyamide 12 polymer can be obta...

Claims

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Application Information

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IPC IPC(8): C08G69/14C08G69/16
CPCC08G69/14C08G69/16
Inventor 刘彪苑先佩高斌陈海波
Owner WANHUA CHEM GRP CO LTD
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