Process for the manufacture of polyamide-12 powder with a high melting point
View Patent ↗The present invention relates to a process for the preparation of polyamide-12 powder by anionic polymerization of lauryllactam in solution in a solvent of the lactam, the polyamide-12 powder being insoluble in this solvent, the polymerization being carried out: in the presence of a catalyst and of an activator; in the presence of a finely divided organic or inorganic filler, the proportion of this filler being less than or equal to 1.5 g per 1000 g of lauryllactam; and in the presence of an amide of formula R 1 —NH—CO—R 2 in which R 1 can be replaced by an R 3 —CO—NH— or R 3 —O— radical and in which R 1 , R 2 and R 3 denote an aryl, alkyl or cycloalkyl radical, the proportion of this compound being between 0.001 mol and 0.030 mol per 1000 g of lauryllactam.
1. A process for the preparation of polyamide-12 powder to obtain a polyamide-12 powder with a melting point of 183±1° C. comprising polymerizing a lauryllactam solvent solution by anionic polymerization, the polyamide-12 powder being insoluble in said solvent, the said polymerization being carried out:
in the presence of a catalyst and of an activator, wherein the ratio of the catalyst to the activator in moles is between 0.8 and 1.2;
in the presence of a finely divided organic or inorganic filler, the proportion of this filler being 0.35 to 0.9 g per 1000 g of lauryllactam; and
in the presence of an amide of formula R 1 —NH—CO—R 2 in which R 1 can be an R 3 —CO—NH—, an R 3 —CO—NH—CH 2 CH 2 — or R 3 —O— radical and in which R 1 , R 2 and R 3 denote an aryl, alkyl or cycloalkyl radical, the proportion of this compound being between 0.001 mol and 0.030 mol per 1000 g of lauryllactam
wherein said powder has a mean diameter of between 15 microns and 100 microns; a melting point of 183±1° C.; has a crystallization temperature of 135±1° C.; and wherein the proportion of catalyst to lauryllactam is from 0.1 to 5 mol per 100 mol of lauryllactam.
2. The process according to claim 1 , in which the finely divided organic or inorganic filler is silica.
3. The process according to claim 1 , in which the amide is selected from the group consisting of ethylenebisstearamide (EBS) and ethylenebisoleamide (EBO).
4. The process according to claim 1 , in which the proportion of amide is between 0.002 mol and 0.022 mol per 1000 g of lauryllactam.
5. The process according to claim 4 , in which the proportion of amide is between 0.005 mol and 0.020 mol per 1000 g of lauryllactam.
6. The process according to claim 1 , in which the polymerization is initiated at a temperature at which the solvent is in a state of supersaturation with lauryllactam.
7. The process according to claim 1 , characterized in that the said polymerization is carried out in the presence of colouring pigments, of TiO 2 , of glass fibre, of carbon fibre, of nanofiller, of nanoclay, of carbon nanotube, of pigments for infrared absorption, of carbon black, of inorganic filler or of flame-retardant additive.
8. A process for the manufacture of objects made of polyamide-12 by sintering of powders by melting caused by radiation, the powders having been obtained according to the process of claim 1 .
9. An object comprising the polyamide-12 powder obtained by the preparation process according to claim 1 .
10. The process of claim 8 , wherein said radiation is a laser beam, infrared radiation or UV radiation.
11. A polyamide-12 powder formed by the process of claim 1 .
12. The polyamide-12 powder according to claim 11 , wherein the powder particles have a mean size of between 25 and 60 μm.
13. The polyamide-12 powder according to claim 11 , wherein the enthalpy of fusion (1st warming) is 114±4 J/g.
14. The polyamide-12 powder according to claim 11 , wherein said powder can be recycled a large number of times without modification to its behaviour.