专利摘要:
A method for preparing a block copolymer of an ether free polylactam and a polyetheramide, e.g., poly(4,7-dioxadecamethylene adipamide) involves polymerizing a lactam, e.g., caprolactam, in contact with the polyetheramide. Resulting block copolymer has utility, e.g., as a fiber.
公开号:SU1508964A3
申请号:SU803006758
申请日:1980-11-14
公开日:1989-09-15
发明作者:Милшон Томпсон Роберт
申请人:Сантек Инк (Фирма);
IPC主号:
专利说明:

The invention relates to a method for producing a block copolymer consisting of two different amide blocks that can be used in the production of fibers, one of these blocks. is polyetheramide, another is polyamine.
The aim of the invention is to increase the efficiency of the process.
Examples Three trials were previously carried out in glass tubes to determine if this method results in a block polymer. Appropriate amounts of solid caprolactam. Poly- (A, 7-dioxadeca-methylene adipamide) (N-30203-6) and solid aminocaproic acid (a known initiator) are loaded into a large Q test tube with two rubber plugs at both ends. These holes are designed for a spiral mixer and nitrogen injection. The tube is freed from air by purging the a.zot and subjected to heating using a suitable steam.
liquid bath. The mixture of materials is mixed using a spiral
(mixer, rotation of which is provided by the air engine, for a specified time. Before cooling the molten material, the mixer is removed from the tube. Table 1 presents data on the amount of each of the loaded materials, used elevated temperature and duration of the heating period.
As shown in the table. 1, previously obtained N 30203-6, loaded in accordance with from the experiments, characterized by different viscosity, which is caused by different chain length. The purpose of using materials with different chain lengths is to determine the effect of chain length on the block of polymer produced. As can be seen from the solubility
- formic acid (concentration of formic acid at 50% recovery), some effect takes place. Test 3 was obviously conducted at too.
SP

s
3150896
low temperature and for too short a period of time, as indicated by the percentage of extractables. This confirms that most lac-5 has not polymerized. The solubility of formic acid in experiments 1–3 indicates that the blocks were obtained, since the statistical polymer would have a value of 33.3 (the concentration of the formic acid, Juic Acid, at 50% recovery).
A reactor with a capacity of 7.5 / 1 l is loaded with 1090 g of solid poly- (4,7-diox-: sadacamethylene adipamide) and g of solid caprolactam. Polyetheramide receive in accordance with the known method, mol. weight. about 30,000, a value of about 111 and a value of z of order. 1b7. 18 g of solid sodium benzenephosphinate, a known antioxidant, is also added to the batch loaded into the reactor. Reactor. purged with nitrogen and in it during the experiments support pressure with nitrogen equal to 10 (0.703 kg / cm). The contents of the reactor are agitated and heated before and at this time a sample is taken. Contents of reaction15
go
25

at the beginning of the formation of statistical chains. The true melting point for industrially produced nylon-6 is about 220 ° C.
After heating for 5 m at 250 ° C, the reactor is cooled to ambient temperature and the product is spun into fiber. The resin has good fiber characteristics as well as good hydrophilic properties. Using lactam instead of caprolactam and polyether amides instead of 7- (dioxadecamethylene adipamide) in these examples leads to similar results.
The properties of the resulting block copolymers with a different number of blocks of polyetheramide and nylon-6 compared with the known: Concentration
N 30203-6
in N - 6
20 30
Tensile strength
Proposed Known 3.3 3.3 3, + 2, it
the torus is kept for another 5 hours, during which samples are taken at intervals of 1 hour.
In tab. Figure 2 shows the results of various tests carried out on the samples. (The effect of the reaction time on the melting point of the copolymer).
The percentage extractable value refers to the amount of monomer or oligomer that remains dissolved in water when the product is subject to
It can be seen washing in boiling water from the data presented in Table. 2, as the reaction time increases, the amount of substance remaining in the water decreases, indicating that more and more caprolactam is polymerized.
Changes in the DSC (differential scanning calorimeter) melting points indicate a change in the number of blocks formed. So, if the true DSC temperature increases, then more blocks are formed as a result of transamidation between the polycaprolactam formed and the polyether imide. However, after about 4 hours of reaction, the true DSC temperature begins to decrease, indicating
权利要求:
Claims (1)
[1]
Invention Formula
The method of producing block copolyamide containing polycaproamide blocks and poly 4,7-dioxadecamethylene di-amide blocks, characterized in that, in order to increase the efficiency of the process, lactam is polymerized in the presence of poly C, 7-Aioxadecamethylene adipamide at 230-250 WITH.
 Table 1
28 12 0.26
28
12 0.7
28 12 0.89
1.35 1.35 1.35
250 5
250 5
190-2 5 2-0,5
0.9
1.1 1.6
类似技术:
公开号 | 公开日 | 专利标题
SU971104A3|1982-10-30|Process for producing polyesteramides
US2174527A|1939-10-03|Polyamides
Coffman et al.1947|Polymeric amides from diamines and dibasic acids
SU1508964A3|1989-09-15|Method of producing block-copolyamide
US4212777A|1980-07-15|Linear, flexible, high tensile strength copolyamides
US3578640A|1971-05-11|Method for the production of thermally stable polycaprolactam
SU1079179A3|1984-03-07|Process for preparing ethers-esters of block-copolymer esteramides
EP0053876A1|1982-06-16|Transparent polyamides
SU651013A1|1979-03-05|Method of obtaining polyamides with higher electric conductivity
US3538058A|1970-11-03|Polyesteramides
CA1039024A|1978-09-26|Method to prepare nylon 6 prepolymer providing a final shaped article of low oligomer content
KR20000016148A|2000-03-25|Linear very high molecular weight polyamides and process for producing them
US3992360A|1976-11-16|Transparent polyamides from 1,3-bis-|-cyclohexane and aliphatic amino carboxylic acid
US6300463B1|2001-10-09|Thermoplastic elastomers
EP0426049B1|1994-12-28|Wholly aromatic copolyamide and shaped article thereof
DK160320B|1991-02-25|COPOLYETHERAMIDS WITH BLOCK STRUCTURE FOR TECHNICAL APPLICATIONS, WITH GOOD TEMPERATURES AND WITH A VISCOSITY IN MELTED CONDITION OF AT LEAST 50 PA X S
SU1496636A3|1989-07-23|Copolyamide
CA1090033A|1980-11-18|Single step preparation of block copolymer of polyamides
CA2000639C|2000-08-29|Melt-processible aromatic polyamides
US3211807A|1965-10-12|Process for obtaining a blend of a polyamide and a poly|
KR850000079B1|1985-02-18|Manufacture of a block copolymer containing a polyetheramide and a polylactam
US3037002A|1962-05-29|Polymerization of caprolactam with amino acids and the products therefrom
US5461141A|1995-10-24|Solid phase polymerization of nylon
Puffr et al.1983|Acidolytic polymerization of N‐methyldodecanelactam
US3699183A|1972-10-17|High molecular weight polyamides with an improved affinity for acid dyes modified with amino epoxy compound
同族专利:
公开号 | 公开日
NL8006173A|1981-06-16|
SE8007984L|1981-05-15|
DK484380A|1981-05-15|
FR2469425A1|1981-05-22|
GB2063280A|1981-06-03|
IN154592B|1984-11-17|
US4297454A|1981-10-27|
DE3043114A1|1981-08-27|
GB2063280B|1983-08-10|
BE886138A|1981-05-13|
FR2469425B1|1985-10-25|
IT8025739D0|1980-11-03|
ES496818A0|1981-10-16|
ES8107272A1|1981-10-16|
DE3043114C2|1989-08-24|
IT1134151B|1986-07-31|
MX156487A|1988-08-29|
SE444178B|1986-03-24|
CA1155585A|1983-10-18|
JPS5682819A|1981-07-06|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题

US4177222A|1973-11-14|1979-12-04|Suntech, Inc.|Block copolymer of poly and polyamide|
US3944629A|1974-06-24|1976-03-16|Monsanto Company|Polyester initiated anionic catalyzed polymerization of lactam|
US4113794A|1975-03-12|1978-09-12|Sun Ventures, Inc.|Copolymer of blocks of random poly and polyamide|
US4136133A|1975-03-27|1979-01-23|Sun Ventures, Inc.|Block copolymer of poly and polyamide|
DE2647309A1|1976-10-20|1978-04-27|Bayer Ag|Block amide! copolymer prepn. - by dissolving oligo-amide in lactam melt and polymerising the soln. by anionically activated polymerisation|
US4044071A|1976-11-08|1977-08-23|Suntech, Inc.|Single step preparation of block copolymer of polyamides|
US4045511A|1976-11-08|1977-08-30|Suntech, Inc.|Minimum energy process for preparing block copolymers of polyamides|
SE423241B|1976-11-08|1982-04-26|Suntech|PROCEDURE FOR PREPARING A POLYAMIDE SEGMENT POLYMER|
US4165346A|1976-11-26|1979-08-21|Sun Oil Company Of Pennsylvania|Copolymer of poly-polycaprolactam containing terephthalic acid|
US4045512A|1976-11-26|1977-08-30|Suntech, Inc.|Melt blending polyamide process|US4417031A|1982-01-07|1983-11-22|Allied Corporation|Process for preparing graft and block copolymers|
US4550157A|1984-05-07|1985-10-29|The Dow Chemical Company|Polyamide block copolymer from lactam and azetidine-2,4-dione|
DE3436359A1|1984-10-04|1986-04-10|Basf Ag, 6700 Ludwigshafen|POLYAMIDE MOLDED PARTS AND METHOD FOR THEIR PRODUCTION|
AT383611B|1984-12-27|1987-07-27|Vysoka Skola Chem Tech|USING A BLOCK copolymer based on polyethylene oxide and poly-6-caprolactam in a porous POWDER sorbent COLLOIDAL STABILIZATION AND organoleptic properties VONORGANISCHE COMPONENTS CONTAINING DRINKS, ESPECIALLY BEER, WINE, SPIRITS AND OBSTGETRAENKEN AND METHOD FOR PRODUCING this sorbent|
US4956423A|1985-10-29|1990-09-11|Occidental Chemical Corporation|Hot-melt adhesives|
US5030710A|1990-04-10|1991-07-09|Texaco Chemical Company|Nylon-6 modified with low molecular weight polyethylene glycol diamines|
US5254668A|1992-06-29|1993-10-19|Texaco Chemical Company|Polyamidopolyfunctional amine from lactam and ether amine|
EP0772484B1|1994-07-28|2008-02-27|Pall Corporation|Fibrous web and process of preparing same|
US5582907A|1994-07-28|1996-12-10|Pall Corporation|Melt-blown fibrous web|
法律状态:
优先权:
申请号 | 申请日 | 专利标题
US06/133,370|US4297454A|1979-11-14|1979-11-14|Manufacture of a block copolymer containing a polyetheramide and a polylactam|
[返回顶部]