JPH0317155A - Magnesium oxysulfate-containing polyamide and production thereof - Google Patents

Abstract

PURPOSE:To obtain a polyamide capable of uniformly dispersing filler without containing air bubble by adding magnesium sulfate to at least one of lactams and catalyst or lactams and promotor, mixing the both and polymerizing lactams. CONSTITUTION:(B) 0.05-10mol% alkali catalyst and (C) 0.05-10mol% promotor (preferably isocyanates, etc.) are used to 100mol% (A) lactams (preferably epsilon- caprolactam and/or omega-laurolactam) and (D) 0.5-40 pts.wt. fibrous or needle-like magnesium sulfate, preferably having 10-50mum fiber length, 0.1-0.5mum fiber diameter and 100-200 aspect ratio is used to 100 pts.wt. the component A. The component D and filler, as necessary, are added to at least one of the components A and B or A and C, then the both are mixed with stirring, thus the component A is polymerized to afford the aimed magnesium oxysulfate-containing polyamide.

Description

Detailed Description of the Invention [Industrial Field of Application] The present invention relates to fibrous or acicular magnesium oxysulfate having excellent mechanical properties and electrical properties, or polyamides and lactams containing this and a filler. Concerning its production method using alkaline polymerization method. [Prior Art] The use of fibrous or acicular magnesium oxysulfate as an additive in thermoplastics and thermosets is known. That is, polypropylene compositions in which crystalline polypropylene is used as a thermoplastic resin and various physical properties are improved are described in Japanese Patent Publication No. 62-9260, and Japanese Patent Application Laid-Open No. 59-96153 describes a vinyl chloride resin assembly with improved rigidity.

Furthermore, JP-A-59-86654 discloses electrical characteristics,
A phenolic resin-based thermosetting molding material that has excellent heat resistance and the like has been disclosed. When adding fibrous or acicular magnesium oxysulfate to these resins,
It is desirable that the molding temperature of the resin is 250°C or less. The reason for this is that fibrous or acicular magnesium oxysulfate has water of crystallization, and when heated to 250° C. or higher, the water of crystallization is released, bubbles are generated, and a good shaped body cannot be obtained.

There has never been an example of using a fibrous or acicular magnesium oxysulfate as an additive for polyamide. The forming temperature of polyamide is as high as 260 to 300°C, and when fibrous or acicular magnesium oxysulfate is used as an additive, flow marks are generated on the shaped body, and bubbles are generated due to the release of crystal water. This is because it is difficult to obtain a good precept form.

In addition, in JP-A No. 62-256829, which is a publicly known document regarding the alkaline polymerization of lactams used in the present invention, fibrous magnesium compounds are exemplified as fibers added during polymerization. , fibrous or acicular magnesium oxysulfate is not described;
Further, the effects of the present invention are neither disclosed nor suggested.

A method for producing polyamide in which lactams are polymerized by the action of an alkali catalyst and a cocatalyst, the so-called alkaline polymerization method, is known. This method is a method of simultaneously polymerizing and forming lactams, and the polyamide obtained by this method is the same as the polyamide obtained by the usual polyamide manufacturing method, that is, the method of polymerizing lactams by heating in the presence of water. It has superior mechanical properties such as tensile strength, bending strength, and initial elastic modulus, and is used as mechanical parts for bearings, pushers, gears, and rolls. However, depending on the application, further improvements in rigidity, dimensional stability, and heat resistance are required. It is known to add fillers such as glass fiber, milled glass, glass powder, wollastonite, potassium titanate, calcium carbonate, molybdenum disulfide, carbon fiber, and Teflon powder to improve these properties. . In addition, to improve electrical properties and provide conductivity or electromagnetic shielding properties, copper powder, silver powder, nickel powder, etc. are added as metal powders, and conductive materials such as stainless steel fibers and aluminum straw fibers are added as metal fibers. It is hoped that

However, the polymerization and formation of lactams by alkaline polymerization is normally carried out in a mold in a static state, and the time required is 2.
Since the time is 0 to 100 minutes, if the specific gravity of the monomer in the molten state and the specific gravity of the filler are different, it is difficult to uniformly disperse the filler throughout the required time. That is, the filler having a higher specific gravity than the molten monomer will settle, and the filler having a lower specific gravity will float. As a result, there is a problem that the dispersion of the filler in the obtained pre-shaped body becomes non-uniform. Conventionally, many methods have been proposed to solve the above problems. For example, a method is known in which the polymerization rate is extremely increased to quickly increase the viscosity of the polymerization system to prevent the filler from sinking and floating. However, this method has the disadvantage that bubbles and cracks are likely to occur in the obtained shaped body.

[Problems to be Solved by the Invention] An object of the present invention is to provide a bubble-free polyamide in which fibrous or acicular magnesium oxysulfate is uniformly dispersed, and a method for producing the same.

Such polyamides can be mixed with glass fiber-containing polyamides and shaped to improve the surface properties of glass fiber-containing polyamides or shapes, and can be used to improve the surface properties of glass fiber-containing polyamides or shapes, and to improve the surface properties of crystalline polypropylene or vinyl chloride resins to which fibrous or acicular magnesium oxysulfate has been added. It is used to improve the mechanical properties of each by mixing with other materials.

Furthermore, another object of the present invention is to improve the mechanical properties of polyamide and to improve the mechanical properties of polyamide by using fibrous or acicular magnesium oxysulfate-1 as an additive in the alkaline polymerization of lactams. The purpose of this invention is to provide a method for producing a polyamide shaped body that uniformly disperses the filler when adding the filler and improves mechanical and electrical properties. [Means for Solving the Problems] The present invention includes (1) fibers. Polyamide containing fibrous or acicular magnesium oxysulfate, (2) After adding fibrous or acicular magnesium oxysulfate to at least one of (A) lactams and catalyst and (B) lactams and co-catalyst, both A method for producing polyamide containing fibrous or acicular magnesium oxysulfate, which comprises mixing with stirring and further polymerizing lactams, (3) (A) lactams and a catalyst, and (B) lactams and Fibrous or acicular magnesium oxysulfate and a filler are added to at least one of the cocatalysts, and then both are mixed with stirring to further polymerize lactams. A method for producing a polyamide containing a filler.

The fibrous or acicular magnesium oxysulfate used in the present invention is prepared by the method described in Japanese Patent Application No. 62-28-2122, that is, hydroxylated with a BET specific surface area of 20 rl/g or less in an aqueous magnesium sulfate solution. Magnesium or magnesium oxide at a concentration of 2
After dispersing to 5% by weight or less, 100 to 30
It can be suitably produced by a method of hydrothermal reaction at a temperature of 0''C.Also, by the method described in Japanese Patent Application No. 63-38609, magnesium sulfate and magnesium hydroxide or magnesium oxide are mixed at different concentrations. is 25
After dispersing to less than % by weight, 1. OO~
When producing fibrous magnesium oxysulfate through a hydrothermal reaction at a temperature of 300°C, it can be suitably produced in the same way as the above method by incorporating a surfactant into the hydrothermal reaction system.

The obtained fibrous or acicular magnesium oxysulfate has a powder chi-ray diffraction spectrum that is ASTM
No. 7-415, and typically the ASTM No. 7-415. MgS○4 ・5Mg(OH)2 ・3H20 which is the specific formula described in 7-415
It is thought that it can be expressed as In addition, the general form of fibrous or acicular magnesium oxysulfate has a specific gravity of 2.0 to 2.5 and a length (fiber length) of several μm to 10 μm.
00 μm, diameter (fiber diameter) of 0.1 to 10 μm, and apparent specific gravity of 0.05 to 0.3, making it an extremely bulky fibrous or needle-like substance.

The preferred shape of the fibrous or acicular magnesium oxysulfate used in the present invention is a fiber length of 10 to 50 u.
m, the fiber diameter is 0-1 to 0.5 um, and the aspect ratio (fiber length/fiber diameter) is 100 to 200.

The amount of the fibrous or acicular magnesium oxysulfate used is preferably 0.5 to 40 parts by weight per 100 parts by weight of the lactam Thi. Usage amount is 0. If it is smaller than 5 layers, the effect of adding fibrous or acicular magnesium oxysulfate is small, and the thickening effect is small, so the filler contained in Part (A) and/or Part (B) is It becomes easy to settle or float, and it becomes impossible to obtain a bolia ξ in which the filler is uniformly dispersed. If the amount used is greater than 40 parts by weight, the viscosity of the portion (A) and/or the portion (B) will increase, making it difficult to inject into the mold. Specific examples of the filler used in the present invention include glass fiber, milled glass, glass powder, wollastonite, potassium titanate fiber, carbon fiber, calcium carbonate, molybdenum disulfide, graphite, and Teflon powder. In addition, as a filler that imparts conductivity, copper powder,
Examples include nickel powder, iron powder, silver powder, Al5 fiber, aluminum flex, stainless steel fiber, carbon fiber, metallized glass fiber, and metalized carbon fiber.

The amount of filler used is based on 100 parts by weight of lactams.
It is preferably 0.1 to 50 parts by weight.

When using fibrous or acicular magnesium oxysulfate and filler, the amount of filler used is as follows.

When using milled glass as a filler, the amount of fibrous or acicular magnesium oxysulfate used is 1 to 20 parts by weight, preferably 3 to 7 parts by weight, per 100 parts by weight of the lactam. The amount is likewise 1 to 50 parts by weight, preferably 10 to 30 parts by weight. Here, if the amount of fibrous or acicular magnesium oxysulfate used is less than 1 part by weight, the thickening effect will be small and the sludge glass will tend to settle. Also, the amount used is 2
If it is more than 0 parts by weight, the viscosity will be high and it will be difficult to pour it into the mold. When using stainless fiber as a filler, the amount of fibrous or acicular magnesium oxysulfate used is 1 to 20 parts by weight, preferably 4 to 8 parts by weight, based on the weight of lactam Igloo, and the amount of stainless fiber used is Similarly, it is 1 to 50 parts by weight, preferably 10 to 30 parts by weight.

Here, if the amount of fibrous or acicular magnesium oxysulfate used is less than 1 part by weight, the thickening effect will be small and the stainless fibers will tend to settle. Furthermore, if the amount used is greater than 20 parts by weight, the viscosity will increase, making it difficult to pour into the mold. When molybdenum disulfide is used as a filler, the amount of fibrous or acicular magnesium oxysulfate used is 1 to 20 parts by weight, preferably 2 to 5 parts by weight, based on the weight of lactam HIOO. The amount used is also o. i-t is 5 parts by weight, preferably 2 to 5 parts by weight.

Here, if the amount of fibrous or acicular magnesium oxysulfate used is less than 1 part by weight, the thickening effect will be small and molybdenum disulfide will tend to settle. Furthermore, if the amount used is greater than 20 parts by weight, the viscosity will increase, making it difficult to pour into a mold.

As for the method of adding the fibrous or acicular magnesium oxysulfate and the filler, it is desirable to first sufficiently dissolve the fibrous or acicular magnesium oxysulfate and then add the filler.

Specific examples of lactams used in the present invention include γ-petite lactam, δ-petite lactam, ε-cabrolactam, ω-enanthulactam, ω-capryllactam, ω-
Examples include undecanolactam, ω-laurolactam, and C-alkyl-substituted ε-caprolactam. These may be used alone or in combination of two or more. Among these, ε-cabrolactam, ω-laurolactam, and a mixture of ε-cabrolactam and ω-laurolactam are preferred.

As the alkali catalyst, all compounds used in known alkaline polymerization methods of lactams can be used. Specific examples include alkali metals, alkaline earth metals, their hydrides, oxides, hydroxides, carbonates,
Examples include alkoxides, Grignard reagents, and reaction products of the above metal compounds and lactams, such as sodium salt, potassium salt, and bromomagnesium salt of ε-cabrolactam. The amount of alkali catalyst used is 0.05 to 10 mol%, particularly 0.2 to 5 mol%, based on the lactams.
It is preferable that

As for the co-catalyst, known co-catalysts for alkaline polymerization can be used. Specific examples include isocyanates such as phenyl isocyanate, cyclohexyl isocyanate, toluene diisocyanate, 4,4-diphenylmethane isocyanate, hexamethylene diisocyanate, polymethylene polyphenyl isocyanate, carbodiimide group-containing diisocyanate, hexamethylene-1. 6-bis Rubamide caprolactam, N.
Carba ξ docabrolactams such as N-diphenyl-P-phenylene biscarbamide lactam, acid chlorides such as penzoyl chloride, terephtha-methyl chloride, sebacoyl chloride, acetyl cabrolactam, penzoyl biscab, adiboyl biscab Examples include acyllactams such as oral lactam, terephthaloyl biscabrolactam, and isophthaloyl biscabrolactam. The promoter may be used alone or in combination of two or more. Among cocatalysts, isocyanate a
, carbaξdolactams and acyllactams are preferably used. The amount of promoter used is 0 for lactams.
．． 05 to 10 mol%, especially O. It is preferably 2 to 5 mol%.

It is desirable that each raw material used in the present invention be thoroughly dehydrated and dried before use.

The alkaline polymerization of lactams in the present invention can be carried out by mixing part (A) and part (B) according to a known method.

The polymerization temperature is higher than the melting point of the Rakum to be polymerized and lower than the melting point of the raw polyamide. A certain amount (A
) and a certain amount (B) are mixed in a weight ratio of 10:l to 1:
10, particularly preferably 5:1 to 1:5.

In the present invention, additives that do not substantially inhibit the polymerization reaction, such as plasticizers, blowing agents, dyes, pigments, antioxidants, ultraviolet absorbers, mold release agents, and impact modifiers, are added to (A) in advance.
and/or may be blended in some amount with (B).

[Function] The fibrous or acicular magnesium oxysulfate used in the present invention undergoes a two-step dehydration reaction at high temperatures and releases molecular water.

In particular, the first dehydration reaction, which is released at about 300"C, has a reaction initiation temperature around 250"C, so when kneading with resin, it needs to be carried out at 250°C or lower, preferably 240°C or lower. be. If the resin is kneaded at a temperature higher than the starting temperature of the dehydration reaction, cavities and pinholes will occur in the shaped body, which is undesirable.

The forming temperature of polyamide is usually 260 to 300°C, and when polyamide and fibrous or acicular magnesium oxysulfate are kneaded, a good shaped body cannot be obtained because of cavities and via holes.

However, the method of the present invention utilizes alkaline polymerization of lactams, and the polymerization and polymerization temperatures are usually 1.
Since the temperature is 60 to 200°C, no dehydration reaction of the fibrous or acicular magnesium oxysulfate occurs, and a good shaped body without cavities or holes can be obtained.

Fibrous or acicular magnesium oxysulfate has a smaller fiber diameter and larger asvect ratio (fiber length/fiber diameter) than ordinary fibrous compounds, such as glass fiber, and also has good affinity for lactams. . Therefore, when kneaded with lactams, it is anisotropically and uniformly dispersed, has high viscosity, and at the same time, the added filler is uniformly dispersed to prevent settling or flotation.

Furthermore, fibrous or acicular magnesium oxysulfate has a great reinforcing effect on polyamide and improves mechanical properties.

[Example] The present invention will be explained below with reference to Examples.

The settling time is determined by the settling time (A) or a certain amount (A) containing filler.
B) is heated to 120'C, placed in a 25mm diameter test tube to a height of locm, and immersed in a 120°C oil bath until the top 1cm becomes transparent.

The evaluation of the physical properties of the test pieces obtained by processing the composites or proboscis of each composition was conducted in accordance with tensile test ASTM-D638 and bending test in accordance with ASTM-D790.

Example 1 (1) Preparation of a portion (A) 750 g of substantially anhydrous ε-1 turnip Rakukum was placed in a flask and melted at 120°C. 3.6 g of sodium methylate powder was added to this solution, and by-produced methanol was removed under reduced pressure. Furthermore, dry fibrous or acicular magnesium oxysulfate 2 was added to the flask.
2. 5 g was added and mixed with stirring. Thereafter, the mixture was thoroughly degassed, a portion of it was taken into a test tube, and the mixture was placed in an oil bath and maintained at 120°C to measure the settling time. The results are shown in Table 1. (2) Preparation of Part (B) 750 g of a substantially anhydrous epsilon lactam was placed in a flask and melted at 120'C. Add hexamethylene diisocyanate to this solution} 8. 5 g was added and mixed with thorough stirring. Further, 22.5 g of dried fibrous or acicular magnesium oxysulfate was added to the flask and mixed with stirring. Thereafter, the mixture was thoroughly degassed, a portion of it was taken into a test tube, and the mixture was placed in an oil bath and maintained at 120°C to measure the settling time. The results are shown in Table 1.

Next, part 650g of a certain portion (A) and part 6 of the precept (B)
50 g was placed in a flask and stirred under reduced pressure to defoam while mixing. Then, preheat to 160'C vertical 3
Place it in a mold of 0cm, width 3cm, depth 15cm, 16
It was kept in a dryer at 0'C for 1 hour. A test piece was made from the obtained shaped product and its physical properties were measured. The result is the first
It is shown in the table. Example 2 (1) Preparation of a portion (A) of fibrous or acicular magnesium oxysulfate 7
It was prepared in the same manner as in Example 1, except that 5 g was used, and the settling time was measured. The results are shown in Table 1.

(2) Preparation of a certain amount (B) of fibrous or acicular magnesium oxysulfate 7
It was prepared in the same manner as in Example 1, except that 5 g was used, and the settling time was measured. The results are shown in Table 1.

Next, part 650g of certain amount (A) and part 650g of certain amount (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After shaping, a test piece was prepared and its physical properties were measured. The results are shown in Table 1.

Example 3 (1) Preparation of f2min (A) 750 g of substantially anhydrous ε-1 turnip lactam was placed in a flask and heated to 120°C. It melted. This }? At night, 3.6 g of sodium methylate powder was added, and by-produced methanol was removed under reduced pressure. Furthermore, dried fibrous or acicular magnesium oxysulfate 2 was added to the flask. 5 g of dried milled glass (manufactured by E1 Denki Glass Co., Ltd., trade name: EPG70-M-0)
1 1 2) 75 g were added and mixed with stirring. After that, thoroughly defoamed, take a part of it into a test tube, put it in an oil bath, keep it at 120°C, and measure the settling time.
Ta. The results are shown in Table I.

(2) Preparation of Substance (B) 750 g of substantially anhydrous ε-1 turnip lactam was placed in a flask and melted at 120°C. 8. Hexamethylene diisocyanate was added to this solution. 5 g was added and mixed with thorough stirring. Furthermore, dried fibrous or acicular magnesium oxysulfate was added to this flask.
2. 5 g and dried milled glass (manufactured by Nippon Electric Glass Co., Ltd., trade name EPG70-M'-0112) 75
g and mixed with stirring. After that, remove the bubbles thoroughly, take a part of it into a test tube, and put it in an oil bath.
The temperature was maintained at 0'C and the settling time was measured. The results are shown in Table 1.

Next, part 650g of a certain portion (A) and part 6 of the precept (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After shaping, a test piece was prepared and its physical properties were measured. The results are shown in Table 1.

Example 4 (1) Preparation of component (A) Component (A) was prepared in the same manner as in Example 3 except that 75 g of stainless fiber (manufactured by Kawasaki Steel Corporation, trade name SMF-SP #5000) was used instead of milled glass. The settling time was measured. The results are shown in Table 1.

(2) Preparation of Kaibun (B) A product was prepared in the same manner as in Example 3, except that 75 g of stainless steel fiber (manufactured by Kawasaki Seirin Co., Ltd., trade name SMF-SP #5 000) was used instead of glass. The sedimentation time was measured using the same method.The results are shown in Table 1.

Next, part 650g of Bokubun (A) and part 6 of Kibun (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After shaping, a test piece was prepared and its physical properties were measured. The results are shown in Table 1.

Example 5 (1) rli. Preparation of part (A) 75 g of molybdenum disulfide (manufactured by Daito Lubricant Co., Ltd., trade name LM-12 MEOZ powder) in place of milled glass
The preparation was carried out in the same manner as in Example 3, except that the following was used, and the sedimentation time was measured. The results are shown in Table 1.

(2) 75 g of molybdenum disulfide (manufactured by Daito Lubricant Co., Ltd., trade name LM-12 MEOZ powder) in place of the milled glass prepared in part (B).
The preparation was carried out in the same manner as in Example 3, except that the following was used, and the sedimentation time was measured. The results are shown in Table 1.

Next, part 650g of certain amount (A) and part 650g of certain amount (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After shaping, test pieces were prepared and their physical properties were measured. The results are shown in Table 1.

Comparative Example 1 (1) Preparation of Part (A) 750 g of a substantially anhydrous ε-cubic lactam was placed in a flask and melted at 120°C. 3.6 g of sodium methylate powder was added to this solution, and by-produced methanol was removed under reduced pressure.

(2) Preparation of Substance (B) 750 g of substantially anhydrous ε-cabrolactam was placed in a flask and melted at 120°C. This tg? Hexamethylene diisocyanate in Fl} 8. 5 g was added and mixed with thorough stirring.

Next, part 650g of certain amount (A) and part 650g of certain amount (B)
50 g was placed in a flask and stirred under reduced pressure to defoam while mixing. After that, a 30cm long tube preheated to 160°C
The mixture was placed in a mold with a width of 3 cm and a depth of 15 cm, and kept in a dryer at 160°C for 1 hour. Test pieces were made from the obtained molded products and their physical properties were measured. The results are shown in Table 1.

Comparative Example 2 (1) Preparation of Kaibun (A) In place of fibrous or scaled magnesium oxysulfate, 22.5 g of ξDo Glass (manufactured by Nippon Electric Glass Co., Ltd., trade name: EPG7 0-M-0 1 1 2) was used. It was prepared in the same manner as in Example 1, except that 1 was used, and the sedimentation time was measured. The results are shown in Table 1.

(2) Adjustment of precept (B) 22.5 g of milled glass (manufactured by Nippon Electric Glass Co., Ltd., trade name: EPG1 0-M-0 1 1 2) was used in place of the fibrous or acicular magnesium oxysulfate. Except for this, it was prepared in the same manner as in Example 1, and the settling time was measured. The results are shown in Table 1. Next, part 650g of precept (A) and part 6 of ibu (B)
50 g was put into a flask and polymerized in the same manner as in Example 1, but a uniform rod-shaped body could not be obtained.

Comparative Example 3 (1) Preparation of Kaibun (A) Except that 22.5 g of stainless steel fiber (manufactured by Kawa VI Steel Co., Ltd., trade name SMF-SP #5000) was used instead of fibrous or acicular magnesium oxysulfate. was prepared in the same manner as in Example 1, and the settling time was measured. The results are shown in Table 1.

(2) Preparation of Part (B) 22.5 g of stainless steel fiber (manufactured by Kawasaki Steel Corporation, trade name SMF-SP#5000) was used in place of the fibrous or acicular magnesium oxysulfate. It was prepared in the same manner as in Example 1 except that the sedimentation time was measured. The results are shown in Table 1.

Next, part 650g of a certain portion (A) and part 6 of the precept (B)
50g was placed in a flask and polymerized in the same manner as in Example 1, but a uniform precipitate was not obtained. Comparative Example 4 (1) Preparation of Part (A) Molybdenum disulfide (manufactured by Daito Lubricant Co., Ltd., trade name L) was used instead of fibrous or scaled magnesium oxysulfate.
M-12 MEOZ powder) 2 2. It was prepared in the same manner as in Example 1 except that 5 g was used, and the sedimentation time was measured. The results are shown in Table 1.

(2) Adjustment of Ibun (B) Molybdenum disulfide (manufactured by Daito Lubrication Co., Ltd., trade name L) in place of fibrous or acicular magnesium oxysulfate
M-12 MEOZ powder) 2 2. It was prepared in the same manner as in Example 1, except that 5 g was used, and the settling time was measured. The results are shown in Table 1. Next, part 650g of the precept (A) and part 6 of the certain part (B)
50 g was put into a flask and polymerized in the same manner as in Example 1, but a uniform rod-shaped body could not be obtained.

Comparative Example 5 (1) Preparation of Kaibun (A) In place of fibrous or acicular magnesium oxysulfate, fibrous or acicular magnesium hydroxide (manufactured by Kyowa Kagaku Kogyo Co., Ltd., trade name Kisuma 7B) 22 It was prepared in the same manner as in Example 1 except that .5 g was used, and the settling time was measured. The results are shown in Table 1. (2) t7. Preparation of component (B) The process of the example was similar to the above except that 22.5 g of fibrous or acicular magnesium hydroxide (manufactured by Kyowa Kagaku Kogyo Co., Ltd., trade name Kisuma 7B) was used instead of fibrous or acicular magnesium oxysulfate. It was prepared in the same manner as above and the sedimentation time was measured. The results are shown in Table 1.

Next, part 650g of a certain portion (A) and part 6 of the precept (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After cutting, test pieces were cut and physical properties were measured. The results are shown in Table 1. Comparative Example 6 (1) Preparation of Kaibun (A) In place of the fibrous or acicular magnesium oxysulfate, 75 g of fibrous or acicular magnesium hydroxide (manufactured by Showa Kagaku Kogyo Co., Ltd., trade name Kiss 77B) was used. The preparation was carried out in the same manner as in Example 1, except that the following was used, and the sedimentation time was measured.

The results are shown in Table 1. (2) Preparation of Part (B) The same procedure was carried out except that 75 g of fibrous or acicular magnesium hydroxide (manufactured by Kyowa Kagaku Kogyo Co., Ltd., trade name Kisuma 7B) was used instead of fibrous or acicular magnesium oxysulfate. It was prepared in the same manner as in Example 1 and the settling time was measured.

The results are shown in Table 1.

Next, part 650g of a certain portion (A) and part 6 of the precept (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After shaping, a test piece was prepared and its physical properties were measured. The results are shown in Table 1.

Comparative Example 7 (1) Preparation of Part (A) 750 g of substantially anhydrous ε-capsulactam was placed in a flask and melted at 120'C. 3.6 g of sodium methylate powder was added to this solution, and by-produced methanol was removed under reduced pressure. Furthermore, 22.5 g of fibrous or acicular magnesium hydroxide (manufactured by Kyowa Chemical Industry Co., Ltd., trade name Kisuma 7B) and dried milled glass (manufactured by Nippon Electric Glass Co., Ltd., trade name EPG1 0-M-0) were added.
1. 12) 75 g was added and mixed with stirring. Thereafter, the mixture was thoroughly degassed, a portion of it was taken into a test tube, placed in an oil bath, maintained at 120°C, and the settling time was measured. The results are shown in Table 1.

(2) Preparation of Ibun (B) 750 g of substantially anhydrous ε-1 turnip lactam was placed in a flask and melted at 120°C. Add hexamethylene diisocyanate to this solution} 8. 5 g was added and mixed with thorough stirring. Furthermore, 22.5 g of dried fibrous or acicular magnesium hydroxide (manufactured by Saiwa Kagaku Kogyo Co., Ltd., trade name Kisuma 7B) and dried milled glass (manufactured by Nippon Electric Glass Co., Ltd., trade name EPG) were added to the flask.
70-M-0 112) was added and mixed with stirring.

Thereafter, the mixture was sufficiently degassed, a portion of it was taken into a test tube, placed in an oil bath, maintained at 120°C, and the settling time was measured.
The results are shown in Table 1.

Next, 650g of a certain amount of (A) and 650g of a certain amount of component (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After shaping, a test piece was prepared and its physical properties were measured. The results are shown in Table 1.

Comparative Example 8 (1) Preparation of component (A) Component (A) was prepared in the same manner as Comparative Example 7 except that 75 g of stainless fiber (manufactured by Kawasaki Steel Corporation, trade name SMF-SP #5000) was used instead of milled glass. The settling time was measured. The results are shown in Table 1.

(2) Preparation of a certain amount (B) Preparation was performed in the same manner as in Comparative Example 7, except that 75 g of stainless fiber (manufactured by Kawasaki Steel Corporation, trade name SMF-SP#5000) was used instead of milled glass. was measured. The results are shown in Table 1.

Next, 650g of a portion of component (A) and 650g of a portion of bokubun (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After shaping, a test piece was prepared and its physical properties were measured. The results are shown in Table 1.

Comparative Example 9 (1) Preparation of Part (A) 75 g of molybdenum disulfide (manufactured by Daito Lubricant Co., Ltd., trade name LM-12 MEOZ powder) in place of milled glass
A sample was prepared in the same manner as in Comparative Example 7 except that the following was used, and the settling time was measured. The results are shown in Table 2.

(2) Adjustment of component (B) 75 g of molybdenum disulfide (manufactured by Daito Lubricant Co., Ltd., trade name LM-12 MEOZ powder) in place of milled glass
A sample was prepared in the same manner as in Comparative Example 7 except that the following was used, and the settling time was measured. The results are shown in Table 1.

Next, part 650g of precepts (A) and part 6 of component (B)
50 g was placed in a flask and mixed in the same manner as in Example 1. After shaping, a test piece was prepared and its physical properties were measured. The results are shown in Table 1.

[Effects of the Invention] The polyamide of the present invention contains fibrous or acicular magnesium oxysulfate. In particular, those containing fillers have various excellent properties because the fillers are uniformly dispersed. The manufacturing method of the present invention is a method for manufacturing such a polyamide, and especially when a filler is used in combination, the settling time of the filler during polymerization and shaping is long, and the filler can be easily and uniformly dispersed. There are no restrictions on the type or amount of filler that can be used.

Claims (3)

[Claims] (1) Polyamide containing fibrous or acicular magnesium oxysulfate. (2) After adding fibrous or acicular magnesium oxysulfate to at least one of (A) the lactams and the catalyst and (B) the lactams and the co-catalyst, both are mixed with stirring and the lactams are further polymerized. A method for producing polyamide containing fibrous or acicular magnesium oxysulfate, characterized by: (3) After adding fibrous or acicular magnesium oxysulfate and a filler to at least one of (A) the lactams and the catalyst and (B) the lactams and the co-catalyst, the two are mixed with stirring, and then the lactams are added. 1. A method for producing polyamide containing fibrous or acicular magnesium oxysulfate and a filler, which comprises polymerizing fibrous or acicular magnesium oxysulfate.