JPS5996534A - Magnetic recording medium - Google Patents

Abstract

PURPOSE:To obtain a magnetic recording medium having superior wear resistance, durability and high reproduction output and enabling high density recording by adding dialkyl sulfosuccinate. CONSTITUTION:A magnetic layer contg. a compound represented by the general formula [where M is H, an alkali metal, NH<+> or a quat. ammonium ion, each of R<1> and R<2> is alkyl, substituted alkyl or alkenyl, each of (l) and (m) is a positive integer of 1-10, and (n) is 0 or 1] is formed on a support to obtain a magnetic recording medium. Said alkyl group is an arbitrary straight chain or branched alkyl group such as pentyl or octyl, and the preferred number of carbon atoms is 1-22. Said alkenyl group is a straight chain or branched alkenyl group such as octenyl or octadecenyl, and the preferred number of carbon atoms is 2-22.

Description

[Detailed description of the invention]

The present invention relates to improving a magnetic recording medium, and more specifically, it improves the dispersibility of magnetic powder contained in a magnetic layer, provides excellent wear resistance, durability, and reproduction output, and enables high-density recording. 1-Regarding magnetic recording media. The magnetic layer of a magnetic recording medium is usually formed by applying a magnetic paint consisting of magnetic powder, a binder, an organic solvent, and other additives onto a support such as polyester. The magnetic properties of the magnetic layer thus formed or T
[1. The magnetic conversion Q' is mainly influenced by the state of dispersion of the magnetic powder. Conventionally, attempts have been made to add various dispersants to the magnetic layer in order to improve the dispersibility of magnetic powder within the magnetic layer. For example, attempts have been made to lubricate the magnetic layer with materials such as metatadecyl pentaacetate and lecithin, but this not only has a low effect on improving dispersion, but also worsens the wear resistance and magnetism, and also increases the interlayer It also has the disadvantage of poor heat resistance, which causes adhesion. In addition, dialkyl sulfoconophosphate is known to act effectively as a dispersant, improve the filling and orientation of magnetic powder, and impart excellent magnetic properties or electromagnetic conversion properties. However, there are drawbacks such as a decrease in the bonding force between the magnetic powder and the binder resin, and a tendency for the dispersant to leach onto the surface of the magnetic layer due to a so-called blooming phenomenon. As a result, powder fall is noticeable, output fluctuations become large, tape squeal occurs, and durability is poor. In order to eliminate the drawbacks of dialkyl sulfosuccinic fffj4 for the magnetic layer, Japanese Patent Laid-Open Nos. 57-152538 and 5
As disclosed in No. 7-152537, liquid paraffin and a fatty acid-modified silicone compound represented by the general formula (with the exception of formula In the middle, y5 and y2 are -cIip or -CO, It is a saturated or unsaturated hydrocarbon having 7 to 21 carbon atoms, n is an integer from 0 to ]00 (), n2 is an integer from 1 to 500, (
, nl+I+2) is a method of adding ]0 (under Eri), JP-A No. 57-15253, No. 15-15
As shown in JP-A-57-15253::S and JP-A-57-152534,
As a binder for magnetic powder, we used a 1-vinyl chloride-vinyl acetate copolymer having an epoxy group, a fiber cord resin and a urethane prepolymer, a fiber cord resin and a polyurekne elastomer, and a fiber cord resin and a low molecule. A method is known in which a dialkyl sulfosuccinate is included in a magnetic coating R using an h1' polyol and a low molecular weight trifunctional incyanate compound. The sialgyl sulfosuccinates shown in these publications are compounds represented by the general formula (,
However, not only does it disclose that R8 and R7 are an alkyl group and M is a monovalent metal, but the technology shown in the specifications of each of the above publications also discloses that dialkyl sulfosuccinates are It is specified that the fractional properties of magnetic powders are not sufficient unless used in conjunction with specific binders or lubricants. However, it has not been shown that dialkyl sulfosuccinates have effective dispersibility in any binder. As a result of various studies on the dispersibility of dialkyl sulfosuccinates with respect to magnetic powder in the magnetic layer, the present inventors discovered a compound represented by the general formula (where M is a hydrogen atom, an alkali metal, NH4+, or an alkali metal). ion, R
1, each target is an alkyl group, a substituted alkyl group, or an alkenyl group, 1 and m are both positive integers of 1 to 10, n represents O or 1, and 1'') is used only with a specific binder. The present invention was achieved by discovering that the magnetic powder contained in the magnetic layer has excellent dispersibility compared to general binders. This was done to improve dispersibility, and the purpose is to provide a magnetic recording medium that has excellent wear resistance, durability, and reproduction output, and is capable of high-density recording. In order to achieve the above object, the magnetic recording medium of the present invention has the following features:
A compound represented by the general formula (where M is a hydrogen atom, an alkali metal, NH, or a bound ammonium ion, and R1,
R2G'! , respectively, are alkyl groups, substituted alkyl groups, or alkenyl groups, and! and In are both 1-
A positive integer of 10, where 0 is O or 1'4! : represents). In the above formula, the alkyl group is any linear or branched alkyl group such as pentyl group, octyl group, 2-ethylhexyl group, dodecyl group, bexabucil group, octadecyl group, etc., and is preferably a carbon alkyl group. Number of atoms: 1
~22 argyl groups. Further, the alkenyl group is a linear or branched alkenyl group such as an offtenyl group or an octadecenyl group, and preferably an alkenyl group having 2 to 22 carbon atoms. However, R1 and W
The total number of atoms of the argyl groups and/or alkenyl groups is 10 or more, preferably 16 or more, and the upper limit of the number of carbon atoms is preferably 44 or less, more preferably 36 or less. Examples of the above-mentioned substituents include halogen (preferably a fluorine atom, a chlorine atom, and particularly preferably a fluorine atom), a carbonyl group, a hydroxyl group, an imino group, and combinations thereof (for example, -8-N)I-, etc.); There may be any two or more substituents. Furthermore, the ether bond (−
0-J? Examples of compounds belonging to the above general formula that may contain a -8- bond are shown in Table 1 below.
In addition to the compounds shown in Table 1, the compounds according to the present invention include, for example, American compounds, 1/[21st)'18. (19), British Patent No. 548.532 specification, +', 'igakosho 5
You can also refer to the manufacturing method disclosed in Japanese Patent No. 225246. , a synthesis example of this compound is shown below-10 Synthesis Example 1 Maleic anhydride 24.5 g (025 mol) and n-
Add equimolar amount of ethylene oquinide to octatool. 130.5 g (0.75 g) of ethylene glycol monooctyl ether and 300 g of toluene
Take m-1' in a 500 mJ eggplant-shaped flask, add 1111 J of concentrated sulfuric acid, attach an ester pipe, and heat and reflux in an oil bath for 6 hours to remove generated filtrate. Next, the reaction product was cooled, neutralized with 3% sodium carbonate solution, washed with water, dehydrated, and the solvent was removed under reduced pressure. Get it. Take 341 g of the above maleic acid diester, add 11.5 g of sodium bisulfite, 20 m of water, and 5 ml of ethanol.

[l-
Heat vigorously in the lower last of OOmj' with stirring at an internal temperature of 85°C. Reaction start 10
It becomes uniform over time and eventually assimilates. The reaction product was dried under reduced pressure, dissolved in ethanol, inorganic salts were filtered off, and the filtrate was dried under reduced pressure to obtain 38.9 g (96 g) of the target product as a white solid.
%) Get it. Synthesis Example 2 The same numbers as in Synthesis Example 1, except that ethylene glycol mono-2-ethylhexyl ether was used for ethylene glycol octyl ether, Table 1.
, 162) was synthesized 14). Synthesis Example 3 In the production method of Synthesis Example 1, Table-I , A3) 17) A compound is synthesized. Synthesis Example 4 0.25 mol of diethylene glycol monostearyl ether obtained by adding 2 times the mole of ethylene oxide to maleic anhydride and steryl alcohol, Toluev 30
0+n-M was placed in a 500+ni eggplant-shaped flask, 11n1 of bisulfuric acid was added, and the mixture was treated in the same manner as in each synthesis example described in Section 2.
p) Crystallization with 11-hexano gives anhydrous crystalline maleic acid diester. Add a potassium bisulfite aqueous solution containing 31.0 g of the above maleic acid diester, and add 10 liters of ethanol.
The reaction and treatment were carried out in the same manner as in Synthesis Example 2 in a 200 mJ flask with n-M to obtain the compound shown in Table 1/164). f￥ I Example 5 Malay anhydride/a (0.5 mol of ethylene glycol mono-n-ocdyl ether, concentrated sulfur e in (1.5%/l)
Then, 0.5 mol of ethylene glycol monol]-pentyl ether was added using a dropping funnel, and the mixture was further reacted, and the resulting product was filtered out of the hydration system. reaction v
P! After cooling, neutralize with 3% sodium carbonate solution, wash with water, dehydrate, remove the solvent under reduced pressure, and distill the remaining liquid under reduced pressure to obtain maleic acid diester. 0.1 mol of this maleic acid diester and 1 pif of sodium bicarbonate
, acid soda]1. ．． 5 g and 10 ml of water 1 methanol 5 mJ
! was treated in the same manner as in the above Synthesis Example to synthesize the compounds shown in Table 1165). Synthesis Example 6 Using ethylene glycol monooctyl ether and ethylene glycol monooleyl needle 1"
Table-I was prepared in the same manner as in Synthesis Example 1, except that
Compound '11/J of A6) was successfully synthesized. Synthesis Example 7 Equimolar ethylene oxide adduct II of fluorine alcohol instead of ethylene glycol 7non-n-octyl ether (Ck 2 CF7 ) 3 CI-J20 CI
It C1120JI Same as Synthesis Example J except for 1-ru for wo f'ffi]! J! From K, the compound shown in Table 1A67) could be synthesized. Synthesis Examples 8 to 11 The compounds in Table IA8) to (611) were also synthesized by the same treatment as in the above synthesis example. Synthesis Example 12 Cloth-1161 was prepared by the same treatment η14 as in Synthesis Example 6 except that itaconic anhydride was used instead of maleic anhydride.
Compound 2) was successfully synthesized. Synthesis Example 13 Tables ~ 1/M13 were prepared in the same manner as in Synthesis Example 1 except that itaconic anhydride was used instead of maleic anhydride.
) was successfully synthesized. Synthesis Example 14 The compound shown in Table 1 (14) was treated with excess INN hydrochloric acid in an aqueous solution, water (6)1, and filtered to give a free sulfonic acid compound in a constant manner. This free h1t sulfonic acid visiting conductor is dissolved in ethanol,
Blow excessive ammonia gas into the reaction thread while stirring,
Allowed time to react. The formed precipitate was filtered and dried, and a white solid (compound No. 14 in Table 1) was almost obtained (obtained as desired. Synthesis Example I5 Using N-methylpyridinium chloride instead of ammonia gas) In the presence of Ag2C)l), Synthesis Example 1
By the same treatment as in 4, the compound shown in Table IA15) could be synthesized. Synthesis Example 16 Using detramethylammonium chloride instead of N-methylpyridinium chloride,
We were able to synthesize the compound 16). In order to incorporate the above-mentioned compound into the magnetic powder in such a recording medium, it is necessary to dissolve it in a solvent such as toluene, methyl ethyl ketone ethyl cellosolve, acetone, or methanol. , magnetic powder is immersed in this solution at a predetermined ratio, stirred and mixed, then filtered and subjected to drying treatment, or
The seeds may be added directly to the magnetic paint in which magnetic powder is dispersed or dissolved in a suitable solvent. The following margin: The compound according to the present invention is usually 05 parts by weight to 30 parts by weight, preferably 05 parts by weight to 1 part by weight, per 100 parts by weight of magnetic powder.
Use in the range of 0 parts by weight. The compound of the present invention is 0.5
If the amount is less than 30 parts by weight, the effect of the present invention will not be significant, and if it exceeds 30 parts by weight, a blooming phenomenon may occur, giving undesirable results. The magnetic paint has ferromagnetic powder, a binder, the compound of the present invention, and a coating solvent as its main components, and also contains M5 additives such as a dispersant, a lubricant, an abrasive, and an antistatic agent depending on the type of paint. urge This magnetic coating material is dissolved and dispersed in an organic solvent at a certain ratio and coated on the Bensanju support to form a magnetic layer. Regarding the manufacturing method of magnetic paint, see Japanese Patent Publication No. 35-IFI, No. 39-26794, No. 43-186, No. 47-28.
No. 043, No. 47-28045, No. 47-28046
All No. 47-28048, No. 47-31445, No. 48-11162, No. 48-21331, No. 48-
No. 33683, West German Patent Publication No. 2060655, and other publications (detailed). Magnetic powders that can be used in the magnetic recording medium according to the present invention include r-Fe20s and CO-containing r-Fe203. , C
O covered -r -F e20. ,, Fe3O4, Co-containing - oxide-based magnetic powder such as Fe304, Cr02, Co
Ni-Fe alloy, Fe-Mn-Zn alloy, Fc-NiZ
n alloy, Fe-CO-1'lJ 1-Cr alloy, Fe-
Co-N1-P 6 bowls, Ni-C0 alloy, Fe, Ni,
As a binder used in a binder made of metal-based magnetic powder such as Co, conventionally known thermoplastic resins, thermosetting resins, reactive resins, or mixtures thereof can be used. As a thermoplastic resin, the softening device is 150℃ or less, the average molecular weight is 10,000 to 200,000, and the average molecular weight is about 20.
0 to about 2.000, such as J, vinyl V-acetate r4χ vinyl copolymer, vinyl chloride-vinylidene chloride copolymer, vinyl chloride-acrylonitrile copolymer,
Acrylic ester-acrylonitrile copolymer, acrylic ester-vinylidene chloride copolymer, acrylic ester-styrene copolymer, methacrylic ester-acrylonitrile copolymer, methacrylic ester-vinyltene chloride copolymer, methacrylic acid Ester-acrylonitrile copolymer, methacrylic ester-vinylidene chloride copolymer, methacrylic ester-styrene copolymer, urethane elastomer, polyvinyl fluoride, JA vinylidene-acrylonitrile copolymer, acrylonitrile-butadiene copolymer, Polyamide resin, polyvinyl butyral, cellulose derivatives (cellulose acetate butyrate, cellulose diacetate, cellulose diacetate, heptalulose gropionate, nitrocellulose, etc.), styrene-butadiene copolymer, polyester, chlorovinyl ether-acrylic ester Copolymers, amine resins, thermoplastic resins of various synthetic rubber threads, and mixtures thereof are used. These resins are disclosed in Japanese Patent Publications Nos. 38-6877 and 39-1.
No. 2528, No. 39-19282, No. 40-5349
Gin, No. 40-20907, No. 41-9463, No. 4
]-14059 No. 4]-16985 No. 42-6
No. 428, No. 42-11621, No. 43-4623, No. 43-15206, No. 44-2889, No. 44
-17947, 44-18232, 45-14
No. 020, No. 45-14500, No. 47-18573
No. 47-22063, No. 47-22064, No. 47-22068, No. 47-22069, No. 47-
22070, U.S. Pat. No. 48-27886, U.S. Pat. No. 3,144,352, U.S. Pat. No. 3,419.420, U.S. Pat. has been done. The thermosetting resin or reactive resin has a molecular weight of 200.00'0 or less in the state of a coating liquid, and after coating and drying, the molecular weight becomes infinite due to reactions such as condensation and addition. In addition, among the amazing resins, the resin has a high heat content.
Preferably, it does not soften or melt during the process. Specifically, examples include phenol resins, epoxy resins, polyurethane 7/curable resins, urea resins, melamine resins, alkyd resins, silicone resins, acrylic reactive resins, mixtures of high molecular weight polyester resins and isocyanate fluoropolymers, and methacrylates. Mixtures of polymers and diisocyanate prepolymers, mixtures of polyester polyols and polyisocyanates, urea porno, aldehyde resins,
These lti fats, which may be mixtures of low molecular weight glycols/polymer diaryls/triphenylmectun triisocyanate, polyamine resins, and mixtures thereof, are described in Japanese Patent Publication No. 39-8103, 4F.
No. 9779, No. 41-7192, No. 4]-8016, No. 41-14275, No. 42-18179, No. 4
No. 3-12081, No. 44-28023, No. 45-1
No. 4501, No. 45-24902, No. 46-1310
No. 3, No. 47-22067, No. 47-22072,
No. 47-22073, No. 47-28045, No. 47
No. 728048, No. 47-28922, U.S. Patent No. 3
．． No. 144,353, No. 3320.090, No. 3,437,510, No. 3,597,273, No. 3,781,210, No. 3,731. ．． No. 211, described in the specification. These binders may be used alone or in combination, and other additives may be added as necessary.5 The mixing ratio of the ferromagnetic powder and the binder is 100 parts by weight of the ferromagnetic powder to 100 parts by weight of the binder. 10-400 East'M, preferably 30-2
00 parts by weight. If the binder is too large, the recording density of the magnetic recording medium will be lowered, and if the binder is too small, the strength of the magnetic layer will be poor, resulting in undesirable situations such as decreased durability and powder falling off. In addition to the above-mentioned binder and fine ferromagnetic powder, additives such as a dispersant, a coupling agent, a lubricant, an abrasive, an antistatic agent, etc. may be added to the magnetic paint for forming the magnetic layer. The dispersants used include caprylic acid, cuffric acid,
Fatty acids with 12 to 18 carbon atoms (H4
C0OH, I (alkyl group having 11 to 17 carbon atoms)
: A soap made of alkali metals (Li, Na, etc.) or alkaline earth metals (MgCa, Ba, etc.) of the above-mentioned fatty acids: Lecithin, etc. are used. In addition to these, primary alcohols having 12 or more carbon atoms and sulfuric esters can also be used. These dispersants are added in an amount of 1 to 20 parts by weight per 100 parts by weight of the binder. These dispersants are published in Japanese Patent Publication No. 39-28369. As a coupling agent, it may be used in combination with a known titanate coupling agent, disilane coupling agent, or the like. A preferred coupling agent is a titanate coupling agent, and when used in combination with the compound according to the present invention, the dispersibility of the magnetic layer or magnetic paint of a magnetic recording medium is significantly improved. Among titanate coupling agents, 6! '11'
. It is preferable to use a titanate-based coupling agent with 6-coordination, and a titanate-based coupling agent with 6-coordination, which is a compound (R1 and IP is straight 4・I] or 1
y', d' 1:10, or R1 is a linear or branched saturated alkyl group, and W represents an aryl group. ) is preferred. Examples of this compound include the following (1) and (2). m-tetraisopropylbis (dioctyl osphite)
Titanate (2) Tetraoctyl bis(ditridecyl phosphite) titanate (to It,, 0% TI[P(-00,,)), o
r+ ]. Lubricants include silicone oil, graphite, molybdenum disulfide, tungsten disulfide, fatty acid esters consisting of monobasic fatty acids with 12 to 16 carbon atoms and monohydric alcohols with 3 to 12 carbon atoms, and fatty acid esters with 17 or more carbon atoms. Monobasic fatty acid and the total number of carbon atoms of the fatty acid are 21.
Fatty acid esters consisting of ~23 monohydric alcohols, etc. can be used. These lubricants are added in an amount of 02 to 2D parts by weight based on the binder 1001 stitches. These are described in Japanese Patent Publication No. 43-23889. Materials commonly used as abrasives include fused alumina, silicon carbide, chromium oxide, colander, synthetic diamond, diamond, synthetic corundum, garnet,
Emery (main components: colander J. and magnetite) is used. These sharpening = 'i agent 4, average particle 0.0
A size of 5 to 5μ is commonly used, and tr'J is preferably 021 to 2μ. These 411 prefecture materials are added in an amount of 1 to 20 tau I- to 100 t of the binder. These a) 11th decision is 11th Kaida 49-L155] No. 0 + 14, U.S. Keke No. 3,00
7.807 Shiha No. 3,041,196, No. 3,6
No. 87,725, British Q'+r Permit No. 1.145, 3.4
No. 9, West Germany special it'F (1) 'J,' PS
) No. 853,211 specification νjK is described. 4'l'T''m, inhibitors include graphite, carbon black, tin oxide-antimony oxide thread compound, tin oxide-titanium oxide-antimono oxide compound, carbon black graft polymer, etc. Natural surfactants such as Zaboni/Nonionic surfactants such as alkylene oxides, glycerin threads, glycidol threads, etc.: Higher alkyl amines, quaternary ammonium salts, pyridine, other ?J, elementary ring forces ( , phosphonium or sulfonium forces (such as cationic surfactants: carboxylic acid, sulfonic acid, phosphoric acid, sulfate ester groups,
Anionic surfactants containing acidic groups such as phosphate ester groups, diamino acids, aminosulfonic acids, amphoteric surfactants such as sulfuric acid of amino alcohols or Nisder phosphates, and the like are used. A surfactant that can be used as an inhibitor in these bands
, U.S. I. No. 2,271,623, U.S. No. 2,240
．． No. 472, No. 2,288,226, No. 2,67
No. 6,122, No. 2,676.924, No. 2,6
No. 76,975, No. 2.6 'J 1,566, No. 2,727.860, No. 2,730.49 s.
) No. 2,742.379, No. 2,739. )!
No. 91, same No. 3. (No. 168,101, No. 3,158
, No. 484, No. 3.2 (l +, No. 253, No. 3.210.191, No. 3,294.54 i1, No. P13J3, 15,649, No. 3.441, 4
No. 13, No. 3,442,654, OLS No. 1,942,665, British Patent No. 1,
077, 3 J No. 7, 1,198,450, etc., 1 J・1) by Ryohei et al. [Synthesis of surfactants and their applications Jl (Soten 1964 edition): A,
W. Bayley, ``Surface Active Agents 1958 Edition'': TP Sisley, ``Encyclopedia of Surface Active Agents Vol.
2016 edition): [Surfactant Handbook J 6th edition (Sangyo Tosho Co., Ltd., December 20, 1960), etc. is described in the adult diseases. These surfactants may be added alone or in combination. Although these are used as antistatic agents, they are sometimes used for other purposes, such as dispersion, improving magnetic properties, improving lubricity, and as coating aids. The magnetic layer is formed by adding niI'l in an organic solvent with the above composition.
(The coating solution is applied onto a non-rutting support. Organic solvents used during coating include ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, and cyclohexanone; methanol, ethanol, propatool, and butanol. Alcohol threads such as methyl acetate, ethyl acetate, butyl acetate, ethyl lactate, esters such as glycol monoethyl acetate, glyco-ethers such as nigericol dimethyl, glycol monoethyl nitrate, dioxane, etc.: pensene, toluene, Tar-based (aromatic hydrocarbons) such as xylene: methylene chloride,
Ethylene chloride, 4JQ+carbon, chloroform,
KM hydrogenated hydrocarbons such as dichlorobenzene can be used. Materials for the support include polyesters such as polyethylene fucrate and polyethylene-2,6-naphthalate, polyolefins such as ylinolobilene 49, cellulose triacetate and cellulose diacetate, and polycarbonate. Norastinok, Cu, A! , gold L4 such as Zn, glass, etc. J! The thickness of these supports is approximately 3 to 100 millimicrons in the case of a film or sheet, preferably 5 to 50 millimicrons, and % in the case of a disk or card. It has a power of 30 mm and 3069 mf to 10 mm mW, and if it is drum-shaped, it is cylindrical, and the type is determined depending on the recorder used. The above-mentioned support may be coated with a magnetic layer (T3ackcoat) for the purpose of supporting Teibako 1, preventing transfer, etc. For example, the American 9-year-old π ``ga'32
No. 804.401, No. 3,293,066,
Same No. 3.617,378, Same No.: U (162,676
No. 3,734,772, No. 3,476,59
No. 6, No. 2,643,048, No. 2,803.
No. 556, No. 2.387,462, No. 2.923
, No. 642, No. 2,997,451, No. 3,00
No. 7,892, No. 3,041.196, No. 3,1
No. 15,420, I', R3, 166,688, etc. IIIW. Further, the form of the support may be any one of tenips, sheets, cards, tissues, drums, etc., and the material must be selected depending on the form. (Magnetic powder and the aforementioned binder, dispersant, lubricant,
! I W'l, 'Ik 1 ton inhibitor, solvent, etc. are kneaded to form a magnetic paint. During kneading, the magnetic powder and each of the above-mentioned components are fed into a kneading machine either simultaneously or individually. For example, there is a method in which magnetic powder is first added to a solution containing a dispersant and kneaded for a predetermined period of time, and then the remaining components are added and kneading is continued to obtain a magnetic paint. For crosstalk dispersion, various types of crosstalk are used. For example, two-roll mill, three-roll mill, pebble mill, sand grinder, Szegvari attritor, high-speed impeller dispersion machine, high-speed stone mill, high-speed impact mill, These include Tisfu Kuichi-der, high-speed mixer, homogenizer, ultrasonic dispersion machine, etc. Technology related to crosstalk dispersion is provided by T.C.PA'l'TON.
AuthorPaint Flow and Pigment
Dispersion (1964 John
The U.S. WF No. 2, 5 8 1, 4 1 4 mentioned in Wiley &Son's
No. 2, No. 855, and No. 156. Application of the magnetic coating material onto the support 1 - Coating methods for forming a magnetic layer include air knife coating, air knife coating, Flavinite coating, lino-throll coating,
Gravure coat, transfer roll coat 1, kiss coat, cast coat, spray coat, etc. can be used, and other methods are also possible, and detailed explanations of these can be found in "Coating Engineering" (published by Asakura Shoten in 1971). It is written. The magnetic layer coated on the support by such a method is dried while subjecting the magnetic powder in the layer to an orientation treatment if necessary. In addition, if necessary, the magnetic layer may be subjected to surface smoothing treatment or to the desired surface. Manufacture a magnetic recording medium by cutting it into shapes. In this case, the orientation magnetic field is approximately 500 to 35
It is preferable that the drying temperature is about 0.00 Gauss, the drying temperature is about 50 to 100°C, and the drying time is about 3 to 10 minutes. The magnetic recording medium produced as described above and containing the compound according to the present invention in the magnetic layer has improved dispersibility of the magnetic powder in the V = magnetic layer, resulting in improved magnetic surface properties, i(F output, Performances such as abrasion resistance and adhesion were significantly improved.The present invention will be specifically explained below with reference to Examples and Comparative Examples. Examples 1 to 5 Among the compounds of Hikari-1, five compounds each of 4) and 5) were prepared in separate batches. Dilute 500 parts of methanol, add 1 inch of co-containing Fe3Q magnetic powder to each of the methanol solutions shown in Table 2 below.
Add 00 copies each! 5 mixtures were dispersed. Next, this dispersion, liquid filtration, natural drying, and drying under reduced pressure at 80°C were performed. S powder was prepared. Table 2 Thereafter, a small amount of the above-mentioned treated magnetic powder was collected and flashed in a water-toluene system, and the treated magnetic powder was completely transferred to the organic layer. It was found that the surface of the magnetic powder was modified by the untreated magnetic powder remaining in the water layer. The treated magnetic powder described in Table 2, % I
-1, I-2, 1-3, I-4 and 1-5,
A magnetic paint was prepared with the following composition. (Composition) Treated magnetic powder 90 parts Vinylidene chloride-acrylonitrile copolymer 16 parts Polyurethane 7 parts Silicone oil
3 part carbon black
3-part methyl ethyl ketone
175 parts of the above composition were placed in a ball mill, thoroughly mixed and dispersed, and a black magnetic paint was obtained. This coating material was applied to one side of a polyethylene terephthalate film with a dry film thickness of 6 microns while applying a 6n field of 2,000 Gauss. The wide magnetic wave (web) obtained in this way was supercalendered, nullified to a width of 12.65 mm, and videotape, f6 I-1 ~
, % I-5 was obtained. Examples 6 to 10 In the compound of the coating-1, /161), 2 pieces 3), 4)
Five of each of the compounds in 5) were diluted in 500 parts of separate methanol, and 00 parts of Fe-Ni-CoI powder was added to each of the methanol solutions as shown in Table 5. , the mixture amount was 11 times. Thereafter, this dispersion was filtered, air-dried, and then dried under reduced pressure at 80° C. to produce treated magnetic powder. Table 5 Processed magnetic powder obtained by
．． Magnetic paints were prepared using 1J-3, II-4 and 11-5 with the following composition. (Composition) Treated magnetic powder 75 parts Partially hydrolyzed vinyl-vinyl acetate 7.5 H1i polyurethane 7.5 parts Silicone oil 1.5 parts Methyl ethyl ketone 70 parts Toluene
60-19 cyclohexanone
After 5 parts of the above composition was placed in a ball mill and sufficiently mixed and dispersed, 3 parts of tolylene diisocyanate was added and mixed uniformly to obtain a magnetic paint. This magnetic paint was applied to one side of a polyethylene terephthalate film having a thickness of 15 microns while applying a magnetic field of 2,000 Gauss to a dry film thickness of 5 microns. The thus obtained wide magnetic wave was applied to magnetic tapes 16N, -1 to atB by the same treatment as in Examples 1 to 5.
-5 was created. Example 11 (Composition) Untreated magnetic powder (Co-containing Fe30 = magnetic powder) 9
0 parts vinylidene chloride-acrylonitrile copolymer 16
7 parts polyurethane 7 parts carbon black 3 parts compounds (Table -
1,16,1 compound) 3 parts methyl iso, butyl ketone 75 parts methyl ethyl keto/
The composite having 175 parts was placed in a poultry mill, and after thorough mixing and dispersion, a black magnetic paint was obtained. Using this magnetic paint, a 12.65 mm to 1'' videotape was prepared in the same manner as in Examples 1 to 5. This tape is called f611. Comparative Example 1 In producing magnetic paint, instead of using Co-containing Feρ and magnetic powder as in JA++ Examples 1 to 15, magnetic powder (processed l! I! magnetic powder) previously treated with the compound of the present invention was used. In addition to using untreated Co-containing Fe, O, i magnetic powder,
A 12.65 mm 1'' videotape was prepared by performing the same treatment as in Examples 1 to 5, and this 12.65 mm videotape was used as Comparison 16 I-1. Comparative Example 2 Instead of using Fe-Ni-Co magnetic powder surface-treated with the compound of the present invention as in Examples 6 to 10, untreated Fe
Hoga using -Ni-Co magnetic powder was subjected to the same treatment as in Examples 6 to 10, and
I made a videotape of LJ. Compare this tape/f
611-2. Comparative Example 3 (Composition) Untreated Co-containing Fe3 o4fdi powder
90 f, ll vinylidene chloride-acrylonitrile copolymer 16g1 (polyurethane
7 parts carbon black
3 parts lecithin 5 parts methyl isobutyl ketone 75 parts notyl ethyl ketone 175 parts The above composition was placed in a ball mill and thoroughly mixed and dispersed to obtain a black magnetic paint. Using this magnetic paint, a videotape with a width of 12.65 mm was prepared by carrying out the same treatment as in Examples 6 to 10. This tape is called I-3. Comparative Example 4 (Composition) Untreated Fe-Ni-Cola magnetic powder 7
5 parts partially hydrolyzed lvf vinyl chloride-vinyl acetate combination 7.5 parts polyurethane resin 7 7.
5 parts Lecithin 5 parts Methinoethyl, ketone 70 parts Toluene 60@ds cyclohexanone 5 parts The above composition was placed in a ball mill and thoroughly mixed and dispersed to obtain a magnetic paint. Using this magnetic paint, a videotape of 12.65 mm rlJ was produced by performing the same treatment as in Examples 6 to 10. This tape is referred to as Comparison/I611-4. Comparative Example 5 A 12.65 mm 11] videotape was prepared in the same manner as in Example 11, except that dioctyl was used instead of the compound in Table 1, No. 5. The results of comparing this tape with Comparison/16I, -5 are shown in Table 6 below. However, 1. (a) Squareness ratio Residual magnetization f3r/' Saturation magnetization Bm ()
+1 Surface property The surface property indicates the value of the average roughness at the center of the sample F light surface measured using a surface roughness meter. (c)■)'Output Using a VTR deck for measuring RF output, 4 Ml-1z
The RF specific output was measured and expressed as a relative value with the RF specific output O as the comparison/%I-1. (d) Using a wear-resistant simulated head to record a 5m long videotape at 7ny's
The tape was repeatedly slid back and forth at a speed of ec, and the subsequent tape surface was judged visually and using a microscope. (e) Adhesion Adhesion was determined by the development of adhesion after being left for 24 hours at a humidity of 80% and a temperature of 40°C. Margin Table 6 below From the results in Table 6, tapes made with magnetic paints using compounds according to the present invention (for example, compounds in Table 1) are better than magnetic paints made with other dispersants (lecithin). It can be seen that the tape produced using the compound according to the present invention is superior in squareness ratio, surface properties, IIF output, abrasion resistance, and adhesiveness (in the case of the comparative example). Among the magnetic tapes made using 192, it is better to pre-treat the magnetic powder with the nα compound in advance and then create a magnetic paint with a predetermined composition, since the above compound is added together with the magnetic powder when creating the magnetic paint. This shows that better performance can be obtained than when it is produced by incorporating it into a material (16 -
1-1-5 and ;161J-1-■1-5/+611)
. Furthermore, CO-containing Fe50. The tape made from the magnetic paint containing Fe-Ni-Co powder has a higher squareness ratio and RF output than the tape made from the magnetic paint containing magnetic powder, but this is because the magnetic material The above properties are based on the magnetic properties of the material itself.
1-C. The same result is likely to be obtained not only with magnetic powder but also with other magnetic powders, Patent applicant: Konishi Roku Photo Industry FF'The', Kake 1゛Representative Patent attorney: Ichinosho Ayao Procedural amendment (Voluntary) September 21, 1980 Mr. Kazuo Wakasugi, Commissioner of the Patent Office ■ Case description 1982 Patent Application No. 205095 2 Title of invention Magnetic recording medium 3 Relationship with the person making the amendment Case 1 Origin of the patent Personal address: 1-26-2 Nishi-Shinjuku, Shinjuku-ku, Tokyo Name (127) Konishiroku Photo Industry Co., Ltd. 6
Number of inventions increased by amendment None 7. Subject of amendment [1] The scope of the outdated claims in the specification is amended as shown in the attached sheet. [2] The column of detailed explanation of the invention of 1% clarity is amended as follows. (1) Specification, 2nd negative] In the second line, the statement "...heat-resistant properties that cause interlayer adhesion..." is changed to "...heat-resistant properties that cause interlayer adhesion..." . (2) In the 4th line of page 5 of the specification, the statement [...NH or stranded ammonium ion...] was changed to [...NH4
Or organic ammonium ion...J Toss 6° (3)
The statement "...positive integer..." on page 5, line 7 of the detailed description is changed to "...integer...". (4) In the first line of page 6 of the specification, the statement "...NIL, or tied ammonium ion..." was changed to "...NJ
(4" or organic ammonium ion...Jy.
H, CI, ell, CI (, C1N ao, 8-CI-
CCX) CaltCH, OCH, CH, CI, CIl,
The description CIl, CI, CI J is written as . (6) "...of the official gazette" in the sixth line at the bottom of page 12 of the detailed description
A certain description is ``...a compound described in a publication and a compound described simultaneously therewith.'' (7) On page 14, line 10 of the specification, the statement "...steryl alcohol..." has been changed to "...stearyl alcohol... (8) The description "...methyl ethyl ketone" on the second line from the bottom of No. 14, 1700 is changed to "1... methyl ethyl ketone,...". (9) Change the NL entry that says [...polyvinyl butyral...] to [...polyvinyl butyral...] on line 8 of page 21 of the specification to [...J]2).QO) Line 4 of page 26 of the specification 01) Change the statement "...tar type (aromatic hydrocarbon):..." on page 40, line 4 of the specification to "...aromatic carbonization."Hydrogen:...'' θ2) Specification page 40, line 6, 1...Chlorinated hydrocarbon"
A certain description is defined as 1...Halogenated hydrocarbon water. 03) Clear all, aR page 30, line 8, "...polyethylene foam" was changed to "...polyethylene teleph..."
・”. 04) On page 30 of the specification, lines 17-19, “...about 3~
The culm degree is 100 millimeters, fjf or 5 to 50 millimeters, and in the case of disks and cards, it is 30 millimeters to 10 millimeters..." 1
-...about 3 to 100 microns, preferably 5 to 5
0 micron, and in the case of disks and cards, 30
0 microfron to 10 millitorr..." 09 In the specification, page 1, page 32, bottom 2nd line, the statement that says ``...grade coat...'' is changed to ``...blade coat...''. 06) Ming & 111 %4 38th member 6th line from the bottom "...
・Examples 1 to J5..." was replaced with "...
In Examples 1 to 5...''. 07) Restatement of details Delete the statement "In accordance with Examples 6 to 1°..." on page 39, line 3. Ql'll "Table-1" in the first line from the bottom of page 40 of the specification
, N5...'' was replaced with [In Example 1o, Table-1, [East 5...'']. Similar to the description Restatement of details 41 from Sadashita, line 188 1...Example 11...'' was changed to ``...Example 10...''
shall be. (20) Ming+? (Amend Book II, page 43, Including-6, to Table-6 below by 1. A compound represented by
R'' is an alkyl group, substituted alkyl group or alchemol group, l and m are integers from 1 to 10, and 6
7 is 0 or 1. ) A magnetic recording medium comprising a magnetic layer containing: Procedural amendment (voluntary) Mr. Kazuo Wakasugi, Commissioner of the Japan Patent Office ■ Indication of the case 1982 Patent Application No. 205095 3 Relationship with the person making the amendment Patent applicant address 26-2, Nishi-Shinjuku 1-chome, Shinjuku-ku, Tokyo No. M
1″/= (8th name) (127) Konishiroku Photo Industry Co., Ltd. Name (7614) Patent attorney Miyao Ichinose 5,
Date of amendment order (1) From line 1 of the specification No. 23 to page 24, line 1, "... 10 to 400 parts by weight, preferably 30 to 200 parts by weight, of a binder..." A certain description is "...5 to 400 parts by weight of binder, preferably 10 to 200 parts by weight...". (2) In the second line at the bottom of page 24 of the specification: ``...Binder 1
00..." is replaced with "...Ferromagnetic powder 100..."
...''. (3) Details @ 5th line from the bottom of page 26 “...Binder 1
00...'' is replaced with "...Ferromagnetic powder 100
...''. (4) 1 on page 27, line 6 of the specification...Binder 100.
``...'' is replaced with ``...Ferromagnetic powder'100...''
”. that's all

Claims (1)

[Claims] (1) A compound represented by the general formula (where M is a hydrogen atom, an alkali metal, NI (4) or an organic ammonium ion, and R
1 and R2 are each an alkyl group, an It-substituted alkyl group, or an alkenyl group, 1 and Ill are positive integers of 1 to 10, and n is 0 or 1. ) A magnetic recording medium comprising a magnetic layer containing: