JPS59201063A - Developer - Google Patents

Abstract

PURPOSE:To reproduce an image which withstands long-term continuous use and is stable at all times by incorporating fine powder of a silicic acid treated with silicone oil having an amine at the side chain. CONSTITUTION:The silicone oil contg. the constituting unit expressed by the formula is usable as a silicon oil having an amine at the side chain to be used for the treatment of fine powder of a silicic acid. The powder is treated with the silicon oil in such a way that the silicone oil is incorporated at 0.2-70wt% in the entire amt. of the treated fine powder of the silicic acid and at 0.0001- 10wt% in the developer. The treatment is accomplished by a method of spraying the silicon oil or the soln. thereof onto the fine powder of the silicic acid under heating and agitating or blowing the silicone oil thereto after gasifying the same or preparing the silicone oil into a slurry and adding the slurry to the powder under agitating. The image which withstands long-term continuous use and is sharp under high temp. and high humidity as well as under low temp. and high humidity is thus obtd. In the formula, R1 denotes hydrogen, alkyl group, aryl group or alkoxy group, R2 denotes an alkylene group or phenylene group, and R3, R4 denote, hydrogen, an alkyl group or aryl group.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a developer for developing latent images in electrophotography, electrostatic recording, electrostatic printing, magnetic recording, and the like. More specifically, the present invention relates to an electrophotographic developer that is uniformly and strongly positively charged, visualizes a negative electrostatic charge image, and provides a high-quality image in a direct or indirect electrophotographic development method.

As a conventional electrophotographic method, U.S. Patent No. 2,297,691
Although a number of methods are known, such as those described in No. (hereinafter referred to as toner), the toner image is transferred to a transfer material such as paper as necessary, and then fixed by heat, pressure, solvent vapor, etc. to obtain a copy. Furthermore, when a process for transferring a toner image is included, a process for removing residual toner on the photoreceptor is usually provided.

Development methods for visualizing electrical latent images using toner include, for example, the magnetic brush method described in U.S. Pat. No. 2,874,063, and the magnetic brush method described in U.S. Pat. No. 2,618,552. Cascade development method and 2,221,7
Powder cloud method described in US Pat. No. 76, U.S. Pat.
, 909,258, which uses conductive magnetic toner, is known.

The toners used in these developing methods have conventionally been fine powders in which dyes and pigments are dispersed in natural or synthetic resins. For example, particles obtained by dispersing a colorant in a binder resin such as polystyrene and pulverizing the particles to about 1 to 30 μm are used as toner. As the magnetic toner, one containing magnetic particles such as magnetite is used. In the case of a system using a so-called two-component developer, the toner is usually made of glass,
It is used mixed with carrier particles such as iron powder.

Positive charge control agents used in such dry developing toners generally include, for example, quaternary ammonium compounds and organic dyes, particularly basic dyes and their salts. Common positive charge control Mlls include pencil dimethyl-hexadecyl ammonium chloride, decyl-trimethyl ammonium chloride, nigrosine base, nigrosine, safranin γ and crystal violet.

In particular, nigrosine base and nigrosine, which is often used as a positive charge control agent, are usually added to thermoplastic resins, melted and dispersed under heating, and then finely pulverized. The particle size is adjusted and used. However, these dyes used as charge control agents have complex structures, inconsistent properties, and poor stability. In addition, it is easily decomposed or deteriorated due to decomposition during thermal kneading, mechanical impact, friction, changes in temperature and humidity conditions, etc., and tends to cause a phenomenon in which charge controllability is deteriorated.

Therefore, when toner using these charge control agents is used in a copying machine for development, as the number of copies increases, the charge control agent decomposes or changes in quality, which may cause deterioration of the toner during durability.

Further, many positive charge control agents are hydrophilic, and due to poor dispersion in these resins, the control agent is exposed on the toner surface when the toner is crushed after bath melt-kneading. Therefore, when the toner is used under high humidity conditions, it has the disadvantage that good quality images cannot be obtained because these control agents are hydrophilic.

In this way, when conventional positive charge control agents are used in toner, charge control agents are generated on the surface of toner particles between toner particles, between toner and carrier, or between toner and toner carriers such as sleeves. This causes variations in the amount of charge that
Development unit 1 Problems such as toner scattering and carrier contamination are likely to occur. Furthermore, this problem becomes more noticeable when a large number of copies are made, and the result is that the copying machine is not suitable.

Furthermore, under high humidity conditions, the transfer efficiency of toner images decreases significantly, and many of them become unusable. Furthermore, even at room temperature and humidity, when the toner is stored for a long time,
Deterioration occurs due to the instability of the positive charge control agent used,
Often unusable.

Furthermore, Japanese Patent Publication No. 53-22447 proposes a method for obtaining a developer with positive charge control properties.

This is a method in which metal oxide powder treated with aminosilane is contained as a component of the developer, but a detailed study of this method revealed that various aminesilane compounds were used, such as colloidal silica, alumina, dioxide, etc. When titanium, zinc oxide, iron oxide, γ-ferrite, magnesium oxide, etc. are treated and a developer is obtained according to the examples described in the specification, any combination has sufficient properties for practical use. It was not possible to obtain a developer exhibiting this, and it became clear that there were several drawbacks.

That is, many developers fail to maintain desirable properties for faithfully reproducing a deposited image. Even products that initially exhibit desirable performance may fail to retain their initial characteristics after long-term continuous use.
It becomes unusable. That is, capri occurs, toner scatters around edges when copying line drawings, and image density also decreases. Other drawbacks are:
When developing and transferring under high temperature and high humidity environmental conditions, a decrease in image density, scattering of line drawings, white spots, fogging, etc. may occur.

An object of the present invention is to provide a developer having positive chargeability.

A further object of "Non-explosion 1J7" is to provide a developer that maintains its initial characteristics even when the developer is used continuously for a long period of time, and that causes no toner aggregation or change in charging characteristics.

Another objective is to develop a developer that reproduces stable images unaffected by changes in temperature and humidity, especially a developer with high transfer efficiency that does not cause splatters or transfer omissions during transfer at high or low humidity. The aim is to provide agents for

Still another object is to provide a developer with excellent storage stability that maintains its initial characteristics even during long-term storage.

Its feature lies in the developer containing fine silicic acid powder treated with silicone oil having an amine in its side chain.

As the silicic acid fine powder constituting one of the constituent components of the developer in the present invention, silicic acid fine powder produced by a dry method or a wet method can be used.

The dry method mentioned here is a method for producing fine silica powder produced by vapor phase oxidation of a silicon halide compound. For example, this method utilizes the thermal decomposition oxidation reaction of silicon tetrachloride gas in a sour hydrogen flame, and the basic reaction formula is as follows.

5iCt4+2H, + 02-+ 5in2+4Hct
Also, in this manufacturing process, for example, by using other metal halide compounds such as aluminum chloride or titanium chloride together with a silicon halide compound, a composite fine powder of silica and other metal oxides can be produced. It is also possible to work hard, and it includes these as well.

Commercially available silica fine powder produced by vapor phase oxidation of a silicon halogen compound used in the present invention includes, for example, those commercially available under the following trade names.

00 80

For example, the decomposition of sodium silicate with an acid can be expressed by the general reaction formula (the reaction formula is omitted below): Na,0 ・XSiO2+Hct+H20-)Si02
・nH2O+Nact Other methods include decomposition of sodium silicate with ammonia salt M or alkali salts, a method of generating alkaline earth metal silicate from sodium silicate and then decomposing it with acid to form silicic acid, thorium silicate There are methods such as converting the solution into silicic acid using an ion exchange resin, and methods using natural silicic acid or silicate.

As the silicic acid fine powder referred to herein, any of anhydrous silicon dioxide (silica) and other silicates such as aluminum silicate, sodium silicate, potassium silicate, magnesium silicate, and zinc silicate can be used.

Commercially available fine silicic acid powders synthesized by a wet method include those sold under the following trade names, for example.

Carplex Shionogi Nibu Seal Nippon Silica Toxeal, Fine Seal Tokuyama Soda Vita Seal
Takihiki Jiruton, Silnetux Mizusawa Kagaku Starsil Shinshin Kagaku Himezil Ehime Pharmaceutical Thyroid Fuji Davison Kagaku Hi-8
il (high seal) Pittsburgh
Plate GlassCo, (Pittsburgh plate glass) 1) urosil F
iillstoff-GesellschaftUlt
Rasil (Ultra Seal) Marquard (,;
'-'-#2) 77-&-v-leshaft Marquardt) Manosil Hardman
and Ho1den Hoesch Chemisc
he Fabrik HoeschK-G Sil-5tone 5t
oner Rubber Co.

(Stoner Lover) Na1co (Nalco) Na1co Che
m, Co.

(Narco Chemical) Quso (shoes) Ph1ladelph
ia Quartz Co.

(Filatelfire Quartz) Santocell Monsanto,
Chemical Co.

(Monsando Chemical) Imsil l1linoi
s Minerals Co.

(Illinois Mineral) Calcium 5ilikat Chemi
sche Fabrik Hoesch.

(Calsilano, Silicato) K-c (Hiemitsussie Fabrikhetsch) Calsil (Calsil) Fiillsto
ff-GesellschaftMarquard
(Fortafil) Imperia
l Chemical Industries Ltd, (
Imperial Chemical Industries) Microcal Josep
h Crosfield &5ons, Ltd.

(Jiesse 7 Crossfield and Sons) Manosil Hardman
and Ho1den (Hardman and Ho-
Vulkasil Farb
Enfabriken Bryer, A, -G, (Falpenfabriken Bryer) Tufknit (
Tough knit) Durham Chemical
s, Ltd.

(Doulham Chemicals) Silmos Shiraishi Kogyo Starex Shinshin Kagaku Fricosil Tagihii Among the above silicic acid fine powders, the specific surface area due to nitrogen adsorption measured by the BET method is 30 mVg or more (especially 50 to 40 mVg).
0 m+Vg) gives good results.

Conventionally, it is known that fine silica powder produced by vapor phase oxidation of a silicon halide compound is added to a developer. However, even in a developer containing a dye having positive charge control properties, when such silica is added, the chargeability changes to negative, making it unsuitable for visualizing a negative electrostatic charge image. Therefore, as a result of researching the above phenomenon, it was found that silica fine powder (generated by conventional vapor phase oxidation of silicon halogen compounds) reduces the charge of positively charged developer,
Or reverse the polarity and find each car. In order to obtain a developer that exhibits more stable and uniform positive chargeability, detailed studies revealed that it is effective to treat fine silicic acid powder with a silicone oil that has an amine in its side chain and incorporate it into the developer. I found out something.

As the silicone oil having an amine in the side chain used in the treatment of the above-mentioned silicic acid fine powder, a silicone oil containing a hexane unit represented by the formula (1'1) can be used.

1 5i-0- sign R2-...Formula (1) (where, horse represents hydrogen, an alkyl group, an aryl group, or an alkoxy group, R2 represents an alkylene group, a phenylene group, and R,, R, Represents hydrogen, an alkyl group, or an aryl group.However, the above alkyl group, aryl group, alkylene group, and phenylene group may contain an amine, or a substituent such as halogen to the extent that the chargeability is not impaired. ) Preferred commercially available silicone oils having an amine in their side chains include, for example, amine-modified silicone oils represented by the following structural formula. (Here, R,, R, represents an alkyl group, an aryl group, R2 represents an alkylene group, a phenylene group, or an alkyl group including an amine, % RA represents hydrogen, an alkyl group, an aryl group.m%n is a number of 1 or more.) Specifically, the following are preferred, and these may be used alone or in a mixed system of two or more.

Amine, equivalent at 25°C Product name Viscosity (cps) SF84
17 (manufactured by Tone Silicone) 120 (1
3500KF393 (manufactured by Shin-Etsu Chemical)
60 360KF857 (manufactured by Shin-Etsu Chemical)
70 830Kxrsc;o
(Manufactured by Shin-Etsu Chemical Co., Ltd.) 250 7601
)KF'861 (manufactured by Shin-Etsu Chemical Co., Ltd.) 35
00 2000KF862 C4n Etsukajisha)
'750 1900KF864 (
(Manufactured by Shin-Etsu Chemical) 170 (J 380
0KFS65 (manufactured by Shin-Etsu Chemical)'
90 4400KF369 (Shin-Etsu Chemical Dan)
20 320KF383 (manufactured by Shin-Etsu Chemical) 20 320X-2
2-3680 (manufactured by Shin-Etsu Chemical) 90 88
00X-22-380D (manufactured by Shin-Etsu Chemical) 2
3 (103s o.

X-22-38010 (manufactured by Shin-Etsu Chemical Co., Ltd.) 350
0 3800
) is the value obtained by dividing the molecular weight by the number of amines per molecule.In the present invention, the amount of silicone oil having an amine in the side chain treated is 0 of the total amount of treated silicic acid fine powder.
．． 2-70% by weight, o, o o in developer
It is preferable to adjust the amount to 10% by weight. Furthermore, the appropriate amount of silicone oil having an amine in the side chain to be treated is determined by setting the amount of silicone oil to be used as When the specific surface area of the acid fine powder is bm2/g and the amine equivalent of the silicone oil having an amine in the side chain is a, particularly good results are obtained when the relationship of formula (I) is satisfied.

In the above formula, if X>-, the silicone oil with an amine in the side chain is in large excess relative to the silicic acid fine powder, and the silicone oil with an amine in the side chain oozes out from the silicic acid fine powder. This may cause problems. Also 'X<
In the case of 30,000, the chargeability is insufficient and it becomes difficult to achieve the object of the present invention.

On the other hand, 25° of silicone oil with amine in the side chain
The viscosity at C is preferably 5000 cps or less, particularly,
3000 cps or less is preferable. Viscosity is 5000c
If it is more than ps, the silicone oil having amine in the side chain will not be sufficiently dispersed into the silicic acid fine powder, which may easily cause defective images such as P1 fog. The treatment with the silicone oil having the following can be carried out, for example, as follows. The silicic acid fine powder is vigorously agitated while being heated if necessary, and the above-mentioned silicone oil/+/ having an amine in the side chain or its solution is sprayed or vaporized onto it, or the silicic acid fine powder is sprayed or vaporized. The treatment can be easily carried out by turning the fine powder into a slurry and adding a silicone oil having an amine in the side chain or a solution thereof while stirring the slurry.

In the present invention, one type or a mixture of two or more types of silicone oils may be used from among the above-mentioned silicone oils having amines in their side chains.

In addition, the applied amount of these treated silicic acid fine powders exhibits an effect when the amount is 0.01 to 20% based on the weight of the developer, and it is especially effective when added to 0.03 to 3%. It exhibits positive chargeability with excellent stability. A preferable addition form is 0.01 to 0.01 to the amount of developer N.
It is preferable that 5% by weight of the treated silicic acid fine powder be attached to the surface of the toner particles.

In addition, the silicic acid fine powder used in the present invention may be further treated with a conventionally known hydrophobizing agent, if necessary.
A known method is used for this purpose, and it is applied by chemically treating with an organosilicon compound that reacts with or physically adsorbs silicic acid fine powder.

Examples of such organosilicon compounds are hexamethyldisilazane, trimethylsilane, trimethylchlorosilane, trimethylethoxysilane, dimethyldichlorosilane, methyltrichlorosilane, allyldimethylchlorosilane,
Allyldimethylchlorosilane, penzyldimethylchlorosilane, fromomethyldimethylchlorosilane, α-chloroethyltrichlorosilane, β-chloroethyltrichlorosilane, chloromethyldimethylchlorosilane, triorganosilylmercaptan, trimethylsilylmercaptan, triorganosilylacrylate, Vinyldimethylacetoxysilane, dimethylethoxysilane, dimethyldimethoxysilane, diphenyljethoxysilane, hexamethyldisiloxane, 1,3-divinyldito2methyldisiloxane, 1,3-diphenyltetramethyldisiloxane, and from 2 per molecule It has 12 siloxane units and one Si is attached to each unit located at the end.
There are dimethylpolysiloxane and the like containing a hydroxyl group bonded to. These may be used alone or in a mixture of two or more.

According to the present invention, when a developer containing fine silicic acid powder treated with silicone oil having an amine in the side chain is used, the triboelectric charging of the developer becomes stable, and uniform positive charging is achieved even under various environments. It becomes like showing. Therefore, when the developer according to the present invention is used, clear high d' without capri! It is possible to obtain images of S degree, and furthermore, there is no image deterioration even when used continuously for a long period of time, and clear images can be obtained even under high temperature and high humidity conditions and low temperature and low humidity conditions.

As the binder resin of the toner that can be used in the present invention, c. a monopolymer of styrene and its substituted products such as polystyrene, polyP-chlorostyrene, and polyvinyltoluene;
P-chlorostyrene copolymer, styrene-propylene copolymer, styrene-vinyltoluene copolymer, styrene-vinylnaphthalene copolymer, styrene-methyl acrylate copolymer, styrene-ethyl acrylate copolymer,
Styrene-butyl acrylate copolymer, styrene-octyl acrylate copolymer, styrene-methyl methacrylate copolymer, styrene-ethyl methacrylate copolymer,
Styrene-butyl methacrylate combination, styrene-α
methyl methacrylate copolymer, styrene-acrylonitrile copolymer, styrene-vinyl methyl ether copolymer, styrene-vinyl ethyl ether copolymer, styrene-vinyl methyl ketone copolymer, styrene-
butadiene copolymer, styrene-isoprene copolymer,
Styrenic copolymers such as styrene-acrylonitrile-indene copolymer, styrene-malein H co-M copolymer, and styrene-maleic acid ester copolymer; polymethyl methacrylate, polybutyl methacrylate, polyvinyl chloride, polyvinyl acetate, polyethylene , polypropylene, polyester, polyurethane, polyamide, polyvinyl butyral, polyacrylic acid resin, rosin, modified rosin, terpene resin, phenolic resin, aliphatic or alicyclic hydrocarbon resin, aromatic petroleum resin, chlorinated paraffin,
Paraffin wax etc. can be used alone or in combination.

Colorants used in the developer of the present invention include known dyes and pigments, such as carbon black, phthalocyanine blue,
It can be widely used such as Indan Stremburu, Hekotok Blue, Permanent Red, Lake Red, Rhodamine Lake, Hansa Yellow, Permanent Yellow, and Benzidine Yellow.

In order to use the developer of the present invention as a magnetic l/toner, it may contain magnetic powder. As such magnetic powder, materials that are magnetized when placed in a magnetic field are used, such as iron,
These include powders of ferromagnetic metals such as cobalt and nickel, and alloys and compounds such as magnetite, hematite, and ferrite. The content of this magnetic powder is 1% per toner weight.
It is 5 to 70% by weight.

The toner is optionally mixed with carrier particles such as iron powder, glass beads, nickel powder, ferrite powder, etc., and used as a developer for the electrical latent image.

The developer of the present invention can be applied to various development methods. For example, a magnetic brush development method, a cascade development method, a method using a conductive magnetic toner described in U.S. Pat. A method using
4-42], Publication No. 21, Publication No. 55-18656,
Examples include the method described in Japanese Patent Publication No. 54-43027, a fur brush development method, a powder cloud method, a touchdown development method, an impression development method, and the like.

[Example 1] 100 parts by weight of styrene-butel methacrylate-dimethylaminoethyl methacrylate (weight ratio 7:2.5:0.5) copolymer, 60 parts by weight of magnetite, and 3 parts by weight of polyethylene wax were mixed. , melt and knead in a roll mill. After cooling, it is coarsely pulverized using a hammer mill, and then finely pulverized using a jet pulverizer. Next, it was classified using an air classifier to obtain black fine powder with a particle size of about 5 to 20 μm.

On the other hand, 100 parts by weight of silicic acid fine powder synthesized by a dry method (trade name, Aerosil +130, specific surface, approximately 130 nlVg manufactured by Aerosil) was stirred and the temperature was maintained at approximately 250'C to form side chains. Silicone oil with amine (viscosity 70 (141) 8% at 25 °C
20 parts by weight of amine equivalent (830) were sprayed and treated for 10 minutes.

To 100 parts by weight of the black fine powder, 0.4 parts by weight of the silicic acid fine powder treated with the silicone oil having an amine in the side chain was added to prepare a toner.

Apply this toner to a commercially available copier (product name: Minicopia PC2).
0, manufactured by Canon Inc.), a clear image without capri was obtained, and the image reflection density was 1.15.
Met. Furthermore, in order to examine the durability of the developer, a durability test of 10,000 sheets was performed, and a clear image (image density 1.18) without capri was obtained, similar to the initial image. On the other hand, when images were produced in the same manner under a high temperature, high humidity environment (30°C, 190C, 19O), the image density was 1.06, and an image without problems such as capri was obtained.
Clear and capri-free images were obtained even under 10° c s 10 q & ).

[Example 2] 100 M parts of styrene-butyl methacrylate-dimethylamine ethyl methacrylate (weight ratio 7:2.5:0.5) copolymer, 50 parts by weight of γ-iron oxide, and 4 parts by weight of polyethylene wax. A fine powder was prepared in the same manner as in Example 1 except for using the following.

Furthermore, silicic acid fine powder synthesized by a dry method (trade name, Aerosil 0X-50, specific surface area approximately 50 mVg)
100 parts by weight (manufactured by Aerology Co., Ltd.) of silicone oil with amine in the side chain (viscosity 60 c at 25°C)
ps, amine equivalent: 360), and treated in the same manner as in Example 1.

To 100 parts by weight of the fine powder, 1 part by weight of the silicic acid fine powder treated with the silicone oil having an amine in the side chain was added to prepare a toner. When this toner was evaluated in the same manner as in Example 1, a clear sepia color image without capri was obtained. :0.5) 80 parts by weight of copolymer, styrene-butadiene (weight ratio 85:1
5) In substantially the same manner as in Example 1, 20 parts by weight of copolymer, 6 parts by weight of phthalocyanine blue, and 4 parts by weight of low molecular weight polypropylene were used to obtain a back color imitation powder having a particle size of about 5 to 20 μm.

On the other hand, 100 parts by weight of silicic acid fine powder synthesized by a dry method (trade name, Aerosil +200, specific surface area: approximately 200 mVg, manufactured by Aerosil) was used as a silicone oil with an amine in the side chain (viscosity at 25°C, 3500 cps, amine equivalent). 3800) and was treated in the same manner as in Example 1 using 100 parts by weight.

12 parts by weight of the above-mentioned backing fine powder, 0.3 parts by weight of treated silicic acid fine powder, and carrier iron powder (trade name, EFV250/400
．． (manufactured by Nippon Tetsuko Co., Ltd.) was mixed with 88 parts by weight to prepare a developer. On the other hand, a negative electrostatic latent image is formed on the OPC photoreceptor, this is developed with the above developer, and the resulting powder image is transferred to plain paper. (composed of a fuser roll coated with silicone rubber and a pressure roll whose surface was coated with silicone rubber). A clear blue image without capri was obtained.

[Example 4] 100 M parts of silicic acid fine powder with a specific surface area of about 90 rnVg synthesized by a wet method and a silicone oil having an amine in the side chain (viscosity 1300 cpsb, amine equivalent 1700
) Except for using 10 parts by weight, the same procedure as in Example 1 was carried out, and a clear image without capri was obtained.

[Example 5] 100 parts by weight of silicic acid fine powder synthesized by a dry method (trade name: Aerosil +380, specific surface area: approximately 380 mVgs, manufactured by Aerosil Co., Ltd.) and a silicone oil having an amine in the side chain (viscosity: 750, amine equivalent: 1900) was carried out in substantially the same manner as in Example 1 except that 40 parts by weight was used, and a clear image without capri was obtained.

[Example 6] 100 parts by weight of silicic acid fine powder with a specific surface area of approximately 120 mVg synthesized by a wet method and a silicone oil having an amine in the side chain (viscosity 1200 cps, amine equivalent 3500
) Except for using 15 parts by weight, the same procedure as in Example 1 was carried out, and a clear image without capri was obtained.

[Examples 7 to 13] Viscosity and amine equivalent were (250 cps, 7600), (
'3500cps, 2000), (1700cps,
3800), (90cps, 4000), (2'0cp
s, 320), (90 cps.

8800), (2300 cps, 38'00) except that a silicone oil having an amine in the side chain was used, and the same procedure as in Example 1 was conducted, and good results were obtained. [Example 14] ] As a silicone oil having an amine in the side chain, the viscosity is 60. Example 1 was carried out in substantially the same manner as in Example 1, except that 98 parts by weight of cps and amine equivalent of 22,500 were used, and a good image was obtained, although slightly inferior to Example 1. Image density was 0.83.

[Comparative Example 1] The same procedure as in Example 1 was carried out using untreated silicic acid fine powder without using the silicic acid fine powder treated with silicone oil having an amine in the side chain, but only a poor image was obtained. I couldn't get it. Image density ID: o, 21.

[Comparative Example 2] It was carried out in the same manner as in Example 1, except that an aminosilane coupling agent was used instead of the silicone oil having an amine in the side chain. Under an environment of normal temperature and normal humidity, An image with an image density of 0.91 was obtained, but in a high temperature and high humidity environment, the image density decreased significantly to 0.34.
There was no L, and only poor images were obtained.

The image densities under each environment in the examples are shown in the table below.

Procedural amendment (Jigen July 26, 1981 Manabu Shiga, Commissioner of the Patent Office1, Indication of the case, Patent Application No. 75848 of 1982,2, Name of the invention: Developer, 3, Person making the amendment, 11 cases) Relationship Patent applicant address 3-30-2 Shimomaruko, Ota-ku, Tokyo Name (100
)Representative of Canon Co., Ltd. Ryu Kaku Part 4, Agent address: 3-30-25 Shimomaruko, Ota-ku, Tokyo 146, Specification subject to amendment 6, Contents of the amendment (1) The scope of the claims is attached in the attached document. Correct as expected.

(2) Insert between lines 16 and 17 on page 17 of the specification, ``Furthermore, it is also preferable to perform a heat treatment at a temperature of about 50 to 400° C.''.

(3) Page 18 of the specification, lines 8 to 14, make the following corrections.

[Also, the silicic acid fine powder used in the present invention may be treated with a treatment agent such as a silane coupling agent or an organosilicon compound for the purpose of hydrophobization according to 8 yellow, and the method can also be a known method. is used and treated with the treatment agent described in 1., which reacts with or physically adsorbs to the silicic acid fine powder. Such processing agents and lans, aminopropyltriethoxysilane, diethylaminopropyltrimethoxysilane, aminophenyl I-rimethoxysilane, dimethylaminophenyltriethoxysilane, dimethylsilicone oil, hexano] 2. Claims (1) ) A developer containing fine silicic acid powder treated with silicone oil having an amine in its side chain.

U load l ・ 1 image no method.

Claims (1)

[Claims] A developer containing fine silicic acid powder treated with silicone oil having an amine in its side chain.